Method for the procedurally economical removal / fractionation of constituents of vegetal starting material, and the production and use of same

Abstract

The present invention relates to a procedurally economical method for removing and / or fractionating constituents consisting of water-soluble and dissolved compounds comprising proteins and / or carbohydrates and / or flavouring agents and / or colouring agents and / or fats and / or toxins; optionally water-soluble and undissolved compounds comprising starch; solid materials comprising cellulose-based fibres and / or lignin-rich shells; a protein-containing biogenic starting material.

Description

[0001] Methods for the process-economical separation / separation of constituents of plant starting materials as well as their extraction and use.

[0002] background

[0003] The composition of plant products, such as seeds, kernels, or grains, can be essentially divided into four main constituents: neutral lipids (8–40%), carbohydrates (15–35%), proteins (20–50%), and fiber (20–40%). Furthermore, plant products contain variable amounts of pigments, odorants, polar lipids, antioxidants, minerals, and other substances. The use of the constituents of such plant products is of central importance in human and animal nutrition. For example, seeds with a high oil content are pressed for oil extraction. After the removal of the neutral lipids, an oil content of 5 to 15% by weight remains in the press residue. This percentage can be reduced to values ​​of 2–8% by weight through a subsequent extraction process, although this requires increased processing effort.

[0004] Plant seeds with a low neutral fat content are crushed or ground, and the resulting particles are sorted using physical methods such as sieving or air classification to obtain fractions with a high proportion of specific constituents. To comply with quality standards for the use of the available products, limits must be observed regarding the levels of neutral lipids, colorings, odorants, flavorings, and antinutritional compounds.

[0005] In addition to neutral lipids, press residues and milled products also contain lipophilic by-products such as carotenoids, lecithins, and lipophilic alkaloids, which are detrimental to the material utilization of the main components, particularly the protein fraction. Odors and flavors are also frequently problematic and reduce product quality. Therefore, processes such as debittering and detoxification have been developed to enable the use of the recoverable products, especially proteins, for human nutrition. These processes are energy-intensive and / or require the use of organic solvents. Furthermore, antinutritive compounds such as ureases, trypsin inhibitors, and alpha-glucosidases may be present in press residues and milled products. According to the state of the art, such compounds are inactivated, for example, by blanching processes.This involves exposing the plant material to hot steam, which inactivates antinutritive enzymes but also inevitably alters the structure of storage proteins, causing them to lose their native form and properties. To carry out such processes as efficiently as possible, the plant material must be very finely ground to enable, for example, efficient debittering using conventional techniques. WO 83 / 00419 proposes grinding the seed material into a very fine flour with particle sizes between 1 µm and 50 µm, which requires further processing steps and increased energy consumption. Other prior art methods remove odor and flavor compounds from the isolated plant protein fractions by washing with organic solvents, such as...Isopropanol, removed (Yumi-ko Yoshie-Star, Functional and bioactive properties of rapeseed protein concentrates and sensory analysis of food application with rapeseed protein concentrates, LWT - Food Science and Technology Volume 39, 2006, pp. 503-512). Furthermore, it is generally required that the residual neutral lipid content in products derived from plant seeds be < 1 wt%. Therefore, according to the state of the art, it is necessary to de-oil the plant material before product extraction or further processing. This applies particularly to protein fractions that can be obtained from plant starting materials. More recently, techniques have been introduced that allow for simultaneous de-oiling and protein extraction. These processes are essentially based on the displacement of the oil from the open cell structures by an alcoholic solution.However, during implementation, it became apparent that a high oil yield required complete digestion of the seed material. Even with the application of strong shear forces using shear mixers or high-pressure homogenizers, only 63% of the oil present in the starting material was separated with the aqueous extract, and approximately one quarter remained bound in the fine solids. In the best-case scenario, an oil yield of only 72% was achieved. While this deficiency could be improved by using an aqueous alcoholic solution according to the Friolex process (EP1228701 AI), this also resulted in significantly higher process costs.

[0006] Due to the quality requirements for applications of sustainably sourced products from the processing of plant seeds and kernels as food for humans, the economic viability of many press residues or milled products from plant seeds / kernels is currently largely unattainable. For example, the majority of press residues from rapeseed are used for animal feed. However, the pressed or milled material also contains plant materials that are not nutritionally valuable, such as lignin-containing fibers. These, in turn, have high potential as valuable materials, since biopolymers and derivatives can be produced from them that are sustainably usable. Methods for obtaining the purest possible lignin-containing fiber fraction from press residues or milled products are not yet known. Furthermore, plant seeds contain significant amounts of fibers, which also represent a valuable resource.The strong binding of proteins and soluble carbohydrates to these fiber structures is the reason why there is currently no method by which the fiber fractions can be separated economically and in pure form from plant seeds.

[0007] Wet-technical processes have been proposed for the extraction of proteins from plant seeds (DE19643961 C2). These processes attempt to extract proteins using alkaline earth metal solutions or inorganic or organic acids. Here, too, complete mechanical digestion of the seed material and intensive mixing of the milled material with the aqueous extraction agents using homogenizers are required. To obtain a fraction with a protein content exceeding 50%, the seed material must be heated to over 70°C. The use of separators or decanters is then necessary for material separation. The protein fraction that can be dissolved in the aqueous medium under these conditions can only be separated in a relevant quantity at a pH range of 2.5 to 4.5 following protein coagulation.Ultracentrifugation or ultrafiltration is required to recover the process water. The use of these separation methods contributes significantly to the high process costs compared to other methods. It has been shown that the physical properties of proteins obtained under state-of-the-art separation conditions, i.e., by acidic or thermal coagulation in a wet process, are significantly inferior to those obtained under neutral pH conditions, e.g., by ultracentrifugation. Furthermore, it is known that with increasing degree of protein denaturation, their water solubility decreases, and their functional properties, such as water-binding and emulsifying capacity, foaming behavior, and stability, correlate with this.Therefore, temperature increases above 60°C, as commonly used in wet extraction processes, should be avoided. Furthermore, the known methods do not remove most antinutritive substances from the recoverable protein fraction. This is particularly true for phytic acid, which, for example, is present in pea protein fractions at a dry weight of 3-5%. Another example is alpha-glucosidases, which are present in protein fractions obtained in this way at a mass concentration of 0.5 to 3.5 wt%. Other antinutritive compounds include trypsin inhibitors, tannins, saponins, lectins, cyanoglycosides, phytohaemagglutinin redase inhibitors, phytic acid alkaloids, gossypol, glucosinolates, and sinapines.

[0008] Plant products, such as plant seeds, also contain endogenous or exogenous substances that are potentially toxic to humans. Endogenous toxins, which are produced by the plant itself, include, for example, phorbol esters in the case of jatropha oilseeds or erucic acid in the case of camelina seeds. Exogenous compounds, which accumulate in plant compartments (protein or oil), include pesticides, herbicides, and fungicides.

[0009] To improve the nutritional and / or functional properties of protein fractions obtained by aqueous digestion of pressed or ground plant seeds, it may be necessary to add further compounds, such as carbohydrates, vitamins, or antioxidants, to the protein fraction. According to the state of the art, this is achieved with protein fractions obtained from a separation process by subsequently adding these compounds to the protein condensates or isolates and mixing them with the protein. However, a uniform distribution / binding of these compounds with proteins, which can be crucial for the development of specific functional and nutritional properties, can only be achieved if electrostatic self-assembly of these compounds occurs in the hydrophilic or hydrophobic protein domains.This results in the combination product (protein + self-assembled compound(s)) having different physical properties than if, as in the prior art, already condensed proteins are "coated" with other compounds, i.e., adhered to or agglomerated with the aggregated proteins. This difference can be of great importance for the qualitative and functional outcome of the product. No prior art methods are known for loading and separating proteins with other compounds during an extraction process in such a way as to obtain a combination product in which a physiological spatial arrangement of the compounds has been established through self-assembly.

[0010] There is therefore a need for a process that allows the constituents of plant products, such as milled products and press residues from plant seeds, to be separated and fractionated according to their main constituents using a simple aqueous digestion and extraction process, while maintaining improved product quality. Furthermore, there is a great need for a wet-technical extraction process for the constituents of plant seeds and kernels that can be operated economically. This particularly concerns the reusability of the process materials used, especially the process water, since such processes generate large quantities of process water with significant total organic carbon (TOC) content. Moreover, these processes are energy-intensive, so there is a great need for a low-energy digestion process for plant seeds and kernels.Furthermore, there is a great need to provide a wet-technical process that ensures complete material utilization of the main components of plant seed and milled products, so that pure fractions of oils, proteins, carbohydrates and fibers can be produced in a directly usable form.

[0011] The Chinese patent application CN 106 720 920 A describes a process for producing soy protein isolate, where a large volume of water is necessary for the hydration of compounds.

[0012] US patent application US 2004 / 009263 AI discloses a process for extracting zein from cornmeal. The protein particles are larger than Iomi.

[0013] EP 2 404 509 AI is a European patent application directed to the extraction of protein from fresh grape seeds. Precipitation is achieved using acid at a pH of 3.

[0014] Liu ui-Lin et al. describe the extraction of proteins from pumpkin seeds in the scientific publication Food Analytical Methods, Springer New York LLC, US, Vol. 10, No. 6, November 21, 2016, pages 1169-1680. An ionic liquid (PEG-choline chloride) is used as the extraction solvent. One problem is that polyphenols and tannins are also known to be extracted using this method and thus enter the product phase.

[0015] Schneider et al. (Nahrung - Foo, Vol. 33, No. 2, January 1, 1989, pages 177-182) describe the aqueous extraction of proteins from broad beans. Water is used for protein extraction. Protein precipitation with hydrochloric acid at a pH of 4.2 is performed. After solid separation, neutralization with NaOH is carried out. The neutralized water is reused; in parallel / alternatively, an aqueous rinsing solution of the protein phase is used. The process was reused 10 times. As expected, the salt concentration increases; since a plateau is reached, sodium chloride must be carried out into the protein phase, which is undesirable. 100% reuse is not recommended; the fresh water savings rate is reported to be 40%. US patent application US 2015 / 073127 AI is directed to methods for isolating proteins from flour or oilcake.Extraction is carried out using a large volume of water, which is then reduced again by ultrafiltration, thereby removing toxic compounds and soluble carbohydrates from the aqueous protein solution. The exemplary processes presented here, representing the state of the art, also demonstrate that no process currently exists that aims for the complete separation of all constituents of a plant-based starting material while ensuring an economically viable and industrially applicable process technology that directly yields all constituents as usable products.

[0016] Therefore, there is a great need for a process that not only enables the complete breakdown of the constituents of a plant starting material and the obtaining of immediately usable products from the purified constituents, but also one that is economically viable, completely eliminates the use of organic solvents, and allows for the complete reuse of the substances used and the required volume of water, while simultaneously improving the products obtainable from the process.

[0017] Description

[0018] The present invention relates to a method for the process-economical separation and / or separation of all constituents comprising

[0019] - water-soluble and dissolved compounds including proteins and carbohydrates and / or flavorings and / or colorings and / or fats and / or toxins;

[0020] - optionally including water-soluble and insoluble compounds, including starch;

[0021] - solid solids comprising cellulose-based fibers and / or lignin-rich shells, which are in dehydrated / compacted form;

[0022] a protein-containing biogenic starting material, wherein the process comprises the following steps:

[0023] 1) Providing the protein-containing biogenic starting material,

[0024] 2a) Adding the starting material of step 1) to an aqueous solution with a pH between 7.5 and 13.5, containing at least one dissolved amino acid with a molar mass of less than 400 g / mol and a solubility of at least 35 g / L in water at 20°C and / or a peptide consisting of 2 to 50, preferably 2 to 10, of these amino acids to completely saturate the constituents of the protein-containing biogenic starting material, until hydrated soluble compounds are obtained and the solids are decompacted.

[0025] 2b) Addition of an aqueous distribution volume with a weight ratio to the dry mass of the protein-containing biogenic starting material of 5:1 to 500:1 and mixing to obtain a distribution mixture of the separated and / or separated constituents from step 2a), yielding dissolved soluble compounds and decompacted solid solids; 3) Separation of the solid decompacted solids and, optionally, the undissolved water-soluble compounds from the distribution mixture of step 2b), yielding an aqueous solution of the water-soluble and dissolved compounds without solid solids and without the optional water-soluble and undissolved compounds.

[0026] 4) Addition of an aggregating agent comprising an aqueous solution containing at least one organic acid and aggregation of the water-soluble and dissolved compounds comprising proteins and / or carbohydrates of the aqueous solution of step 3) to obtain a suspension of the aggregated compounds comprising the proteins and / or carbohydrates (i.e. the proteins and, if present, the carbohydrates) and an aqueous phase containing the non-aggregated, water-soluble and dissolved compounds.

[0027] 5) Separation of the suspension from step 4) and dehydration of the aggregated compounds by separation of water, yielding dehydrated aggregated compounds and a clarified aqueous phase, and optionally purification of the clarified aqueous phase.

[0028] 6) Addition of the clarified aqueous phase from step 5) as an aqueous solution to step 2a) and / or as an aqueous distribution volume to step 2b), or

[0029] Use of the clarified aqueous phase from step 5) to purify the separated solids from step 3), or

[0030] Use of the clarified aqueous phase from step 5) to purify the separated solids from step 3) obtaining an aqueous washing phase and adding the aqueous washing phase as an aqueous solution to step 2a) and / or as an aqueous distribution volume to step 2b).

[0031] A protein-containing biogenic starting material is preferred, which is a non-lignified material.

[0032] It concerns plant material.

[0033] Preferably, the at least one amino acid and / or the one peptide is a cationic amino acid and / or a peptide containing at least one cationic amino acid.

[0034] To separate or divide the main constituents of plant seeds, grains, or kernels, their disintegration is necessary. Disintegration can be achieved through a prior art physical process, such as mechanical methods like peeling / skinning, comminution, crushing, pressing, or grinding, or thermal methods like blanching. However, thermal methods have the disadvantage of being energy-intensive and, more importantly, potentially damaging the constituents of the starting materials, rendering them unusable or only partially usable.

[0035] Among mechanical processes, pressing differs from other disintegrative processes in that cell and tissue structures in the pulping material are largely destroyed. This causes oil to be released, so that, in combination with residual moisture, e.g., from seeds, amphiphilic compounds such as phospholipids, glycolipids, free fatty acids, and also proteins are emulsified. The heat generated by friction simultaneously causes these and other components of the seed to bond together to form a homogeneous, practically water-free mass. This also includes broken or shattered fiber components. Therefore, press cakes are generally very hard and hydrophobic, exhibiting only a low capacity for water absorption. One problem with press cakes resulting from a pressing process is that they only swell over the course of several days when further processing with water is attempted to separate the constituents.Furthermore, insoluble aggregates remain that cannot pass through a coarse sieve. Therefore, the breakdown of a press cake resulting from a pressing process remains incomplete when using pure water. Although swelling can be significantly accelerated by adding an alkali, many insoluble aggregates still remain. Consequently, the formation of insoluble aggregates in a press cake resulting from a pressing process cannot be prevented with either a basic or a neutral aqueous phase. A nearly complete separation of the proteins from the solid constituents is not achievable with the previously described process.

[0036] Furthermore, aqueous processing leads to the breakdown or swelling of complex carbohydrates, such as starch, which quickly causes the resulting slurry to become slimy. The components of the pressed or milled products do not dissolve when acids are used.

[0037] The milling process also involves the disintegration of cell and fiber structures. Unlike pressing, however, the various components do not clump together. Therefore, the milled product dissolves relatively well in water, forming smaller aggregates. An alkaline solution also causes faster swelling. However, this also results in "slime formation" and the formation of insoluble aggregates that are visible to the naked eye. These insoluble aggregates cannot be dissolved further in the subsequent stages of the process using an aqueous solution. Furthermore, combining a milling process with subsequent treatment using an alkali has the disadvantage that a nearly complete separation of the proteins from the solid constituents cannot be achieved. US patent application US 2015 / 073127 AI is directed to methods for isolating proteins from flour or oilcake.Extraction is carried out using a large volume of water, which is then reduced again by ultrafiltration, thereby removing toxic compounds and soluble carbohydrates from the aqueous protein solution. Precipitation with an alcohol or acetone then takes place. According to the disclosure, the separation of hydrophobic compounds, such as polyphenols, can only be achieved using the organic solvents employed. Since organic solvents destroy the tertiary structure of proteins, this can impair protein functionality. Whether the functionality of the products is preserved is not evident from the patent application. The product claims relate to isolates with a low content of solvents, sinapic acid, glucosinolates, and fats. The content of flavorings is not disclosed. Information on other hazardous substances is not apparent. The protein solubility is between 74% and 81%.Surprisingly, solutions of dissolved amino acids and / or peptides have been found to rapidly and completely separate the constituents in plant products such as seeds, kernels, or grains. It has been found that the constituents present in press residues and milled products can be very easily separated from one another in an aqueous medium by complete wetting with such an aqueous solution, i.e., impregnation. The formation of both mucilage and insoluble aggregates is achieved using an aqueous solution with a pH between 7.5 and 13.5, containing at least one dissolved amino acid with a molar mass of less than 400 g / mol and a solubility of at least 35 g / L in water at 20°C, and / or peptides consisting of 2 to 50 of these amino acids. Furthermore, complete impregnation of the protein-containing biogenic starting material is required.

[0038] In particular, and surprisingly, proteins detach from their solid constituents and simultaneously dissociate into their subunits. The dissolved proteins then pass through a membrane filter with a sieve size of 1000 and, very likely due to a large hydration shell, remain partially or permanently dissolved in the aqueous medium. The solubility can be recognized, for example, by the fact that the proteins remain suspended, i.e., they do not sediment or only settle to a very small extent. This can be detected, for example, by visual inspection or by determining the turbidity of the solution. Furthermore, complexed carbohydrates, such as starch, do not dissolve or swell only minimally in aqueous solutions containing dissolved cationic amino acids and / or peptides.On the other hand, proteins are rapidly and completely dissolved from both fiber compounds and shell components, allowing the latter to sediment very quickly while the proteins remain in solution. This enables a very simple and efficient separation of the lignin-rich shell components. The dissolution of proteins is facilitated in particular by aqueous solutions containing dissolved cationic amino acids and / or peptides from 2-50, preferably 2-20, and even more preferably 2-10 cationic amino acids such as Arg, Lys, His, and Phe, preferably Lys, His, and Arg, and particularly preferably Lys and His. This allows, for the first time, the isolation of fiber structures from these plant products, which can be classified as cellulose-based fibers due to their composition, to be achieved.Furthermore, it was found that cellulose-based fibers, from which proteins had been dissolved and thus decompacted, swell considerably in the aqueous digestion phases, making them very easy to separate from the dissolved proteins, for example, using conventional filtration techniques. In addition, it was found that the minimum solubility of the dissolved proteins shifts to a neutral pH range, allowing the proteins to condense and separate under very gentle conditions. Moreover, the process makes it possible to completely reuse the process water phases and to make the resulting products immediately available for applications without generating any residues or waste streams. This was particularly true when using cationic amino acids and peptides.A preferred method is therefore one in which, in addition to the at least one cationic amino acid and / or peptides consisting of 2 to 50 of these amino acids, no other amino acids are present in the aqueous solution with a pH between 7.5 and 13.5.

[0039] Therefore, the invention is directed to a process that enables a wet-technical complete digestion of plant products, in particular of plant disintegration products, such as pressed and ground products of seeds, kernels and grains, for the purpose of obtaining pure ingredients (constituents), such as in particular proteins, carbohydrates, cellulose-based fibers and lignin-rich shell components.

[0040] Furthermore, the process is aimed at the separation and production of functionally and / or nutritionally high-quality protein products from plant disintegration products. The process is also aimed at the production of functionally and / or nutritionally high-quality combination compounds / aggregates with proteins from plant disintegration products.

[0041] Furthermore, the process is aimed at the production and preservation of high-quality and / or functional cellulose-based fibers and / or lignin-rich shell products.

[0042] Furthermore, the process is aimed at the economical use of the compounds and water volume required for the process, as well as the reusability of the process solutions used and the residue-free material recycling of the raw and process materials.

[0043] Furthermore, the processes according to the invention are aimed at the use of the obtainable functionally and / or qualitatively high-quality valuable material fractions, e.g. as food, food additives, starting materials in the chemical, pharmaceutical or agricultural industries.

[0044] The object of the present invention is therefore to provide a method by which the constituents of plant starting materials and in particular of disintegration products, such as press residues and milled products of plant seeds, are separated / separated by an aqueous process without further pretreatment, so that the main components are completely separated from each other in an aqueous process liquid, from which the dissolved and solid constituents can be separated in successive process steps and obtained in pure form.

[0045] The invention also aims to simultaneously remove unwanted or separately usable organic and / or inorganic compounds and, if necessary, to make them available for further use after their separation.

[0046] Furthermore, the object of the invention is to provide a method by which protein fractions can be obtained that contain further organic compounds which originate from or are added to the starting material, thereby improving the product properties of the obtainable combination products.

[0047] Ultimately, the object of the invention is to provide a method that economically ensures the reusability of the process fluids and the compounds used for digestion. Surprisingly, it is possible to digest disintegration products of plant seeds, kernels, and grains using an aqueous process and to separate them into their main components using suitable process technology, obtaining pure products with improved product quality.

[0048] The requirements for economic process engineering can also be met in a highly advantageous way by one of the process sequences described herein.

[0049] Detailed description

[0050] Surprisingly, it was found that aqueous solutions containing amino acids and / or peptides in dissolved form cause proteins to detach from other constituents of a plant starting material, thereby dissolving the previously existing bond / compacting between and under the constituents of the starting material, and subsequently the various constituents are present in a decompacted, separable, and pure form.

[0051] Surprisingly, it was found that, in addition to the release of proteins from their matrix and their disintegration into subunits, the aqueous digestion solutions according to the invention also result in complete hydrogenation of the proteins. This leads to significant expansion and water binding of the proteins dissolved in the aqueous solutions containing dissolved cationic amino acids and / or peptides, causing them to remain suspended in the aqueous digestion medium in isolated form with a low specific gravity. Thus, a strong turbidity of an aqueous digestion solution according to the invention, with which rapeseed press cake had been treated, remained consistently turbid for more than six weeks. Subsequent condensation of the dissolved proteins completely clarified the digestion solution; the resulting condensates consisted of >90 wt% proteins.

[0052] It was found that aqueous solutions containing dissolved amino acids and / or peptides caused a rapid decomposition of press residues or flours into their constituent parts, which was not the case with pure water, an alkaline solution, or an acidic solution. These effects were particularly pronounced when cationic amino acids and / or peptides containing cationic amino acids were present in the digestion solutions. It was demonstrated that the separation of the constituents of the plant material occurs at the interfaces of these constituents, as there was practically no adhesion to the surfaces of the solid constituents, such as those of fibers, husks, or complex carbohydrate compounds. This separation process is highly effective even at room temperature.Such residue-free separation of surface adhesions from the solid constituents of the starting materials could not be achieved with other solutions, or not under the same conditions.

[0053] The effectiveness of the process was demonstrated for the use of aqueous solutions of individual dissolved cationic amino acids, dissolved peptides, and peptides containing said amino acids or functionalities of these amino acids, as well as for combinations of various dissolved amino acids and dissolved peptides with cationic amino acids and / or peptides. The cause of this surprising effect—the separation of constituents at their interfaces—is unclear. A preferred method is one for separating organic constituents from plant starting materials, in which the separation of the constituents is achieved using an aqueous solution containing dissolved amino acids and / or peptides. A particularly preferred embodiment of the process is one in which the dissolved amino acids and / or peptides are dissolved cationic amino acids and / or peptides.

[0054] The processes according to the invention can be carried out with one or more dissolved amino acids and / or dissolved oligo- or polypeptides with different amino acid sequences, or with different dissolved oligo- or polypeptides, each of which is an oligo- or polypeptide of a single amino acid, provided that these substances are solubilizable in an aqueous medium. It has been shown that even hydrophobic amino acids are suitable for achieving the separation and decomposition of proteins according to the invention, provided they are in solution, such as phenylalanine in an oligopeptide with lysine. It is necessary that the amino acids and / or peptides are present in a form completely dissolved in water and are added to the organic material to be decongested in this form, or that they can come into contact with it in a water-soluble form. The amino acids arginine, lysine, histidine, and phenylalanine are particularly suitable.Other alpha-carboxylic acids are also suitable. Di-, tri-, or oligopeptides, as well as polypeptides composed of one, two, or more amino acids, are also suitable. Short-chain peptides, e.g., DG, are preferred. Peptides consisting of amino acids with both hydrophobic and hydrophilic side groups are particularly preferred, such as (listed alphabetically by amino acid name) GLK, QHM, KSF, ACG, HML, SPR, EHP, or SFA. Peptides with both hydrophobic and cationic and / or anionic side groups, such as RDG, BCAA, NCR, HIS, SPR, EHP, or SFA, are also particularly preferred. Further examples with four amino acids are NCQA, SIHC, DCGA, TSVR, HIMS, or RNIF, and with five amino acids are HHGQC, STYHK, DCQHR, HHKSS, TSSHH, and NSRR. RDG, SKH or RRC are particularly preferred.Particularly preferred are di, tri or oligopeptides as well as polypeptides containing at least one cationic amino acid or di, tri or oligopeptides as well as polypeptides containing a functionality characteristic of a cationic amino acid.

[0055] When using cationic amino acids, the term "peptide", which is then used without further specification, means that a peptide consists of 2-50, preferably 2-20 and further preferably 2-10 amino acids, preferably proteinogenic amino acids, wherein the peptide consists of at least 20%, preferably at least 30%, further preferably at least 50%, still more preferably at least 80% and most preferably 100% of the amino acids from cationic amino acids, in particular Lys, His and Arg.

[0056] Thus, the present invention also relates to a method for the process-economical separation and / or separation of all constituents, comprising

[0057] water-soluble and dissolved compounds including proteins and carbohydrates and / or flavorings and / or colorings and / or fats and / or toxins;

[0058] - optionally water-soluble and insoluble compounds including starch; solid solids including cellulose-based fibers and / or lignin-rich shells;

[0059] nes protein-containing biogenic starting material, the process comprising the following steps:

[0060] 1) Providing the protein-containing biogenic starting material,

[0061] 2a) Adding the starting material of step 1) to an aqueous solution with a pH between 7.5 and 13.5, containing at least one dissolved cationic amino acid with a molar mass of less than 400 g / mol and a solubility of at least 35 g / L in water at 20°C and / or peptides of 2 to 50, preferably 2 to 10, of these amino acids, preferably at least one dissolved proteinogenic cationic amino acid and / or peptides of 2 to 50, preferably 2 to 10, of these proteinogenic cationic amino acids, to completely saturate the constituents of the protein-containing biogenic starting material, until hydrated soluble compounds are obtained and the solids are decompacted.

[0062] 2b) Addition of an aqueous distribution volume with a weight ratio to the dry mass of the protein-containing biogenic starting material of 5:1 to 500:1 and mixing to obtain a distribution mixture of the separated and / or separated constituents from step 2a), yielding dissolved soluble compounds and decompacted solids.

[0063] 3) Separation of the solid decompacted solids and optionally the undissolved water-soluble compounds from the partition mixture of step 2b) to obtain an aqueous solution of the water-soluble and dissolved compounds without solid solids and without the optional water-soluble and undissolved compounds,

[0064] 4) Addition of an aggregating agent comprising an aqueous solution containing at least one organic acid and aggregation of the water-soluble and dissolved compounds comprising proteins and / or carbohydrates of the aqueous solution of step 3) to obtain a suspension of the aggregated compounds comprising the proteins and, if present, the carbohydrates, and an aqueous phase containing the non-aggregated, water-soluble and dissolved compounds.

[0065] 5) Separation of the suspension from step 4) and dehydration of the aggregated compounds by separation of water, yielding dehydrated aggregated compounds and a clarified aqueous phase, and optionally purification of the clarified aqueous phase.

[0066] 6) Addition of the clarified aqueous phase from step 5) as an aqueous solution to step 2a) and / or as an aqueous distribution volume to step 2b), or

[0067] Use of the clarified aqueous phase from step 5) to purify the separated solids from step 3), or

[0068] Use of the clarified aqueous phase from step 5) to purify the separated solids from step 3) obtaining an aqueous wash phase and adding the aqueous wash phase as an aqueous solution to step 2a) and / or as an aqueous

[0069] Distribution volume (step 2b).

[0070] Preferably, the protein-containing biogenic starting material is non-woody plant material.

[0071] However, the use of sulfur-containing amino acids can lead to undesirable sensory effects and structural and functional changes in proteins and cellulose-based fibers. For example, in the first step of the process according to CN 106 720 920 A, an aqueous solution containing cysteine ​​with a pH of 6-7 is provided. Since cysteine ​​has an isoelectric point of 5.3, sufficient hydration of proteins is not possible with this solution; in particular, hydration of compounds enclosed in solids, such as cellulose-based fibers, cannot be achieved. The description of the Chinese patent application indicates that in step 1, the pH is adjusted to 6-7 using an aqueous sodium hydroxide solution. Thus, cysteine ​​was present in an acidic solution and had to be neutralized with sodium hydroxide. Consequently, hydration of the proteins by cysteine ​​did not occur.

[0072] Effective hydration of proteins bound in / to fibers is known and, as shown in this application, cannot be achieved under these conditions. Furthermore, a large volume is initially added for hydration, which is very impractical if an expensive ingredient must be present in a certain and relevant concentration. The present application employs a method using impregnation, employing the minimum amount of water required to mediate hydration with the smallest amount of compounds contained therein. Additionally, cysteine ​​chemically interacts with proteins; for example, it modifies gluten (flour protein fraction) by depolymerizing the molecules of the glutenin fraction through thiol-disulfide exchange with the intermolecular disulfide bonds. This means that the cysteine ​​breaks the bond that holds the long chain molecules together.As a result, the dough becomes more elastic and develops faster, which is not always desirable and often poses a problem.

[0073] US patent application US 2004 / 009263 AI discloses a process for extracting zein from cornmeal. Sulfur-containing compounds, and in particular sulfur-containing amino acids, are used to selectively crosslink them with sulfur compounds from proteins. In both cases, proteins are chemically modified, which poses a problem if the goal is to obtain the natural proteins. A maximum pH of 7 is permitted during extraction. An alcohol is used for the extraction process. The protein particles are larger than 1 / 2 inch.

[0074] In a particularly preferred method, the aqueous solution with a pH between 7.5 and 13.5 contains, in addition to the at least one cationic amino acid and / or peptides consisting of 2 to 50 of these amino acids, no other amino acids.

[0075] Preferably, the at least one dissolved amino acid according to step 2a) has a molar mass in the range of 75 g / mol to 350 g / mol, more preferably from 100 g / mol to 320 g / mol, more preferably from 140 g / mol to 300 g / mol and / or a solubility of at least 75 g / L in water at 20°C, more preferably at least 100 g / L in water at 20°C and more preferably at least 140 g / L in water at 20°C and / or it is an α-, β- or γ-amino acid and / or a proteinogenic and / or non-proteinogenic amino acid.

[0076] The use of amino acids is particularly advantageous because they are physiological constituents of proteins and can remain in a protein fraction to be obtained. It is especially advantageous to select amino acids that are present in insufficient quantities in the separable protein fraction for human or animal nutrition and can be specifically added to the obtainable product. The same principle applies to the use of oligo- and polypeptides, provided they do not exhibit allergenic or toxic potential. An aqueous solution is preferred in which the dissolved amino acids and / or peptides according to the invention are present without further additives at a self-regulating pH of the solution.

[0077] In further preferred applications, the pH of the aqueous solution containing dissolved amino acids and / or peptides is changed by adding a base or an acid. This can be done, for example, to increase the solubility of one or more of the amino acids / peptides. Cationic amino acids such as arginine, lysine, or histidine are particularly suitable for this purpose. Hydroxide ions, as well as tertiary or quaternary amines such as triethylamine or ammonia, are also suitable. The selection and applicable concentration depend on the application (e.g., production of a food ingredient), the effects on the organic components to be dissolved (e.g., induction of hydrolysis or denaturation), and the leaching properties from the product and the process fluid (if problematic).The selection of a suitable acid and its concentration depend analogously on the application and its potential presence in the product. Suitable acids include, for example, organic acids such as lactate, pyruvate, citric acid, oxalic acid, phosphoric acid, ascorbic acid, acetic acid, and EDTA, as well as inorganic acids such as phosphoric acid and sulfuric acid. The selection criteria for a suitable base or acid are known to those skilled in the art.

[0078] However, it is also possible to achieve solvent mediation using ternary systems, i.e., with the aid of co-solvents. Suitable co-solvents include alcohols such as isopropyl alcohol, ethanol, or methanol, as well as ethoxylates, ethers, esters, DMSO, betaines, sulfobetaines, or imidazolines, but other solvents can also be used. The use of only low concentrations is preferred. Suitable co-solvents can also be organic compounds with low or no polarity. For example, carboxylic acids such as hexanoic or octanoic acid can be added. Alternatively, alkyl compounds such as hexane or octane, as well as methyl esters of fatty acids and triglycerides such as rapeseed or sunflower oil, can be used. Combinations of various low-polarity to non-polar organic solvents are preferred.The use of a low concentration relative to the concentration of dissolved amino acids and / or peptides is preferred. The use of slightly polar or nonpolar compounds is particularly advantageous when the organic agglomerates to be cleaved contain amphiphilic or nonpolar compounds. The addition of slightly polar to nonpolar organic compounds facilitates the aggregation of the amphiphilic to nonpolar compounds to be separated within a developing lipid phase, thereby making it easier to separate them from an aqueous phase containing proteins and other hydrophilic compounds. Preferred nonpolar compounds include neutral fats such as triglycerides, alkanes, or fatty acid methyl esters.

[0079] A preferred method is one for separating organic constituents from plant starting materials, in which slightly to non-polar organic solvents are used for the separation of amphiphilic or non-polar compounds.

[0080] The effect of using a solution of dissolved cationic amino acids and / or peptides on the solubility properties of the proteins dissolved by the methods was also unexpected. It is known from the literature that aqueous plant proteins exhibit a minimum solubility at a pH between 2.5 and 4.5 and can be coagulated by adding acids or corresponding buffer systems within this pH range, whereas this is not the case at pH levels above 5. During coagulation, the proteins unfold, resulting in the complete loss of their tertiary structure and, depending on the pH, also a loss of their secondary structure. This significantly alters the physicochemical properties of such degenerated proteins. Among other things, their water-binding capacity is greatly reduced. Other properties, such as crosslinkability, are also lost.The degree of denaturation is inversely correlated with the pH during coagulation with an acid. Depending on the degree of degeneration, coagulated proteins are no longer soluble in water or only partially soluble. Surprisingly, very rapid and complete condensation of proteins that had been separated with dissolved cationic amino acids and / or peptides and were present in solution in the aqueous medium occurred even with the addition of minimal amounts of acid. It was found that complete condensation of the dissolved proteins occurred at a neutral pH, i.e., pH 7, or in a near-neutral pH range, i.e., between 5.5 and 8. Such condensates can be broken down into very fine particles by vigorous agitation. A particularly preferred method is one in which, in step 4), the pH of the aqueous solution from step 3) is adjusted to a pH value in the range between 5.5 and 8.

[0081] Surprisingly, it was found that the method can shift the solubility minimum of dissolved proteins into a neutral or near-neutral pH range.

[0082] Surprisingly, a rapid decrease in the pH of the solution containing the proteins separated and dissolved according to the invention to a pH of < 5 resulted in only minimal aggregation of the dissolved proteins. The aggregation rate decreased further with decreasing pH, and the proteins were present in a milky form. Even a decrease in pH below 3 did not cause coagulation of the dissolved proteins. Thus, the inventive methods allow, surprisingly and advantageously, the minimum solubility of dissolved proteins to be shifted to a pH range greater than 5. Furthermore, it was surprising that the condensates did not lose their tertiary structure. Unlike protein coagulates, which lose their tertiary structure, the physicochemical properties of the resulting protein condensates were preserved.Furthermore, it has been shown that the condensation process, once initiated, continues spontaneously without the need for the addition of any of the condensing agents listed herein. This allows for complete spontaneous condensation of undenatured proteins without any significant inclusion of compounds added to initiate the condensation reaction. This is particularly advantageous because it eliminates the need for a purification process of the resulting protein mass, as is common practice in the prior art. Moreover, only a small amount of condensing agents is required. Furthermore, complex purification steps of the process solution, such as the neutralization of an acidic solution, are unnecessary. Finally, as described below, the process solution is immediately available for reuse in another process step.Furthermore, it was documented that the obtainable protein products, due to the preservation of their physicochemical properties, exhibit improved product characteristics compared to similar protein preparations from the prior art. Thus, the inventive method enables the separation of proteins at a neutral pH, thereby significantly improving the functional properties of the separated proteins, as demonstrated below. Therefore, a preferred embodiment of the inventive method involves dissolving proteins in / with a cationic amino acid and / or peptide solution to shift the minimum solubility of the dissolved proteins to a pH range preferably > 5, more preferably > 5.5, more preferably > 6, and more preferably > 7.Furthermore, it is preferred to achieve a solubility minimum of the dissolved proteins of < 13, more preferably of < 12, even more preferably of < 11 and more preferably of < 10. A shift of the solubility minimum of the dissolved proteins to pH 7 is particularly preferred.

[0083] A preferred method is one that achieves an increase in the minimum solubility of dissolved proteins.

[0084] A preferred method involves shifting the solubility minimum of dissolved proteins into a pH range between 5.5 and 8.

[0085] A preferred method is one for the condensation and separation of non-degenerated or nearly non-degenerated proteins, in which proteins dissolved in an aqueous solution containing dissolved amino acids and / or peptides are condensed by a condensing agent. A particularly preferred embodiment of the method is one in which the dissolved amino acids and / or peptides are dissolved cationic amino acids and / or peptides.

[0086] Proteins that are not, or nearly not, degeneratively altered and can be obtained by condensing dissolved proteins are preferred.

[0087] A preferred method involves shifting the solubility minimum to a pH range between 5.5 and 8 by dissolving amino acids and / or peptides, and allowing the dissolved proteins to be condensed and separated by adjusting the pH of the solution to a value between 5.5 and 8. A particularly preferred embodiment of the method is one in which the dissolved amino acids and / or peptides are dissolved cationic amino acids and / or peptides.

[0088] It has been shown that for the same proteins in which an increase in the minimum solubility has been achieved using the methods according to the invention, such as those from rapeseed or soybean press cake, when they were preparatively extracted from the starting material, the minimum solubility was in a pH range of 2.8 to 4.2.

[0089] Furthermore, it was surprisingly demonstrated that for proteins where the solubility minimum has been shifted into a neutral or near-neutral range by the dissolved cationic amino acids and / or peptides, the dissolved and hydrated proteins can also be condensed with a variety of ionic or non-ionic compounds. For example, condensation according to the invention could be achieved with a pH-neutral CaCl₂ solution, as well as with solutions containing silicate and / or carbonate anions. The protein condensates are characterized by the fact that they form very voluminous three-dimensional structures that exhibit only a slight tendency to sedimentation due to a large hydration shell.In contrast to coagulates produced by acid precipitation of plant protein isolates with acids at a pH between 2.5 and 4.5, the condensates or the dehydrated mass of condensates were rapidly soluble upon resuspension in water, whereas this was not the case, or only to a small extent, for the acid-coagulated proteins. Such coagulated proteins also had significantly smaller volumes and a considerably lower proportion of bound water. Therefore, in contrast to coagulated proteins, the condensed proteins according to the invention retain a hydration shell, which enables rapid hydration of condensed and / or condensed and dehydrated proteins. Surprisingly, it has been shown that these properties have a decisive influence on further processing steps of the condensed and / or condensed and dehydrated proteins.In particular, easier hydration significantly improves processes such as purification, conditioning, functionalization, or bonding / contacting with other compounds.

[0090] Surprisingly, it has been shown that dissolved cationic amino acids and / or dissolved peptides containing cationic amino acids or exhibiting a positive overall charge are particularly suitable for enabling the increase in the minimum solubility of dissolved proteins according to the invention. Dissolved cationic amino acids and / or dissolved peptides containing cationic amino acids or exhibiting a positive charge are therefore particularly preferred. Arginine, lysine, histidine, and their derivatives are especially preferred.

[0091] A preferred method is one in which an increase in the minimum solubility of dissolved proteins is achieved by dissolved cationic amino acids and / or dissolved peptides containing cationic amino acids.

[0092] Furthermore, it was surprising that the proteins, in which the solubility minimum had been shifted to a neutral pH range using the amino acid and / or peptide solutions according to the invention, and the dissolved proteins had been condensed by adjusting the pH to this range, were completely or almost completely odorless and tasteless when separated from the aqueous medium, and also contained no or almost no pigments that could be leached out by an aqueous medium. Moreover, the protein fraction obtained had a neutral pH. Proteins obtained in this way were very easily soluble upon resuspension in water.Surprisingly, it was found that cationic amino acids and / or peptides, in particular, when dissolved and added to such a suspension, caused protein hydration even at very low concentrations. This resulted in the hydrated and condensed proteins exhibiting a very high water-binding capacity. This was determined by condensing the hydrated proteins and removing free water through a filter (sieve size Iomit) in a vacuum filter. The non-flowing residue was weighed and dried in a drying oven, and its dry weight was determined. The water-binding capacity was calculated from the difference in weight relative to the dry weight. This capacity ranged from 430 to 850 wt% for such resuspended proteins.

[0093] Furthermore, it could be shown that preparatively obtained proteins, which exhibited a solubility minimum in a pH range between 2.5 and 4.5, after suspension in an amino acid and / or peptide solution prepared according to the invention, had a solubility minimum between pH 6.5 and 8.5 and could be condensed, dehydrated and separated with the compounds listed herein. It was then found that the water-binding capacity of the same proteins, obtained from the starting materials by means of an extraction process and exhibiting a minimum solubility at a pH between 2.8 and 4.2, was between 140 and 220 wt% after 10 hours of resuspension in water, while the water-binding capacity of the same proteins, when suspended or resuspended in a solution with dissolved cationic amino acids and / or peptides, increased to values ​​between 450 and 650 wt%.

[0094] Therefore, in a preferred embodiment of the process, coagulated proteins are suspended and / or resuspended and hydrated using an amino acid and / or peptide solution, thereby achieving a water binding capacity of preferably > 400 wt%, more preferably > 500 wt%, further preferably > 600 wt% and even more preferably > 700 wt%.

[0095] A preferred method is one for hydrating coagulated proteins by suspension in a solution of dissolved amino acids and / or peptides. A particularly preferred embodiment of the method is one in which the dissolved amino acids and / or peptides are dissolved cationic amino acids and / or peptides.

[0096] Cationic amino acids and / or peptides are preferred. The preferred concentration of the cationic amino acids and / or peptides present in the suspension with the proteins to be hydrated is between 1 mmol and 3 mol / l, more preferably between 1 mmol and 1 mol / l, and further preferably between 1 mmol and 0.5 mol / l. The temperature at which the hydration of proteins according to the invention takes place is preferably between 5 and 90°C, more preferably between 10 and 60°C, and further preferably between 15 and 45°C. The pH of the solution in which the hydration of proteins according to the invention takes place is preferably between 7.5 and 13.5, more preferably between 7.5 and 12.5, and further preferably between 7.5 and 11.5. Preferably, the solution containing the proteins to be hydrated is agitated; a propeller mixer is preferred.The time required for complete protein hydration depends on the other process parameters and must therefore be determined individually. A duration between 5 minutes and 5 days is preferred, more preferably between 10 minutes and 1 day, and further preferably between 15 minutes and 1 hour. A preferred method involves hydrating proteins using amino acid and / or peptide solutions. A particularly preferred embodiment of the method uses dissolved cationic amino acids and / or peptides.

[0097] A preferred method is one for the suspension and / or desuspension and hydration of condensed / aggregated / complexed proteins with amino acid and / or peptide solutions. A particularly preferred embodiment of the method is one in which the dissolved amino acids and / or peptides are dissolved cationic amino acids and / or peptides.

[0098] A preferred method is one for increasing the water-binding capacity of proteins by means of dissolved cationic amino acids and / or peptides.

[0099] Separation and separation processes.

[0100] It is known from the prior art that proteins linked or complexed with other compounds exhibit only low water uptake and water-binding capacity. This explains why seeds, grains, or kernels are only slowly and incompletely permeated by water, even after mechanical disintegration and digestion. It has been shown that prior art bases and acids are not suitable for achieving the complete digestion of plant starting material into its main constituents, even after mechanical disintegration. Investigations into the separation of constituents of plant starting materials in aqueous solutions showed that alkaline aqueous solutions prepared with alkaline earth metals did not lead to the complete dissolution of the solid aggregates of press residues.Surprisingly, aqueous solutions of highly water-soluble amino acids initially caused the starting materials to swell considerably, and then disperse spontaneously. Gentle stirring made the main constituents visible in the aqueous phase, allowing them to be isolated. It was subsequently demonstrated that immersing the starting materials in aqueous solutions containing dissolved amino acids and / or peptides also resulted in the rapid and complete dissolution of the constituents, which could then be isolated. This was particularly evident in the presence of cationic amino acids or peptides containing cationic amino acids.

[0101] In a preferred embodiment of the process, mechanically disintegrated plant starting materials are added to an aqueous solution containing one or more amino acids and / or peptides in dissolved form and left therein until complete separation of the main constituents of the starting materials has occurred and these are dissolved or suspended in a separable form. The weight ratio between the starting material and the aqueous solution is preferably between 1:5 and 1:500, more preferably between 1:10 and 1:150, and further preferably between 1:15 and 1:50. The temperature at which this takes place is freely selectable; preferably a temperature between 10 and 120°C, more preferably between 15 and 90°C, and further preferably between 20 and 60°C. Preferably, the mixing is carried out continuously or discontinuously.The duration of the process step in which the separation and distribution of the constituents of the starting material in a volume of water occur simultaneously depends on the process parameters and must be determined individually. Such a test can be performed, for example, by taking a representative sample from the agitated solution mixture and filtering it through a sieve (sieve size I0m). The process is complete if no aggregates of different constituents of the starting materials are recognizable in the sieve residue and the constituents can be easily separated.

[0102] A preferred method is one in which the separation of the constituents of mechanically disintegrated seeds, grains or kernels is achieved by immersing the seeds, grains or kernels in a solution containing dissolved amino acids and / or peptides until the constituents can be easily separated.

[0103] Surprisingly, it was then found that soaking the plant materials in aqueous solutions containing dissolved amino acids and / or peptides led very rapidly to complete penetration of the aqueous solution by the plant material, which swelled slightly in the process. Subsequent addition of water then enabled complete dissolution of the constituents of the plant material. This was particularly true in the presence of cationic amino acids or peptides containing cationic amino acids. It was shown that even low concentrations of dissolved cationic amino acids and / or peptides, such as arginine or its derivatives, were sufficient to achieve this kind of separation of the composite structures of the plant materials. Conversely, a high concentration of dissolved amino acids and / or peptides accelerated the dissolution process.It has been shown that this process leads to disintegration between the main constituents of the plant material. It was found that distributing a completely saturated plant starting material in a sufficiently large volume of water results in the immediate and complete dissolution of the starting material's constituents, so that the various constituents are already present in isolated form. It was found that this method, compared to immersing the starting materials in an aqueous solution where separation and distribution of the dissolved constituents occur simultaneously, significantly reduces the amount of dissolved amino acids and / or peptides required for complete dissolution of the constituents.For example, it was demonstrated that a solution of arginine with a concentration of 10 mmol / l led to the complete separation of the constituents of the starting material within 1 hour, when the starting material was introduced into the solution at a weight ratio of 1:20. This weight ratio was sufficient to allow for the isolation of the constituents. If the plant starting material was completely saturated with the same solution, for which a mass-weight ratio of 1:1.2 was sufficient, and after 4 hours the saturated mass was dissolved and dispersed in water at the same mass ratio as in the preliminary investigation (1:20), an immediate and complete distribution of the constituents of the starting material was also observed.Comparative investigations with aqueous solutions of basic compounds showed that complete penetration was not possible and / or that, after distribution in a volume of water after 4 and 6 hours, only insufficient separation of the constituents of the starting material occurred. It could thus be shown that impregnating the plant starting material with an aqueous solution containing dissolved amino acids and / or peptides results in the breakdown of the constituents of the plant starting material, thereby enabling the distribution of the constituents in a sufficiently large volume of water without further addition of the compounds according to the invention. The process thus allows for a significant saving of amino acids and / or peptides required for the separation of the constituents of the starting materials according to the invention.In a preferred embodiment of the process, a separation / division phase takes place in which the plant starting material is brought into contact with an aqueous solution of amino acids and / or peptides present therein in dissolved form, such that complete impregnation / penetration of the plant starting material with the aqueous solution occurs. The presence of complete impregnation can be verified, for example, by mechanically finely dividing the impregnated starting material and visually or analytically confirming the completeness of the wetting.

[0104] A preferred method is one for separating constituents of plant starting materials, in which the constituents of the plant starting material are separated by impregnating the plant starting material with an aqueous solution containing dissolved amino acids and / or peptides. A particularly preferred embodiment of the method is one in which the dissolved amino acids and / or peptides are dissolved cationic amino acids and / or peptides.

[0105] In a preferred embodiment of the process, a step is carried out in which the mechanically disintegrated plant starting material is placed in a suitable container and impregnated with one of the aqueous solutions according to the invention, containing dissolved amino acids and / or peptides. Impregnation here means that, in the case of finely dispersed impregnated material, it is completely moist (moisture content > 20 wt%). Impregnation can be detected, for example, visually, e.g., by a change in color, or analytically, e.g., by a change in electrical conductivity. The term "moist" does not mean that the starting material is wet; no free liquid separates when the impregnated, moist starting material is centrifuged with 2,000 g. Impregnation with the aqueous solutions can be carried out using methods from the prior art.A suitable device for this purpose is, for example, a mixing vessel that allows for complete circulation of the mixture and into which the aqueous solution is added until complete saturation is observed in a representative sample. In another embodiment of the process, the plant-based starting material is distributed on a conveyor belt or a conveyor screen belt, and the distributed starting material is sprayed with the aqueous solution. Preferably, the plant-based starting material is treated with a volume of the aqueous solution containing dissolved amino acids and / or peptides, and in particular cationic amino acids or peptides with cationic amino acids, in a mass ratio of 1:0.5 to 1:10, more preferably between 1:1 and 1:8, and further preferably between 1:1.2 and 1:4.The temperature at which impregnation can take place is freely selectable; preferably a temperature between 6 and 90°C, more preferably between 10 and 60°C, and even more preferably between 18 and 40°C. After confirmation that impregnation is complete, the impregnated plant material can remain in the container in a resting or further agitated state, or be transferred to another container until the next process step. Transfer can be accomplished using known conveying techniques, for example, with a conveyor belt.

[0106] In a further preferred embodiment, the separation / separation process according to the invention is used to completely swell the plant starting material. The volume of aqueous solutions containing dissolved amino acids and / or peptides required for complete swelling of the starting material is greater than that required for complete saturation of the starting material. This can be particularly advantageous if the separation / separation mixture from this process step is to be transferred to another container with a pumping device; the swollen material can be easily conveyed using pumping devices from the prior art, e.g., through a pipeline.It was demonstrated that after the mechanically processed starting material swells, and this swelling does not increase further with the addition of more water, the separation process is complete. The constituents can then be completely separated from one another using water alone, without the need for any further addition of dissolved amino acids, peptides, or other compounds. In contrast to moistened starting materials, the fully swollen starting material is considered wet. Complete swelling can be recognized, for example, by the fact that the swollen material can no longer bind any additional water. This is evident from the fact that further addition of water does not lead to any further increase in the volume of the swollen, homogeneous material, and that centrifugation (2000 g) separates only a minimal amount of free liquid phase.To determine whether further water binding is possible, a 0.3 molar solution of the amino acid and / or peptide solution can be added in small volume units to a sample of the swollen material, the mass of which is determined. If a free aqueous phase forms, the swelling process is complete; otherwise, the addition of the amino acid and / or peptide solution to the mixture should be continued. The volume of aqueous solutions containing dissolved amino acids and / or peptides added naturally varies considerably depending on the starting material used and its form. A mass ratio of the starting material to the aqueous solutions containing dissolved amino acids and / or peptides between 1:4 and 1:20 is preferred, more preferably between 1:5 and 1:15, and further preferably between 1:6 and 1:10.The temperature at which the impregnation can take place is freely selectable; preferably a temperature between 6 and 90°C, more preferably between 10° and 60°C, and even more preferably between 18 and 40°C. The fully swollen plant material can remain in the container in a resting or further agitated state, or be transferred to another container until the next process step. Transfer can be accomplished using known conveying techniques, for example, with a screw pump that allows transport through a pipeline.

[0107] A preferred method for separating constituents of plant starting materials is one in which the constituents of the plant starting material are separated by swelling the plant starting material with an aqueous solution containing dissolved amino acids and / or peptides. A particularly preferred embodiment of the method is one in which the dissolved amino acids and / or peptides are dissolved cationic amino acids and / or peptides. In a preferred embodiment of the method, aqueous solutions containing dissolved amino acids and / or peptides at a concentration of preferably 1 mmol / l to 5 mol / l, more preferably 50 mmol / l to 1 mol / l, and further preferably between 100 mmol / l and 400 mmol / l are added for the process step of separating the plant starting material, which is carried out by means of an impregnation or swelling process.

[0108] The aqueous solution can be added once, several times, or continuously, as needed. The digestion process preferably takes place at ambient temperatures or within the previously specified temperature ranges. In other process embodiments, it may be advantageous to carry out the separation process at a reduced or elevated temperature. A reduced temperature is advantageous, for example, if a thermosensitive compound is to be obtained as a product from the mixture, and an elevated temperature is advantageous, for example, if simultaneous microbial reduction is desired.

[0109] To achieve complete separation of the constituents of the plant starting material, it is preferred to maintain a residence time between complete soaking or swelling and the execution of the next process step, preferably between 5 minutes and 24 hours, more preferably between 10 minutes and 12 hours, and more preferably between 20 minutes and 6 hours. Agitation of the mixture after soaking or swelling is not necessary. However, agitation, e.g., using a stirrer, can be carried out to prevent settling of components. The temperature of the mixture during storage / transport until the next protest call can be freely chosen; preferably a temperature between 6 and 90°C, more preferably between 10 and 60°C, and more preferably between 18 and 40°C.

[0110] A simple test procedure can be used to determine whether a mixture from this process step is suitable for transfer to the next process step. For this purpose, a representative sample is taken from the mixture and added to water (25°C) in a mass ratio of 1:20 and agitated for 2 minutes at 200 rpm. The entire suspension is then filtered (sieve size Iommi). The sieve residue is examined visually and / or microscopically for the presence of aggregates of constituents from the plant starting material. If no aggregates are present, sufficient separation of the constituents of the starting material has been achieved and the process step is complete.

[0111] Distribution procedure

[0112] In a preferred embodiment, after the process step in which the constituents of the plant starting material are separated, the constituents are distributed and singulated. Due to the complete dissolution of the proteins from other constituents, they acquire a high water-binding capacity. Therefore, a large aqueous distribution volume is required for spatial separation of the constituents.

[0113] Surprisingly, it was found that the separation of constituents of plant starting material according to the invention is enabled in a particularly advantageous way by providing a sufficiently large volume of water for the distribution and singulation of the solid and soluble dissolved constituents of the starting material, thereby directly obtaining particularly pure fractions. It was found that if an insufficient volume of water is provided in the distribution phase, the solid constituents of the plant starting material obtainable by filtration techniques cannot be singulated and exhibit adhesions of soluble constituents of the starting material. Therefore, a crucial criterion for the distribution and singulation of the solid constituents of the starting material according to the invention is the provision of a sufficiently large distribution volume.Furthermore, it has been shown that the condensation and / or aggregation and / or complexation of dissolved compounds by condensing agents according to the invention does not occur, or only occurs incompletely, if the dissolved soluble compounds are not present in a sufficiently large aqueous distribution volume. It has been shown that the required volume of water depends in particular on the composition, type, and concentration of the soluble constituents of the starting material, and therefore the required volume of water for carrying out the process step according to the invention must be determined individually.Determining a sufficiently large volume of water, which enables both the separation of the solid constituents of the starting material and the complete or almost complete condensation and / or aggregation and / or complexation of the soluble compounds dissolved therein with the condensing agents according to the invention, can be easily carried out by a person skilled in the art using the investigation methods described below.

[0114] In a preferred embodiment, the separation / division mixture is dissolved in water. For this purpose, clarified process water from subsequent process steps can be used, or deionized or untreated municipal or well water.

[0115] Preferably, a sufficiently large volume of water in the distribution phase is determined by preparing a dilution series with a sample from the previous process step (the separation / division mixture) (e.g., 10 g). After a stirring phase of 3 minutes, the suspension is filtered (sieve size Iommi). The filter residue is analyzed (visually or microscopically) for deposits / adhesions of soluble and water-soluble compounds. A suitable solution of a condensing agent is added to the filtrate in increasing doses. A sufficiently large dilution volume is present when there is no deposit / adhesion to the solid constituents of the starting material contained in the filter residue, and complete condensation and / or aggregation and / or complexation of the dissolved soluble compounds present in the distribution mixture occurs.

[0116] A preferred method is one for separating constituents of plant starting materials, in which the constituents of the plant starting material are separated using an aqueous solution containing dissolved amino acids and / or peptides, and subsequently a sufficiently large volume of water is provided for the distribution of the constituents. An embodiment of the method using dissolved cationic amino acids and / or peptides is particularly preferred.

[0117] A preferred method is one for determining a volume of water sufficient to isolate solid constituents of a plant starting material without adhesion and to completely or almost completely condense soluble compounds of the starting material, which are present in dissolved form, with a condensing agent.

[0118] The volume of water required for carrying out the following process step according to the invention is provided in a suitable container.

[0119] In a preferred embodiment, the water volume of this process step, or the mass ratio between the separation / division mixture of the preceding process step and the water phase of the distribution process step, is determined based on empirical or guideline values. Naturally, such value ranges can lie above or below the value determined by measuring a sufficiently large water volume required for optimal further process execution. In this process embodiment, a water volume to dry mass ratio of 5:1 to 500:1 is preferred, more preferably 10:1 to 150:1, and further preferably 15:1 to 50:1. The method of introducing or bringing into contact the separation / division mixture and the water phase of this process step is arbitrary.Preferably, the starting material is introduced using a high-performance shear mixer or another intensive mixer, together with the aqueous phase. This is particularly advantageous because it allows for the immediate separation of the constituents of the starting material in the aqueous phase, thus enabling the immediate further processing of the distribution mixture for material separation. In principle, all known methods for mixing solutions and suspensions can be used for this process step. The distribution process can be continuous or batchwise. The distribution process can be carried out at any temperature; preferably, the temperature range of the aqueous suspension is between 6 and 90°C, more preferably between 10 and 60°C, and even more preferably between 18 and 40°C.The duration of the distribution process is arbitrary; a duration of 1 minute to 24 hours is preferred, more preferred is 5 minutes to 5 hours, and further preferred is 10 minutes to 1 hour.

[0120] In one embodiment of the methods described herein, the mixing to obtain a distribution mixture of the separated and / or separated constituents from step 2a) is carried out by means of an intensive mixer.

[0121] The partitioning process is sufficient and complete when, in a representative sample taken from the partitioning mixture and subsequently filtered through a coarse (1 mm mesh) and a fine (1 mm mesh) sieve, no visible aggregates of different constituents of the plant starting materials are discernible to the naked eye at the sieve stage. Successful partitioning of the starting material constituents can also be confirmed by placing a sample of the partitioning mixture into a graduated cylinder and observing the rapid separation of three phases, or, in the presence of lipids, four readily distinguishable phases. This separation should not take longer than four hours.

[0122] The bottom phase is characterized by a high proportion of lignin-rich fiber materials, if present. The layer above contains a high proportion of cellulose-based fiber materials and complex carbohydrates. The aqueous phase above this contains dissolved soluble compounds, particularly dissolved proteins and dissolved soluble carbohydrates, as well as other soluble compounds. If lipids are present, they float to the surface of the aqueous solution. The composition and proportions of the other dissolved compounds vary considerably depending on the application of the process. These compounds can include sugars, vitamins, amino acids, carboxylic acids, polyphenols, dyes, and flavorings, all of which are present in dissolved form within the aqueous distribution volume.

[0123] Provided that the investigation into the completeness of the distribution process has shown sufficient separation of the constituents of the starting material, an immediately subsequent residue-free separation of the dissolved organic compounds and solids is possible.

[0124] A preferred method is one for separating constituents of plant starting materials, in which, following the separation of the constituents of the plant starting material by means of an aqueous solution containing dissolved amino acids and / or peptides, the constituents of the starting material are distributed in an aqueous phase. A particularly preferred embodiment of the method is one in which the dissolved amino acids and / or peptides are dissolved cationic amino acids and / or peptides.

[0125] In a particularly preferred embodiment, dilution with water ensures that the concentration of dissolved amino acids and / or peptides present in the distribution mixture following the distribution process is not reduced below 10 mmol / l, more preferably not below 30 mmol / l, and even more preferably not below 50 mmol / l. In a further preferred embodiment of the process, the presence of a specific concentration of the amino acids and / or peptides according to the invention can be adjusted by adding further dissolved amino acids and / or peptides. This can be achieved by a single, intensive mixing addition or by continuous mixing. It is advantageous to avoid air inclusion or bubble formation, as this can lead to foaming. Therefore, the use of laminar mixers is advantageous. Foaming can be prevented by known techniques.A further aspect of the invention is the monitoring and optional adjustment of the pH of the distribution solution. This can be achieved using alkalis or acids from the prior art; preferred acids are hydrochloric acid or formic acid, and preferred bases are sodium hydroxide or urea. A pH of the distribution solution between 7.5 and 13 is preferred, more preferably between 8.0 and 12.5, and further preferably between 8.5 and 11.

[0126] In further preferred embodiments, additives can be added to the distribution mixtures to achieve additional particularly advantageous effects. Such effects relate, for example, to surface conditioning of cellulose-based fibers that are expanded with the process water in this process step. Such conditioning can, for example, increase the water-binding capacity, which makes it easier to separate the cellulose-based fibers in subsequent process steps and results in improved product properties. Furthermore, the addition of adsorbents can, for example, facilitate the removal of dyes, toxins, or electrolytes, among other things.The selection of one or more additives to be added to the distribution volume of this process step depends on the specific application and the starting material and can be determined by a specialist. Possible additives include, for example: urea, DMSO, zeolites, and ion exchange resins.

[0127] In a further preferred embodiment, a further process step involves separating the solid components from the aqueous distribution mixture, which in one embodiment are essentially represented by the fibers and complex carbohydrates contained therein. This separation is particularly advantageous because the fibers, which are present in an aqueous distribution volume after separation according to the inventive process, exhibit a very high water-binding capacity and thereby enclose the dissolved proteins present in the aqueous solution, as well as other dissolved soluble compounds, within the three-dimensional structures formed by these fibers.Through condensation, aggregation, or complexation of the dissolved organic compounds occurring in such an aqueous distribution phase, the dissolved organic compounds contained in the fibers are either lost from recovery or the fibers laden with these compounds are aggregated or complexed with the condensates that form, thereby incorporating them into the recoverable fraction of condensed organic compounds. Therefore, separating the fibers while recovering the bound water content is a particularly preferred embodiment of the process. It has been found that this is also a crucial criterion for obtaining fractions of condensed soluble compounds that are completely or almost completely odorless and / or tasteless.It was further found that odor and / or flavor compounds, as well as other compounds such as colorants, which are undesirable in a food product, are present, particularly in the aqueous phase, bound to / into the fibers, and especially to / into the cellulose-based fibers. Therefore, when expanded cellulose-based fibers are encapsulated in condensates of organic compounds, the dissolved odor / flavor and / or colorants still present in the expanded cellulose-based fibers are also trapped within them. Even after dehydration of the condensates, they remain and are essentially responsible for an undesirable taste / odor and / or color. Consequently, a crucial criterion for obtaining a sensorially defect-free fraction of condensed and dehydrated soluble constituents of the starting material is the complete or near-complete separation of solid particles.It has been shown that this criterion is met when, after expansion / hydration of soluble compounds and fibers, as well as swelling of complex carbohydrates, the suspension of dissolved soluble compounds passes freely through a filter with a sieve size of 1000. Such solutions / suspensions are fiber-free or nearly fiber-free. Nearly fiber-free means > 98 wt%.

[0128] Surprisingly, it was demonstrated that complete or near-complete separation of solid particles present in the aqueous dispersion mixture is possible using filters with a significantly larger mesh size than the volumetric diameters determined for the particles and fibers in the dispersion mixture. Here, the term "solid particle" refers to three-dimensional structures that do not pass through a filter with a mesh size of 1000. This provides a very simple process technique for selectively separating all or nearly all solid particles from the dispersion mixture, which retains dissolved proteins and other soluble and dissolved compounds.The surprising and particularly advantageous effect resulting from the process according to the invention is the obtaining of an aqueous phase in which the main constituents of the plant starting material, which are present as solids, are no longer contained and which contains practically all of the soluble proteins that were present in the starting material in a dissolved and hydrated form. Therefore, in a preferred embodiment, the process according to the invention is carried out such that, following a distribution of the constituents in an aqueous distribution volume, an aqueous solution is obtained by a filtration process containing dissolved and hydrated proteins that is free of solids.

[0129] A preferred method is one for separating constituents of plant starting materials, in which the constituents of the plant starting material are separated using an aqueous solution containing dissolved amino acids and / or peptides, such that the solid components are completely or almost completely removed from dissolved proteins in an aqueous dispersion phase by means of filtration techniques. A particularly preferred embodiment of the method is one in which the dissolved amino acids and / or peptides are dissolved cationic amino acids and / or peptides.

[0130] A preferred method is one for separating constituents of plant starting materials, in which the constituents of the plant starting material are separated using an aqueous solution containing dissolved amino acids and / or peptides, and following distribution of the constituents in an aqueous distribution volume by a filtration process, an aqueous solution containing dissolved and hydrated proteins is obtained, which is free or nearly free of solid particles. A particularly preferred embodiment of the method is one in which the dissolved amino acids and / or peptides are dissolved cationic amino acids and / or peptides.

[0131] Suitable sieving devices are known from the prior art. Particularly suitable are sieving devices that simultaneously agitate the feed material / sieve residue, such as vibrating or gyratory sieves, since the accumulating sieve residue significantly impedes the passage of the aqueous phase. Other particularly suitable filtration techniques include, for example, arc sieves, belt filters, or screen decanters. Centrifugal separation methods, such as decanters, centrifuges, or separators, can also be used. A disadvantage of centrifugal separation is that higher molecular weight proteins can also be carried out with the solids in the gravity field, and further purification of the resulting solid mass is necessary to separate the dissolved soluble compounds carried out with the solids. This is preferably achieved using a suitable filtration technique.

[0132] The required sieve size for obtaining a filtrate of the aqueous solution of the distribution mixture, in which, after passing through one or more sieves, a solids content of < 2 wt%, more preferably < 1 wt%, and further preferably < 0.1 wt%, is present, must be determined for each individual application. A sieve size of > 50 μm, more preferably > 80 μm, and further preferably > 10 μm is preferred for one of the filters. The advantage of a sieve with a larger sieve size is that a significantly larger volume of the distribution solution can be filtered per unit time, with considerably lower material and process costs. In a preferred embodiment, fractional separation of solid constituents of the plant starting material is carried out, which can preferably be performed in a single process step. For example, complex carbohydrates (e.g., starch granules), which are partlyDimensions of 0.5–2 mm can be selectively separated using a pre-screen, as the fibers, depending on the starting material, pass completely through such a pre-screen with the volume flow. Therefore, the process is also suitable for the selective separation of complex carbohydrates, such as starch granules.

[0133] A preferred method is one for separating constituents of plant starting materials, in which the constituents of the plant starting material are separated using an aqueous solution containing dissolved amino acids and / or peptides, and following distribution of the constituents in an aqueous distribution volume, complex carbohydrates are selectively separated by filtration. A particularly preferred embodiment of the method is one in which the dissolved amino acids and / or peptides are dissolved cationic amino acids and / or peptides.

[0134] In a particularly advantageous embodiment, the filter residue obtained from this process step is dewatered. Methods for this are known in the prior art. Screen presses or screw presses, or centrifugal methods such as centrifuges or decanters, are particularly suitable. This allows the screen residue to be reduced to a residual moisture content of preferably < 80 wt%, more preferably < 60 wt%, and more preferably < 40 wt%. In a preferred embodiment of the process, the obtainable filtrate liquid is added to the filtrate liquid from the preceding filtration process. This advantageously enables the virtually loss-free retention of the process liquid of the distribution phase and the dissolved compounds contained therein.On the other hand, the solid constituents obtained in this way, which are almost free of soluble constituents of the plant starting material, can be obtained in a highly condensed and therefore transportable form. Furthermore, the further processing of the solid constituents is significantly simplified.Surprisingly, the odor / flavor and / or colorants contained in the distribution mixture phase obtained by dehydrating the separated solids, which is tested for the absence of particles larger than 1000 by means of a filter before being added to the previously separated distribution mixture phase, are not bound to or carried away with the obtainable condensates of the soluble constituents of the starting material when the soluble constituents of the distribution mixture phase are condensed according to the methods described herein, so that no odor / flavor and / or colorants are introduced into the condensed and dehydrated product phases of the soluble constituents.

[0135] This process step yields a fiber-free solution that preferably contains > 98 wt%, more preferably > 99 wt% and most preferably > 99.5 wt% of the mass of proteins originally present in the starting material.

[0136] The remaining process conditions can be freely chosen. The filtrate and the sieve or press residue are collected or discharged in separate and suitable containers.

[0137] In a further preferred embodiment, a further process step involves condensation and / or aggregation and / or complexation of the dissolved proteins and / or other dissolved compounds of the filtrate from the previous process step. The aim of this condensation process is to achieve a combination of dissolved or hydrated proteins and / or other dissolved compounds that enables the formation of a protein mass or product mass which can be separated using known separation techniques and obtained with minimal process water. Surprisingly, this aim can be achieved even with low concentrations of the condensing agents listed herein in dissolved form.Particularly suitable condensing agents include acids, preferably organic acids such as citric acid or lactic acid, as well as salts such as NaCl, complexing agents such as EDTA, and adsorbents. Soluble divalent cations, such as aluminum, calcium, and magnesium salts, are also preferred. Furthermore, ammonium compounds such as ammonium sulfate, as well as betaines, sulfobetaines, and imidazolines are suitable. Surfactants such as DMSO or DDT are also suitable. Silicates and carbonates are also suitable. Combinations of the condensing agents listed herein are also advantageous, such as a combination of citric acid and aluminum chloride. The use of aqueous solutions of the condensing agents is preferred.

[0138] The temperature at which condensation and / or aggregation and / or complexation occurs can, in principle, be freely chosen. A temperature between 6 and 90°C is preferred, more preferably between 10 and 60°C, and more preferably between 18 and 40°C. Maintaining a specific pH range is preferred; the optimum is determined by the selection or combination with the condensing agent. The optimal pH range can be determined using the method described above. The pH of the aqueous solution containing dissolved compounds, at which the condensation and / or aggregation and / or complexation of the dissolved proteins and / or other dissolved compounds according to the invention takes place, is preferably in a range above 5.5, more preferably above 6, and more preferably above 7.Furthermore, it is preferred to achieve a solubility minimum of the dissolved proteins of < 13, more preferably of < 12, even more preferably of < 11 and more preferably of < 10.

[0139] Surprisingly, the addition of carbonates led to the formation of condensates containing predominantly proteins, but also other compounds such as soluble carbohydrates. Solutions of sodium carbonate, sodium bicarbonate, or sodium bicarbonate added to the fiber-free filtrate solution containing dissolved compounds were more time-efficient in the condensation of these compounds than when these compounds were added to the process solution as solids. Surprisingly, a similar formation of predominantly protein-containing condensates was also possible with silicate compounds. Compounds such as sodium metasilicate and sodium orthosilicate proved particularly suitable. Aqueous solutions of these compounds are especially effective.

[0140] Furthermore, it was surprising that a combination of carbonate and silicate compounds increased the aggregation effect of the individual compounds, so that when combining the compound classes, the total amount of condensing agents used to achieve the same separation result was lower than when using only one of the compounds.

[0141] A preferred method involves the condensation / aggregation / complexation of a protein-containing aqueous phase by carbonates and / or silicates.

[0142] A preferred method for separating constituents of plant starting materials is one in which the constituents of the plant starting material are separated using an aqueous solution containing dissolved amino acids and / or peptides, and following distribution of the constituents in an aqueous distribution volume and separation of solid constituents, dissolved compounds are condensed using carbonates and / or silicates. A particularly preferred embodiment of the method is one in which the dissolved amino acids and / or peptides are dissolved cationic amino acids and / or peptides.

[0143] The suitability of the various possible condensing agents must be selected individually for each application. Suitability can be easily determined by a person skilled in the art by adding and mixing various condensing agents in increasing concentrations to samples of the fiber-free solution containing dissolved compounds, and in particular the dissolved proteins. Condensation can be observed with the naked eye after a short residence time. The appropriate concentration can be selected by centrifuging a sample solution in which condensation has occurred and treating the supernatant again with condensing agents. If no more visible condensates / aggregates / complexes form and / or can be separated, the solution contains < 6 wt%, preferably < 4 wt%, and most preferably < 2 wt% of the dissolved compounds or dissolved proteins to be condensed.

[0144] The additional quantity determined by this test procedure can be used for process execution and control. Conversely, the process can also be monitored using this test procedure. If condensates / aggregates / complexes are obtained upon addition of the identical and / or other condensing agents according to the invention to a supernatant obtained after centrifugation of the process liquid in which the condensation process has already taken place, the corresponding condensing agent(s) can then be added to the process liquid and mixed with it. In other words, the required quantity of condensing agent(s) has been added to the process liquid when, in the supernatant of a centrifuged sample of the process liquid, no condensation of dissolved or hydrated proteins occurs after the addition of a condensing agent.Surprisingly, this goal can be achieved with even low concentrations of the condensing agents listed herein. Particularly suitable condensing agents include acids, preferably organic acids such as citric acid or lactic acid, as well as salts such as NaCl, complexing agents such as EDTA, and adsorbents. Soluble divalent cations, such as aluminum, calcium, and magnesium salts, are also preferred. Furthermore, combinations of the condensing agents listed herein are advantageous, such as a combination of citric acid and aluminum chloride.

[0145] The preferred condensing agents are preferably completely dissolved in an aqueous medium. According to the invention, it is also possible to prepare two or more of the condensing agents together in a solution and add them to the solution containing dissolved compounds. Optionally, a buffer to adjust the pH of the solution can also be added. The suitable concentrations can be easily determined by a person skilled in the art and are based on the process conditions. The influence of other process parameters can also be investigated using the described techniques.

[0146] The preferably one or more dissolved condensing agents, which are added together and / or consecutively to the solution containing dissolved compounds, can be added continuously and / or discontinuously, from drop to jet. When applied as a solid, it is preferred to add the condensing agent(s) in powdered form.

[0147] In a preferred embodiment of the process, the added condensing agent(s) are mixed with a stirrer and gentle agitation of the process liquid. Thorough mixing must be ensured. The duration of the mixing is, in principle, freely selectable. In a preferred embodiment, this occurs only for the duration of the addition of one or more condensing agents or for a duration between 10 seconds and 5 minutes, more preferably between 20 seconds and 2 minutes.

[0148] Surprisingly, it was found that after the introduction of the condensing agents according to the invention, condensation and / or aggregation and / or complexation of previously dissolved compounds occurs within a few seconds to a few minutes, becoming visible to the naked eye as three-dimensional structures, while the previously cloudy aqueous solution simultaneously clarifies. It has been shown that the process can also be controlled based on the visual impression and the onset of clarification of the process solution. The resulting condensates increase in size over time, even without the addition of further condensing agents, and begin to sediment within a few minutes to a few hours, allowing them to be easily separated as a fraction from the then-clarified aqueous phase and further condensed.It was found that the amount of condensed organic compounds obtained during the condensation process decreases considerably when a greater quantity of condensing agents is added than is required for complete condensation. This is particularly true when the pH of the reaction solution is lowered below 5.0 by a condensing agent. Therefore, in a preferred embodiment of the process, the pH of the reaction mixture is continuously or discontinuously monitored during the addition of condensing agents. It is also preferred to implement process control in which a minimum pH value is specified. The pH value that is preferably not undercut is 4.5, more preferably 5.0, even more preferably 5.5, and further preferably 6.0.

[0149] In a preferred embodiment of the process described herein, the pH of the aqueous solutions is not reduced below 5 during the process. A key innovation of the process described herein is that the separation of the proteins does not require lowering the pH to values ​​below 4.5, ideally below 5, and that voluminous aggregates / condensates of dissolved proteins are formed, which are suspended and spontaneously sediment, even at a neutral pH. In contrast to a protein precipitate, the protein aggregates / condensates obtainable by the process described herein are completely soluble in neutral water, resulting in a milky suspension that can completely pass through an Iomi sieve. Protein precipitates, on the other hand, do not readily dissolve in water.For this reason, in CN 106 720 920 A, hydrolysis must be carried out in step 5 and homogenization of the resulting protein fraction in step 8 to obtain a protein isolate, since precipitation is carried out at a pH of 4.5 in step 2. It is known in the prior art that proteins that have passed through a pH range below 4 exhibit altered physicochemical properties and that such altered proteins are practically no longer capable of foaming.

[0150] As in other processes for protein recovery described in the prior art, in which dissolved proteins are separated from an aqueous phase by means of precipitation (acid and / or solvent precipitation), it was not taken into account that other compounds present in the aqueous suspension, such as soluble carbohydrates, dyes, flavorings, phenols, antinutritional compounds, or toxins, are also incorporated into the forming precipitate and cannot be washed out by simply rinsing the precipitate phase. This is the crucial difference in the process technology of the present application, since the completely dissolved proteins aggregate in a physiological form, retaining their hydration shell, thereby largely preventing the adhesion of other compounds, which are kept in solution by the amino acids / peptides present in the solution.Furthermore, the aggregated and condensed proteins can be rinsed with water to remove any remaining impurities present in the bound aqueous phase. Therefore, the protein fractions obtained with this process step are immediately usable as a product, e.g., for human consumption, and contain no sensorially perceptible flavorings or antinutritional compounds. Deodorization of the resulting protein fraction, as proposed in CN 106720920 A, is not required with the process technology proposed here, which is of particular importance for process economy.

[0151] In particular, dissolved and hydrated pectins can be incorporated into a protein precipitate phase by acid treatment. The process described herein enables the non-protein compounds dissolved by the amino acid / peptide solution to be selectively aggregated and separated following the aggregation / complexation and separation of the proteins by changing the pH of the solution and / or adding other aggregating agents. Furthermore, it is known in the prior art that protein precipitates obtained using an acid and / or an organic solvent essentially lose their water-binding capacity. This is also evident in CN 106720920 A, where, after acid precipitation, the moisture content of the obtainable protein fraction is less than or equal to 55%.The low water content of this protein phase indicates that coagulation has occurred; these proteins have essentially lost their water-binding capacity, which is accompanied by a loss of functional protein properties, such as foaming behavior and rheological properties (thickening effect), which are particularly important in protein concentrates. CN 106 720 920 A exemplifies the dilemma arising from a technique for solubility mediation using an alkaline solution and precipitation with an acid, as well as the subsequent need for neutralization (again using an alkaline solution). This process generates salt, which, if the process water phases are used in subsequent process iterations, negatively impacts the process and necessitates removal or the addition of fresh water. This has a significant impact on process economics.Consequently, in CN 106 720 920 A, neutralization is carried out after precipitation by adding an alkali to the acidic precipitate to adjust the pH of the protein sludge to between 6 and 8. The disadvantage of this step is that a solution volume 3 to 5 times the weight of the protein phase must be used, thus significantly increasing the energy input for drying the protein phase. Therefore, it is desirable to avoid neutralization so that the protein phase can either be dried or used directly after dehydration. CN 106 720 920 A demonstrates that flavorings and astringents cannot be sufficiently removed from the protein precipitate using the proposed aqueous method; therefore, a further step of steam deodorization is necessary to obtain a low-aromatic final product. This further reduces process efficiency.Also exemplary of the prior art, CN 106 720 920 A specifies the necessity of a spray-drying process step to produce a protein preparation that is at least partially soluble. With the process described therein, spray drying, which has a very high energy requirement, is not necessary. Furthermore, it has been found that sulfur-containing amino acids or peptides, due to their known reactivity with proteins, lead to undesirable product properties in the available proteins (su), so that sulfur-containing amino acids or peptides should not be present, or only in a small proportion, in any of the aqueous solutions according to the invention. European patent application EP 2 404 509 AI discloses a process for extracting protein from fresh grape seeds. This requires the use of a buffer containing glycine, soda, and hydrogen chloride or sodium hydroxide with a pH between 8.5 and 10.5.The minimum ratio between the extraction solution and the solid is 1:5, and the minimum time for this step is 3 hours. Precipitation is achieved with acid at a pH of 3. Soaking for hydration is not recommended in order to achieve efficient process economy through a lower water volume ratio. Furthermore, the product properties of the proteins are not mentioned.

[0152] Liu ui-Lin et al. (Food Analytical Methods, Springer New York LLC, US, Vol. 10, No. 6, November 21, 2016, pages 1169-1680) use an alcohol for precipitation. The method uses microwave heating and ultrasound and is energy-intensive, and therefore not designed to be process-economical.

[0153] In a particularly preferred embodiment of the method according to the invention, step 4 of the method is carried out without the use of organic solvents.

[0154] In a particularly preferred embodiment, a settling period is observed after the addition of one or more condensing agents, during which no or only minimal mixing of the mixture occurs. The required duration of the condensation phase can be determined analogously; preferably, it is between 5 minutes and 10 hours, more preferably between 10 minutes and 5 hours, and even more preferably between 15 minutes and 2 hours. If the settling period is to be reduced to a minimum, the sufficiently minimum duration after the addition of the condensing agent can be easily determined by centrifuging a sample and verifying, analogously to the above description, the completeness of the condensation and / or aggregation and / or complexation achieved by the condensing agent(s).

[0155] In a preferred embodiment of the process, the condensed / aggregated / complexed soluble compounds / proteins are made recoverable in the form of a sediment. Preferably, the sediment phase is discharged via a bottom outlet and fed into a further process step. The condensation phase preferably takes place at ambient temperatures, ideally within a temperature range of 15 to 40°C. In further advantageous embodiments, this phase takes place at a lower or higher temperature. A temperature range of 5 to 15°C on the one hand and 40 to 80°C on the other is preferred. Selecting a lower temperature can be advantageous, for example, in the recovery of thermolabile compounds. Selecting a high temperature, e.g., 60°C, can be chosen, for example, to kill microorganisms, e.g., by pasteurization, in the case of microbial contamination of the starting material.On the other hand, heating can also inactivate allergens, certain toxins, and antinutritional compounds.

[0156] A preferred method is for obtaining a protein-containing sediment consisting of condensed / aggregated / complexed proteins.

[0157] Surprisingly, it was found that odor and flavor compounds, which are also dissolved by the digestion process and are present in solution in the distribution mixture, are not adsorbed onto or complexed with the protein condensate(s) / agglomerate(s) / complex(s) forming by the inventive processes for condensing / aggregating / complexing the proteins. Odor and flavor compounds still present in the water fraction bound to or enclosed by the protein fraction are separated from the protein fraction, along with the water in which they are dissolved, by one of the processes described herein. If necessary, the produced protein fraction can be washed by one of the sidestream processes described herein.Furthermore, it was surprising that toxins and hazardous substances that may be contained in plant press residues or milled products, such as erucic acid, phorbol esters, or synthetic pesticides, are present in dissolved form in the distribution solution, separated from proteins. Under the process conditions according to the invention, which are used for the condensation of the dissolved compounds / proteins, the solubility of dissolved compounds that do not correspond to a protein, a soluble carbohydrate, a phospholipid, or a glycoglycerolipid remains intact. Thus, with a selection of the condensing agent according to the invention, no condensation / aggregation / complexation of toxins or hazardous substances, hereinafter also referred to as hazardous substances, occurred, and no release or...The introduction of such compounds into the condensates / aggregates / complexes of the condensed soluble compounds / protein fraction or into the recoverable protein fractions occurred. In a preferred embodiment, the solubility of toxins and harmful compounds contained in plant press residues or milled products can be maintained or increased, for example, by adding one or more classes of compounds, such as alcohols, esters, or ethers, during this and / or further process steps.

[0158] A preferred method is one in which the solubility of toxins and hazardous substances in an aqueous protein solution is maintained or increased following the separation of the constituents of the plant starting material by means of an aqueous solution containing dissolved amino acids and / or peptides. A particularly preferred embodiment of the method is one in which the dissolved amino acids and / or peptides are dissolved cationic amino acids and / or peptides.

[0159] In a further preferred embodiment, a further process step involves dehydrating the condensed / aggregated / complexed soluble compounds / proteins by removing water. This can be achieved using techniques known to those skilled in the art. Centrifugal processes are particularly suitable, as is the use of a decanter. The water removal enables the recovery of a dehydrated mass of the soluble compounds or the obtaining of a protein mass that is preferably free-flowing, more preferably a spreadable mass, and most preferably a dimensionally stable mass of condensed and dehydrated soluble constituents of the starting material. Correspondingly preferred is a protein mass with a residual moisture content of < 90 wt%, more preferably < 80 wt%, more preferably < 70 wt%, and even more preferably < 60 wt%, and still more preferably < 40 wt%.The desired residual moisture content can vary for different applications, so the parameters of the separation device must be adjusted accordingly. In principle, the separation process aims for the highest possible separation efficiency. When using a decanter, separation preferably takes place with > 2,000 g, more preferably with > 3,000 g, and further preferably with > 3,500 g. The residence time in a decanter is preferably > 10 seconds, more preferably > 20 seconds, and further preferably > 30 seconds. Separation at ambient temperatures between 15 and 40°C is preferred. In other advantageous embodiments, a lower or higher temperature can be selected, in the range of 5 to 15°C or between 40 and 80°C, respectively.

[0160] Surprisingly, it was found that the compounds condensed using the process technology according to the invention, and in particular condensed proteins, form volumes that allow dehydration to be carried out using filtration techniques. The soluble and dissolved compounds present before condensation / agglomeration / complexation, which freely passed through a sieve with a mesh size of 1 / 3, had, in their condensed form as they were at the end of the condensation process step, a volume that no longer permitted free passage through a filter with a mesh size of 200 1 / 3; the filtrate contained practically no proteins. Thus, dehydration of condensed soluble proteins and / or other condensed constituents can be carried out with great advantage by means of filtration, resulting in no or virtually no loss of condensed soluble compounds / proteins.Furthermore, it has been shown that bound water can be separated from the proteins condensed according to the invention by pressing them on or in a filter fabric, thus maintaining the previously specified residual moisture content. Therefore, the process according to the invention is particularly suitable for obtaining a dehydrated protein phase with a residual moisture content of < 90 wt%, more preferably < 80 wt%, further preferably < 70 wt%, and even more preferably < 60 wt%, and still more preferably < 40 wt%, obtainable by means of a filtration technique for condensed proteins. Filtration methods are known to those skilled in the art. Belt filters or chamber filters, or filter presses and chamber filter presses, as well as vacuum belt filters, are preferred.

[0161] A preferred method is for obtaining dehydrated proteins which, following separation of the constituents of the biogenic starting material using an aqueous solution containing dissolved amino acids and / or peptides, can be obtained by filtration of condensed proteins. A particularly preferred embodiment of the method is one in which the dissolved amino acids and / or peptides are dissolved cationic amino acids and / or peptides.

[0162] Surprisingly, it was found that dehydrated proteins obtained in this way are completely or almost completely odorless and / or tasteless, dissolve very quickly in water, and release no or practically no dyes into the aqueous medium. "Almost completely" means > 98%.

[0163] A preferred method is for obtaining dehydrated proteins obtained after separation of the constituents of the biogenic starting material using an aqueous solution containing dissolved amino acids and / or peptides. These proteins are completely or nearly completely odorless and / or tasteless, dissolve very rapidly in water, and release no or practically no dyes into the aqueous medium. A particularly preferred embodiment of the method is one in which the dissolved amino acids and / or peptides are dissolved cationic amino acids and / or peptides.

[0164] Furthermore, it was found that such dehydrated proteins can be further purified very easily and gently in the resulting dehydrated form. In a preferred embodiment, the dehydrated protein mass is applied to a filter belt with a specific thickness and, with or without the addition of another filter, is perfused with a liquid and / or steam and / or gas from below or above. The subsequent drying can be carried out as before or using a different drying method. In another embodiment, the resulting dehydrated soluble constituents / proteins undergo further processing in a sidestream process, preferably involving purification. Processing the condensed and dehydrated substituents in a sidestream process is preferred.

[0165] Surprisingly, a mass balance analysis of the products obtained from biogenic starting materials revealed that the proteins contained therein were separated at > 95 wt% and obtained in dehydrated form. Therefore, a process is preferred in which preferably > 95 wt%, more preferably > 97 wt%, and further preferably > 98.5 wt% of the proteins present in a plant starting material are separated and dehydrated.

[0166] A preferred method is one in which > 95 wt% of the proteins contained in a biogenic starting material are obtained in the form of dehydrated proteins following separation of the constituents of the biogenic starting material using an aqueous solution containing dissolved amino acids and / or peptides. A particularly preferred embodiment of the method is one in which the dissolved amino acids and / or peptides are dissolved cationic amino acids and / or peptides.

[0167] The obtainable dehydrated soluble constituents / proteins can be used directly in an application, stored, or further processed in their obtained form. Storage in suitable containers is preferably carried out under refrigerated conditions. Surprisingly, the protein condensates produced according to the invention were found to exhibit very good storage stability. For example, no microbial colonization was observed in a protein condensate obtained from rapeseed press cake with a residual moisture content of 50% by weight after 14 days of storage at 6°C. Furthermore, it was shown that the initial neutrality of taste and odor remained unchanged. The dehydrated proteins also retained their excellent solubility in water.

[0168] In a preferred embodiment of the process, the dehydrated proteins, either in the form obtained or after suspension in water or a liquid solution, are subjected to a drying process. Spray drying and freeze-drying are preferred. This advantageously allows the production of powdered protein mixtures, protein concentrates, or protein isolates. However, other prior art drying processes and techniques can also be used.

[0169] A preferred method is a process for producing dehydrated proteins with high storage stability, obtainable by separating the constituents of the biogenic starting material using an aqueous solution containing dissolved amino acids and / or peptides. A particularly preferred embodiment of the process is one in which the dissolved amino acids and / or peptides are dissolved cationic amino acids and / or peptides.

[0170] Depending on the starting material used and the process parameters, large quantities of the clarified process water phase from process step 5) are generated, particularly in large-scale industrial production. Since this phase still contains significant amounts, sometimes exceeding 100 mmol / l, of the dissolved amino acids and / or peptides used, reuse of the clarified process water phase is necessary for an economically efficient process. It was found that the condensing agents also contained in this phase, which were not discharged with the product of process step 5), make the reuse of the clarified water phase from process step 5) difficult or even impossible in the subsequent process steps of the main process, as this leads to condensates, e.g., of proteins, in process steps 2b) and 2c).2) which were then present in the filter residue in process step 3), thus leading to product loss and increased purification efforts for the products obtainable from this process step. Surprisingly, it was found that the use of the clarified process water phase from process step 5) can be particularly advantageous for removing dissolved soluble proteins that are still present in the bound water phase of the cellulose-based fibers and lignin-rich shell components obtainable in the filter residue of process step 3).It was demonstrated that rinsing and cleaning the separable solids from process step 3 with the clarified process water phase from process step 5 resulted in a highly effective removal of dissolved organic compounds still present in the solids. These organic compounds then migrate into the enriched process water and remain there after separation of the solids. Surprisingly, the effectiveness of removing dissolved compounds still present in the filter residue from process step 3 using the clarified process water phase from process step 5 was significantly higher than when the filter residue was rinsed and cleaned with fresh water.Surprisingly, this also resulted in a significant reduction in the concentration of complexing agents in the clarified process water phase of process step 5). After rinsing and purifying the solids obtained from process step 3), their concentration was considerably lower than before. It was found that the remaining concentrations of condensing agents in the resulting process water phase, after separation of the purified solids, did not lead to aggregation of soluble organic compounds when introduced into process steps 2a), 2b), or 2) of the main process.Furthermore, it was found that the concentration of dissolved amino acids and / or peptides used to separate the constituents of the starting material was higher in the process water phase after rinsing and cleaning the filter residues of process step 3) in a bypass process path than in the clarified process water phase of process step 5). This advantageously allows the recovery of compounds used to separate the constituents of the starting material and simultaneously produces a process water phase suitable for separating the constituents of the starting material.Therefore, recirculating the process water phase obtained from process step 5) via a sidestream process for rinsing and purifying cellulose-based fibers and / or lignin-rich shell components is a particularly preferred process design. This allows for highly efficient recycling of the compounds used for separating constituents of the starting material and the condensing agents, while optimizing product production. Furthermore, this process design significantly reduces the process costs associated with rinsing and purifying the cellulose-based fibers and / or lignin-rich shell components in the sidestream process.Thus, a process-economical method for separating constituents of a starting material can be provided by recirculating the process water phases between a main process and a sidestream process.

[0171] A preferred method and process control for the process-economical separation of constituents of a plant starting material is preferred.

[0172] If one of the bypass process processes according to the invention is not carried out, or not carried out directly, in a further preferred embodiment, the clarified aqueous process water phase(s) obtained after the separation of the condensates / aggregates / complexes of process step 5) and / or the separated aqueous phase obtained during the dehydration of the condensed condensates / aggregates / complexes in a further bypass process step can be purified. It has been found that the removal of condensing agents still present in the clarified process water phase of process step 5) can be achieved by various methods. For example, ionized calcium can be precipitated by titration with phosphoric acid and then removed from the aqueous medium by filtration.On the other hand, a change in the process water pH range to values ​​below 10 caused by the use of an acid as a condensing agent can be adjusted to the required pH level by adding a suitable base that does not impede the process flow when the purified process water is reused, e.g., using urea. Other compounds can be reduced or removed by adsorptive processes or within the framework of a dialysis process, e.g., by electrodialysis.

[0173] In a process according to the invention, the clarified process water phases obtained from process step 5 contain only small amounts of suspended solids and are already clear or almost clear. Suspended solids and / or turbidity can be easily removed using prior art methods. Fine and ultrafine filters from the prior art are particularly suitable for this purpose. This allows a turbidity-free water phase to be obtained. Furthermore, dissolved electrolytes, such as sodium, potassium, calcium, chloride, iron, copper, etc., may be present in varying amounts. If necessary, these can be removed using prior art methods, for example, by electrodialysis or ion exchange compounds. Additionally, toxins and / or hazardous compounds may be present in the process solution.Prior art methods exist for removing such compounds, mostly organic, from an aqueous medium. Adsorptive techniques, such as column chromatography or activated carbon filtration, are among those suitable. If thermolabile compounds posing a risk to human health are present, the process water phase can also be heated to a temperature and for a duration sufficient to inactivate or decompose these compounds. Advantageously, the aforementioned optional purification steps do not remove any dissolved amino acids and / or peptides remaining in the process water phase(s).Using one or more of these process embodiments for the purification of process water phases, which can be carried out sequentially or in parallel in any order, a purified process water phase is obtained that contains dissolved amino acids and / or peptides suitable for the separation of constituents of a biogenic starting material and in which a low concentration of condensing agents is present and which does not interfere with the reuse of the purified process water phase, as well as a sufficient reduction or elimination of toxic and harmful compounds.

[0174] In a preferred embodiment, the process water phase obtained from the rinsing and cleaning of filter residues of process step 3 in a sidestream process or other sidestream process is subjected to one of the purification process steps according to the invention.

[0175] Thus, by selecting one or more of the optional process steps of process step 6) in a process-adaptive manner, the process water phase flow can be designed in a highly advantageous way to ensure optimal value creation of the process and guarantee the reusability of the process water phases. The individual optional process implementations can be summarized into the following optional process sub-steps:

[0176] 6.1) Provision of process water for a sidestream process 6.2) Return and provision of the used process water phase from the

[0177] Sidestream process of step 6.1)

[0178] 6.3) Purification of the process water phase, obtainable from step 5) and / or 6.2) and / or a sidestream process

[0179] 6.4) Provision of a clarified and purified process water phase,

[0180] This results in various possible combinations for the execution of process step 6), which are characterized by the number and sequence of the optional process steps, such as: 6.1 then 6.2 then 6.3 then 6.4 or 6.3 then 6.4 or 6.3 then 6.1 then 6.2 then 6.4 or 6.2 then 6.3 then 6.1. The aqueous process water phases from different process steps of the main and / or sidestream process can also be combined and reused in one of the process steps or subjected to purification using the purification methods listed herein.

[0181] Therefore, it is particularly advantageous to feed the clarified and purified process water phase into one of the process steps for separating constituents of plant starting materials in a subsequent process run. This makes the process water phase obtained from this process step suitable for reuse as a process water phase.

[0182] A preferred method is a process for separating constituents of plant starting materials, in which the constituents of the biogenic starting material are separated using an aqueous solution containing dissolved amino acids and / or peptides, and following distribution of the constituents in an aqueous distribution volume and subsequent separation of solid and condensed soluble constituents, a clarified process water phase is obtained, which is purified and then reused for one of the process steps. A particularly preferred embodiment of the process is one in which the dissolved amino acids and / or peptides are dissolved cationic amino acids and / or peptides.A preferred method is for separating constituents of plant starting materials, in which the constituents of the biogenic starting material are separated using an aqueous solution containing dissolved amino acids and / or peptides. Following distribution of the constituents in an aqueous distribution volume and subsequent separation of solid and condensed soluble constituents, a clarified process water phase is obtained. This clarified phase is used for rinsing / purification in a sidestream process, subsequently purified, and then reintroduced into one of the main process steps. A particularly preferred embodiment of the method is one in which the dissolved amino acids and / or peptides are dissolved cationic amino acids and / or peptides.

[0183] A preferred method involves reusing the clarified and purified process water phase to separate the constituents of a biogenic starting material using an aqueous solution containing dissolved amino acids and / or peptides. A particularly preferred embodiment of the method is one in which the dissolved amino acids and / or peptides are dissolved cationic amino acids and / or peptides.

[0184] Preferably, the clarified and / or clarified and purified process water phase contains < 3 wt%, preferably < 1.5 wt%, and most preferably < 0.5 wt% of organic compounds. Preferably, it is a clear solution with no or only a minimal amount of suspended solids. Preferably, the process enables wastewater-free operation. Preferably, the clarified and / or clarified and purified process water phase is stored, temporarily stored, or immediately reused in a suitable container. If storage is necessary, providing suitable conditions is advantageous. In one embodiment, the clarified and / or clarified and purified process water phase is cooled during storage. Cooling to < 10°C is preferred, more preferably to < 8°C, and further preferably to < 6°C.The shelf life of the clarified and / or clarified and purified process water phase is preferably > 7 days, more preferably > 14 days, and further preferably > 4 weeks. In this context, "shelf life" means the absence of potentially harmful germs, pathogens, or toxins in concentrations that pose a health risk. In other words, a shelf-stable clarified and / or clarified and purified process water phase suitable for reuse is safe for use in food production. The clarified process water phase can be reintroduced into the process at various process steps via a suitable pumping and piping system.

[0185] In a preferred embodiment, a clarified and / or clarified and purified process water phase, obtainable from process step 6), is reused. It has been shown that, particularly when using the process water phase from process step 6) (provision of a clarified and purified process water phase), the amount of amino acids and / or peptides used for the purpose of separating constituents of the starting material can be reduced compared to using a fresh water phase in process steps 2a) and / or 2b) or 2). Thus, very good dissolution of the soluble constituents of the starting material by the amino acids and / or peptides according to the invention, which were present in both a clarified and a clarified and purified process water phase from process step 6), was observed.Furthermore, the distribution result is identical when using the process water phase of process step 6) (recirculation and provision of the used process water phase from the bypass process) as when using the same volume of fresh water for the distribution of the separated constituents of the starting material in process steps 2b) and 2). It was also shown that a larger quantity (dry mass) of obtainable condensed / aggregated / complexed soluble constituents is obtained than when fresh water is used for the same process. This was particularly true for the production of a protein fraction. Furthermore, a measurable difference was observed in the products produced.Thus, there is excellent reusability of a clarified and / or clarified and purified process water phase for a separation and recovery of constituents of a starting material in one of the process steps according to the invention.

[0186] A preferred method for separating organic constituents from plant starting materials is one in which a clarified and / or clarified and purified process water phase from the main and / or sidestream process steps is reused for the process. The preferred method is thus characterized by the following process steps:

[0187] 1) Providing raw materials,

[0188] 2a) Mixing the starting material from step 1) with an aqueous solution containing dissolved amino acids and / or peptides to separate the constituents of the starting material,

[0189] 2b) Provision of an aqueous distribution volume and distribution of the separated / released

[0190] Constituents of the mixture from step 2a),

[0191] 3) Separation of solid particles from the dispersion mixture of step 2b) to obtain a fiber-free aqueous solution of dissolved constituents of the starting material, 4) Condensation / aggregation / complexation of the dissolved constituents of the aqueous

[0192] Solution of step 3) to obtain an aqueous phase containing condensed soluble constituents of the starting material,

[0193] 5) Separation and dehydration of the condensed soluble constituents of the starting material from step 4) and obtaining a dehydrated condensate from step 4) as well as a clarified process water phase,

[0194] 6) Use of the clarified process water phase from step 5) for one or more of the optional process steps:

[0195] 6.1) Provision of a process water phase for a sidestream process;

[0196] 6.2) Recycling of the process water phase from step 6.1) obtained from a sidestream process and provision of the used process water phase from a

[0197] Bypass process

[0198] 6.3) Purification of the process water phase obtained from process steps 5) and / or 6.2

[0199] 6.4) Provision of a clarified and purified process water phase,

[0200] 7) Reuse of clarified and / or clarified and purified process water phase, wherein the clarified and / or clarified and purified process water phase of step 7) is obtained from one or more processes of step 6) and the reuse takes place in step 2a) and / or 2b) or a sidestream process.

[0201] In a further variant of the process, process steps 2a) and 2b) are carried out in a single process step, process step 2. For this purpose, the plant starting material from process step 1) is brought directly into contact with a solution volume that, firstly, contains a sufficient concentration of dissolved amino acids and / or peptides, wherein the dissolved amino acids and / or peptides are preferably dissolved cationic amino acids and / or peptides to ensure the separation of the constituents of the biogenic starting material according to the invention, and secondly, has a sufficiently large water distribution volume to enable the distribution of the constituents of the starting material according to the invention. The concentration of the dissolved amino acids and / or peptides, as well as the volume or ratio to the starting material, can be determined using the methods described herein.A concentration of dissolved amino acids and / or peptides between 10 mmol / L and 800 mmol / L is advantageous. The other applicable process parameters apply analogously to those described in individual process steps 2a) and 2b). Following process step 2), the process can be continued with process step 3) as described herein.

[0202] A preferred method is one characterized by the following process steps:

[0203] 1) Provision of plant-based starting materials,

[0204] 2) Mixing the plant starting material from step 1) with an aqueous solution containing dissolved amino acids and / or peptides to separate the constituents of the plant starting material, as well as with an aqueous distribution volume and distribution of the separated constituents.

[0205] 3) Separation of solid particles from the dispersion mixture of step 2b) to obtain a fiber-free aqueous solution of dissolved constituents of the starting material, 4) Condensation / aggregation / complexation of the dissolved constituents of the aqueous solution of step 3) to obtain an aqueous phase containing condensed soluble constituents of the starting material,

[0206] 5) Separation and dehydration of the condensed soluble constituents of the

[0207] Starting material of step 4) and obtaining a dehydrated condensate from step 4) as well as a clarified process water phase,

[0208] 6) Use of the clarified process water phase from step 5) for one or more of the optional process steps:

[0209] 6.1) Provision of a process water phase for a sidestream process;

[0210] 6.2) Recycling of the process water phase from step 6.1) obtained from a sidestream process and provision of the used process water phase from a sidestream process

[0211] 6.3) Purification of the process water phase obtainable from process steps 5) and / or 6.2 6.4) Provision of a clarified and purified process water phase, 7) Reuse of clarified and / or clarified and purified process water phase, wherein the clarified and / or clarified and purified process water phase of step 7) is obtained from one or more processes of steps 6) and the reuse takes place in step 2) or a bypass process.

[0212] The method according to the invention additionally enables numerous method variants, which allow for further highly advantageous embodiments.

[0213] Procedure variants of procedure step 1

[0214] In a preferred process embodiment, the plant-based starting material, and especially in the case of press residues or milled products of plant seeds, is provided under special conditions. In one embodiment, the filling of the container (and possibly also in subsequent process steps) takes place under protective or inert gas conditions. This prevents, for example, oxidative changes that occur under ambient air conditions. This can be of crucial importance, particularly for the product properties that can be maintained. In the case of such a design, the containers of the subsequent process steps must also be equipped / designed accordingly.

[0215] In another embodiment of the process, the container(s) of step 1 and the subsequent process steps are explosion-proof.

[0216] A preferred method is one for separating constituents of plant starting materials, in which the plant starting materials are provided in a suitable container.

[0217] A preferred method is one for separating constituents of plant starting materials, wherein the plant starting materials are provided in a suitable container and device by and with which a protective / inert gas atmosphere can be produced and maintained.

[0218] Procedural variants of procedural steps 2), or 2a) and 2b)

[0219] In one embodiment, one or more further compounds are added before, during, or after the biogenic starting material of step 1 is mixed with an aqueous solution containing dissolved amino acids and / or peptides. In a preferred embodiment, this allows, in particular, the lipophilic constituents of the biogenic starting material to be separated from the amphiphilic and hydrophilic constituents of the biogenic starting material and subsequently separated.

[0220] For example, an alcohol can be added to dissolve and / or keep in solution components of the press residue or a milled product during subsequent process steps. Suitable alcohols include, for example, isopropanolol, methanol, ethanol, or octanol. The addition of a small volume fraction of one or more alcohols is preferred. A volume fraction of 0.1 to 30 vol% is preferred, more so 0.5 to 20 vol%, further preferred between 0.8 and 10 vol%, and even more preferably between 1 and 8 vol%. This allows compounds, such as dye compounds, to be detached from other constituents of the starting material and / or kept in solution. In a preferred process embodiment, one or more alcohols are added to the process mixture in an optional process step (2a) and / or (2bl).

[0221] In one embodiment of the process, oxidative processes that can occur in one of the aqueous media in which the constituents of the starting material are dissolved are reduced or prevented by antioxidants. The optional process step(s) 2a2) and / or 2a2) in which one or more antioxidants are added to the process liquid is / are preferred. This is particularly advantageous for protecting, for example, polyphenols, vitamins, or dyes from oxidation that may occur during the process and for preserving them in a non-oxidized form.

[0222] A preferred method is one in which one or more organic and / or inorganic compounds are added in process step 2a) and / or 2b) to the optional process steps 2al) 2a2) 2bl) or 2b2) to dissolve, keep soluble and / or protect organic compounds of the starting material.

[0223] A preferred method is one in which the at least one compound added in process step 2al), 2a2), 2bl) or 2b2) is an alcohol and / or an antioxidant.

[0224] In a further preferred embodiment, lipophilic compounds and / or organic solvents are added in one or both of the optional process steps 2a3) and / or 2b3). This can be particularly advantageous to enable the formation of a separate organic phase / lipid phase in subsequent process steps and / or to facilitate the dissolution, especially of neutral lipids. Suitable solvents include, among others, hexane, pentane, octane, methyl esters, triglycerides, paraffins, or silicone oils. Thorough mixing of the added compounds and solutions with the reaction mixture is preferred.

[0225] It has been shown that lipids, and in particular neutral lipids, do not bind to the hydrated constituents of the starting material present in the partition mixture and are detached by hydrated compounds. This effect can be used to particularly advantageous effect to selectively or non-selectively combine lipids and / or lipophilic compounds present in the partition mixture into a lipid phase. The lipids forming the lipid phase may already be present in the biogenic starting materials and / or be added in one of the process steps. The use of lipid mixtures and / or combinations with organic solvents is advantageous. It is particularly preferred to use a preferably already purified triglyceride phase obtained from the pressing of the starting material.The formation of a lipid phase allows micellar lipids and lipophilic compounds to be incorporated into the lipid phase in a particularly advantageous manner, making them very easy to separate from the aqueous phase and potentially use them further. This applies, among other things, to the extraction of sinapine, tocopherols, fat-soluble vitamins, or dyes. The lipid phase, which preferably forms spontaneously, precipitates on the surface of the aqueous medium and can thus be separated from it using known separation techniques, such as a skimmer.

[0226] In further preferred embodiments, lipophilic compounds can be added in optional process steps 2a3) and / or 2b3), which advantageously enable the formation of a lipid phase. It has been found that, for example, the addition of a cooking oil results in the separation of a lipid phase on the aqueous process phases, which then floats to the surface. It has been found that lipids present as constituents in the biogenic starting material are also present in this phase. A mixture of the aqueous process solution(s) with the lipophilic compounds is preferred. The separation of the lipophilic phase can be carried out by a settling process or a centrifugal process. The separation of a separate lipid phase preferably takes place at the end of process step 2, i.e., before process step 3.

[0227] A preferred method is for separating lipophilic constituents of plant starting materials, in which lipophilic compounds are added in process step 2a3) and / or 2b3) and mixed with the process mixture.

[0228] A preferred method is one in which, in process step 2a3) and / or 2b3), a neutral lipid and / or organic lipophilic solvent is / are added and mixed with the aqueous mixture.

[0229] A preferred method is one in which a lipid phase is formed, through which and with which lipophilic compounds can be removed and recovered from the distribution mixture.

[0230] A preferred method is one in which a lipid phase that forms or can form during process step 2b) or 2) is removed from the aqueous distribution solution before carrying out process step 3).

[0231] Procedure variants of procedure step 2b)

[0232] In one embodiment of process step 2b), process step 2b4) involves the removal of hydrophilic and / or amphiphilic compounds from the distribution mixture. This can be achieved through adsorption / complexation / filtration / dialysis / hydrolysis processes. For example, dyes and odorants can be bound / immobilized to various adsorbates, such as activated carbon or zeolites. Furthermore, enzymes can be used, for example, to deactivate antinutritive compounds. Toxins can also be complexed, for example, by chelating agents. Additionally, dialysis processes can be used to reduce ions and small molecules, such as toxins.

[0233] A preferred method is one in which hydrophilic and / or amphiphilic compounds are removed from a distribution mixture by means of adsorption / complexation / filtration / dialysis / hydrolysis processes.

[0234] A preferred method is one in which, in process step 2b4), adsorption / complexation / filtration / dialysis / hydrolysis of hydrophilic and / or amphiphilic compounds takes place.

[0235] Procedure variants of procedure step 3

[0236] In one embodiment of the process, the solid constituents of the starting material undergo differential filtration. In a preferred embodiment, filters with different screen sizes are used for this purpose, with larger particles being filtered out first and smaller particles being filtered out in one or more further filtration stages. Vibrating or rotary vibrating screens are preferably used for differential separation according to particle size. In addition to size-selective separation of the particulate components of the distribution mixture, separation according to particle density can also be carried out. Methods for this are known from the prior art, such as the use of hydrocyclones. This allows the separation of fibrous materials, as well as insoluble and complex carbohydrates, into individual fractions that can then be used for material recovery, in a particularly advantageous manner. The separation of the fibrous materials, or...The optional process step 3a) can be used to separate the particulate components present in the distribution mixture according to their size and / or density (specific gravity) by means of sieving techniques and / or eddy current processes, as described in more detail below.

[0237] A preferred method is one in which, in process step 3a), the dissolved fibrous materials and particulate components can be separated according to their size and / or specific gravity using differential sieving and / or eddy current techniques and subsequently used.

[0238] In a preferred variant of process step 3, process step 3b) involves the separation of microcomplexes / particles following the separation of fibers. Microcomplexes / particles are defined as aggregates with a size between 0.5 and 20 μm. These aggregates consist largely of carbohydrates or fibers. The removal of these aggregates can be achieved using centrifugal methods or filtration techniques. By selecting appropriate parameters, the microcomplexes can be separated without protein loss.

[0239] A preferred method is one in which, in process step 3b), small complexes / particles are separated without loss of dissolved proteins.

[0240] A method is particularly preferred in which, in step 3), the separation of the solid materials from the distribution mixture of step 2b) is carried out by means of filtration or sedimentation.

[0241] Procedure variants of procedure step 4

[0242] In a preferred embodiment, in step 4) compounds comprising carbohydrates, phospholipids, glycolipids, glycoglycerolipids, antioxidants, vitamins are added to and / or already contained in the aqueous solution of step 3), which are bound to the dissolved proteins and aggregated together with the proteins.

[0243] In a further preferred embodiment, the method according to the invention comprises step 4a) after step 4) and before step 5).

[0244] Separation of the aggregated proteins and subsequent addition of one or more further aggregating agent(s) to aggregate the dissolved carbohydrates according to step 3).

[0245] In a further preferred embodiment, in process step 4a), before, during, or after the initiation of the condensation / aggregation / complexation of the dissolved soluble constituents, such as the proteins, one or more compounds from the fiber-free, protein-containing solution are added to bind / complex with the proteins and thus incorporate them into the recoverable protein fraction. In a particularly preferred embodiment, in process step 4a), compounds are added to the aqueous, fiber-free, protein-containing solution, preferably comprising phospholipids, glycolipids, carboxylic acids, antioxidants, vitamins, and / or carbohydrates.In a further particularly preferred embodiment, in process step 4a), compounds are added to the aqueous, fiber-free solution containing protein. These compounds preferably comprise phospholipids, glycolipids, carboxylic acids, antioxidants, vitamins, and / or carbohydrates, and / or are already contained therein. They bind to the dissolved proteins and aggregate together with the proteins. In a process variant, this process step can also be carried out in process step 2 as process step 2b5). In one embodiment of the process, the dissolved compounds or classes of compounds present in the fiber-free aqueous solution of process step 4 are differentially aggregated / complexed with the dissolved proteins and / or other dissolved compounds.This can be achieved by adding one or more compounds to the fiber-free protein solution in process step 4b) before, during, or after the initiation of condensation / aggregation / complexation of the proteins and / or other solutes. These compounds decrease the solubility of non-protein compounds. For example, carbonates can be added to alter the solubility of glycolipids, or chelating agents can be added to alter the solubility of phospholipids. Other compounds can also be used, such as NaSO4, ammonium sulfate, CaCl2, MgCl2, acetates, tartrates, or silicates. This reduces the solubility of one or more solutes, causing them to adhere to / complex with the proteins.This preferably occurs during the condensation / aggregation / complexation of the proteins in this process step. This allows the compounds whose solubility in the reaction mixture is reduced to be incorporated into the forming protein condensates / aggregates / complexes, making them recoverable in this form. This process preferably takes place at a neutral pH, ideally between 6 and 8. Adjusting the reaction temperature, which may differ from that preferred when condensing agents are added consecutively, is also suitable for influencing the solubility.

[0246] A preferred method is one in which, in process step 4a), one or more compounds are added to the aqueous process solution to bind to and / or incorporate dissolved and / or condensing / aggregating / complexing and / or condensed / aggregated / complexed proteins by adding the one or more compounds before, during, or after the initiation of the condensation / aggregation / complexation of the proteins. A preferred method is one in which, in process step 4b), compounds dissolved in the aqueous process solution bind to or condense / aggregate / complex with the dissolved proteins by adding these compounds before, during, or after the initiation of the condensation / aggregation / complexation of the proteins. The complexed protein fraction can be condensed to a dehydrated mass using centrifugal techniques, such as a decanter.

[0247] A preferred method is one in which, in step 4b), compounds present in solution in the aqueous process solution are bound to the dissolved proteins by condensing / aggregating / complexing these compounds with the dissolved proteins.

[0248] A method is particularly preferred in which, in step 5), the separation of the suspension from step 4) is carried out using a filtration method.

[0249] Procedure variants of process step 6):

[0250] In a preferred embodiment, in process step 6), compounds still contained in the clarified aqueous phase of process step 5) are reduced / removed by purifying the process water phase. This can be achieved by adsorption, aggregation, complexation, or dialysis. In this process step, one or more compounds or classes of compounds can be removed from the aqueous phase using prior art methods. For example, dissolved odor and flavor substances can be removed with clay minerals such as calcium bentonite, saponite, or kerolite. Zeolites or activated carbon preparations, activated coke, silica gels, molecular sieves, aluminas, aluminum oxide, and styrene polymers can also be used. Furthermore, dyes can be removed with suitable adsorbents, such as activated carbon. The clarified process liquid from step 5) may also contain phospholipids and / or glycolipids.This can be controlled by the process parameters of the preceding process steps. In one embodiment, one or both of these compound classes are removed by adding precipitating agents to the process fluid. Suitable reagents include, among others, silicates, carbonates, oxides of magnesium, calcium, aluminum, or copper compounds, such as copper chloride or calcium carbonate. This causes aggregation / complexation of these compounds, resulting in agglomerates that can be seen with the naked eye. After a sufficient time and concentration of the precipitating agents, which is reached when no further aggregates form, these can be separated and collected using centrifugal separation techniques. Coagulating agents, such as (NH4)2SO4, CaSO4, MgSO4, Na2SO4, or organic substances like glucano-lactone, are also preferred.It is preferred to remove the resulting condensates / aggregates and complexes from the process water phase by means of a filter technique or centrifugal methods.

[0251] In a further advantageous embodiment of process step 6), the ionic and ionizable compounds present in the clarified process liquid, such as sodium, potassium, magnesium, or calcium, are reduced. For this purpose, known ion exchange resins, such as Amberlite XAD 16HP, XAD 7HP, XAD 1180NFPX 66, or Dowex 1x8, can be added to the process liquid, or electrodialysis of the process liquid can be carried out.

[0252] A preferred process includes, in process step 6), purification of the process water phase by reducing or removing dissolved organic and / or inorganic compounds in the clarified water phase through adsorption, aggregation, complexation, or dialysis. In a further preferred embodiment, toxins, herbicides, pesticides, or other harmful compounds are removed from the clarified water phase by suitable methods. Suitable methods include, for example, ultrafiltration or nanofiltration of the solution or adsorption of the toxins or hazardous substances.

[0253] In a further preferred embodiment, dissolved compounds and / or microorganisms are inactivated and separated by thermal treatment. The preferred temperature range for the thermal treatment is between 40° and 120°C or between 18° and 0°C. Separation is achieved by altering the solubility of the compounds / microorganisms to be separated through thermal treatment, causing them to condense and / or complex. The resulting condensates / aggregates can then be removed from the liquid using known separation techniques. Suitable separation methods include centrifugal processes as well as filtration and sieving techniques. This process step can be used, among other things, to separate compounds belonging to the class of carbohydrates.

[0254] A preferred method is one in which, in process step 6), the process water phase is purified, undergoing thermal treatment in which dissolved compounds and / or

[0255] Microorganisms are condensed and / or complexed and then separated.

[0256] In a further particularly preferred embodiment of process step 6), further purification steps are carried out to reuse the clarified process water phase.

[0257] These include, among other things, the possible reduction or removal of germs / spores. This can be achieved using well-known methods such as microfiltration (sterile filtration) or irradiation (UV or gamma rays).

[0258] A preferred method is one in which, in process step 6), a method for reducing and / or removing germs and spores is carried out.

[0259] Surprisingly, it has been shown that the water phases used can be completely recycled and reused in the process. Since large quantities of process water are required in this technology, this is of considerable economic importance. Wastewater generation from the separation process can be completely avoided. It has been demonstrated that the continuous reuse of the process fluids has no negative impact on the quantity and quality of the product fractions.

[0260] In a particularly preferred embodiment of the method, one or more sidestream process steps are carried out in addition to the described main process steps. The execution of these process steps is optimal and can be temporally and spatially independent of one another. However, for process economy, it is advantageous and therefore preferred to link the main process sequence and the sidestream process sequence 3-1 temporally and spatially.

[0261] A preferred method consists of a main process and a sidestream process for obtaining separated and purified constituents of plant starting materials, in which, for process economy, the process water phases of the main process steps are used in sidestream process steps and vice versa. Sidestream process 3-1

[0262] The inventive process steps of the optional sidestream process enable, in a particularly advantageous and surprising manner, further highly beneficial effects in the material utilization of the sieve residues obtained in process step 3). The composition of the corpuscular organic components of the sieve residue depends on the starting material. In principle, the following main components can be found: cellulose-based fibers, lignin-based shell components, and complex carbohydrates, wherein the complex carbohydrates are predominantly present in the form of corpuscular components up to and including completely preserved starch granules. Microscopic analyses have shown that the individual fractions are present in pure form, i.e., not complexed with each other or with proteins or other organic compounds.This allows for further fractionation of these components using very simple mechanical separation processes. In the optional process steps of the sidestream process 3-1, the sieve residue or filter cake obtained in process step 3) (optionally pre-fractionated by process step 3a) or 3b)) is used. In process step 3-1.a, the material is mixed with an aqueous phase in a reaction vessel (R3 according to Scheme 1). Preferably, this is a clarified process water phase, which is obtained, for example, after process step 5) and fed into the process step from the storage tank V5a. However, any other aqueous phase as well as fresh water can also be used.The ratio of water to filter residue depends on the remaining impurities, preferably between (w:w) 1:1 and 500:1 wt%, more preferably between 2:1 and 200:1 wt%, and further preferably between 3:1 and 100:1 wt%. Intensive mixing is preferably carried out, for example with a high-performance shear mixer or a colloid mill. The process temperature can be increased, preferably to values ​​between 35 and 70°C, more preferably to 40° to 60°C. The duration of the mixing depends on the other process parameters and is determined by the purity of the compounds obtainable by fractionation. In the optional process step 3-1.b, complex carbohydrate aggregates and insufficiently ground starting materials (e.g., grains, leaves) are first separated.In a preferred application of the process, the suspension from reaction container R3 is sieved within a liquid-filled container using a suitable sieve size that allows > 95% of the cellulose-based fibers and lignin-based shell components to pass through. The passing fiber and shell components then sediment in the collection container (A3) and are present together with the process liquid. During the sieving process, for example, the sieve is flowed over and / or passage is facilitated by vibration of the sieve, whereby carbohydrate particles and large particles do not pass through the sieve. The retained complex carbohydrates or particles can then be removed from the sieve and fed into the product container P2. These products can be used for further applications. In a further preferred process step 3-1.The particulate matter suspended in the collection vessel A3 is separated according to its density using an eddy current separator (e.g., a hydrocyclone), preferably separating the lighter cellulose-based fibers via the upper flow and the heavier lignin-based shell fractions via the lower flow. In a further preferred process step, the aqueous phases of the upper and lower flows from the hydrocyclone separation, a method for separating the particulate components, are added to the process water phase. Preferably, the separation is carried out using filtration techniques, such as a vibrating screen, or centrifugal methods, such as centrifuges or decanters. The resulting fractions (cellulose-based fiber and lignin-rich shell fractions) are then subjected to a drying process or used for further processing.The resulting process water phases can be combined and, for example, returned to process steps 2a), 2b), or 3) without further purification. This process thus allows for the highly advantageous recovery of pure fractions of cellulose-based fibers and lignin-rich shells. Furthermore, the process water required for this can be recycled to upstream process steps. Preferably, the process water from the bypass process step 3-1.c is introduced into the storage tank V5b.

[0263] A preferred method is one in which cellulose-based fibers, lignin-rich shell fragments and / or complex / complexed carbohydrates can be separated and used in pure form from biogenic starting materials.

[0264] Preferred are pure fractions of cellulose-based fibers, lignin-rich shell fragments and / or complex / complexed carbohydrates, available in pure form according to one of the processes according to the invention.

[0265] Pure means that other organic components / compounds are present in a weight fraction of < 10%.

[0266] The following section will discuss particularly advantageous process engineering aspects: Extraction of lipids from biogenic starting materials.

[0267] According to current technology, when extracting proteins and / or carbohydrates from oil-containing biogenic starting materials, such as the seeds of oil plants like rapeseed or soybeans, an oil removal process is carried out. This involves pressing the seeds or grains or extracting them using organic solvents. This is necessary because lipophilic compounds, primarily triglycerides, would otherwise be removed along with the proteins or carbohydrates, thus reducing product quality. Complete oil removal from the plant seeds or extracts is also required because of the odor and flavor compounds contained in the oil fraction. Literature shows that the remaining lipids accumulate in the protein fraction during protein isolation and negatively affect the sensory properties (bitter, rancid taste and smell).This off-flavor is transferred to foods when protein supplements are used and is therefore undesirable.

[0268] Prior art methods for oil removal involve extracting nonpolar lipids from aqueous solutions / suspensions of crushed plant seeds by contacting the plant material with organic solvents at room or elevated temperatures for an extended period. The resulting solvent contains neutral fats and dissolved toxins. Such applications require complex processes and can lead to residual organic solvents in the recovered products. This is particularly true when an alcohol is used as the solvent, as it is difficult to remove from the aqueous phase and therefore significantly limits the reusability of the aqueous extraction solution. Furthermore, alcohols irreversibly damage valuable constituents such as polyphenols.Patent DE10101326 AI describes a simplified process in which supercritical CO2 is added as a solvent to crushed plant seeds, and crude oil and an oil-depleted residue are obtained by means of phase separation. Qualitative properties of obtainable protein fractions are not disclosed. Such processes are associated with significant energy expenditure and are hardly suitable for large-scale industrial application.

[0269] In other processes, the extraction of neutral lipids is carried out directly with organic solvents such as hexane or pentane, usually at high temperatures. This also removes amphibious compounds such as free fatty acids, phospholipids, vitamins, and polyphenols, meaning these compounds are either lost or must be extracted from the offcuts. On the other hand, it has been shown that lecithin-rich protein concentrates exhibit excellent emulsifying properties and are therefore of great interest in the food industry. To achieve this, purified or crude lecithin is added to the isolated protein according to current technology, for example, using a spray technique. Such a procedure requires considerable process-related and therefore also economic effort to obtain protein isolates with exceptionally good emulsifying properties.In a study investigating qualitative differences between two protein fractions obtained from rapeseed press cake, one fraction being obtained after oil removal using hexane, followed by aqueous fractionation and precipitation by an acid, and the other by aqueous fractionation and recovery of the protein fraction by ultracentrifugation, the water solubility of the protein fraction in the first process was only 24% at a pH of 7-9, while in the second process it was 50% (Yumiko Yoshie-Stark, Chemical composition, functional properties, and bioactivities of rapeseed protein isolates, Food Chemistry, Volume 107, 2008, p. 32-39). It is known from the literature that the solubility of globulins is influenced by the folding of the protein chain.If physical modification occurs through pH shift and / or thermal treatment above the denaturation temperature, the structure and charge distribution at the molecular surface change. If nonpolar amino acid residues reach the solvent interface, the solubility decreases significantly. Certain physical modifications of the structure, such as those induced by pH, are often reversible, whereas thermal denaturation generally leads to irreversible changes in structure and properties. Therefore, it is advantageous to use a de-oiling process that neither employs an organic solvent nor involves heating.

[0270] Surprisingly, it was found that, using a process according to the invention, neither the presence of an organic solvent nor the use of elevated temperatures is required to separate neutral lipids from proteins and carbohydrates. Furthermore, protein fractions containing phospholipids at a content of 2 to 15 wt% could be obtained using the process embodiments according to the invention. In addition to phospholipids, other so-called fat-related substances, such as free fatty acids, carotenoids, isoflavonoids, and tocopherols, were also found in protein or carbohydrate fractions. Such amphiphilic components of the biogenic starting materials have high nutritional potential and can be desirable in protein and carbohydrate fractions.It was demonstrated that such amphiphilic compounds can be obtained in chemically and physically unchanged form along with the protein fractions obtained from the process. Furthermore, the obtainable protein fractions exhibited no off-flavor. Additionally, the recovered protein fractions displayed very good physical properties, with a water solubility (NSI) of > 70%.

[0271] Furthermore, the process techniques according to the invention enabled the separation of neutral fats. Since these are mostly present in micellar form together with phospholipids and / or glycoglycerolipids, their separation is considerably more difficult, even in an aqueous medium. Surprisingly, it was found that, under certain conditions, it is possible to completely or almost completely separate neutral lipids from the other constituents of the biogenic starting material during the process according to the invention. In a particularly preferred embodiment of the process, the temperature of the reaction mixture is increased in step 2b), or 2), and / or before or during the addition and mixing of the condensing agent in step 3). A temperature increase to 50° to 95°C is preferred, more preferably to 55° to 75°C, and even more preferably to 60° to 70°C.It was found that neutral fats bound by this process dissolve and precipitate on the surface of the aqueous reaction mixture according to their specific gravity. Preferably, the condensing agents are added only after the desired temperature has been reached and with gentle agitation of the medium. It is particularly advantageous to carry out one or more of the process steps 2a) - 2a3) and / or 2b) - 2b3) separately or together before, during, or after the temperature has been reached. The recovery of the lipid phase that forms is preferred; this can be obtained, for example, by skimming or overflow methods.

[0272] A preferred method is an aqueous process for the de-oiling of plant proteins, which can be carried out at room temperature and / or elevated temperature.

[0273] A preferred method is a process for separating organic constituents from plant starting materials, in which neutral lipids are removed by an aqueous solution containing dissolved amino acids and / or peptides, and a protein fraction is obtained that has a water solubility of > 70%. A particularly preferred embodiment of the process is one in which the dissolved amino acids and / or peptides are dissolved cationic amino acids and / or peptides. A preferred method is a process for separating organic constituents from plant starting materials, in which neutral lipids are removed and proteins are obtained by an aqueous solution containing dissolved amino acids and / or peptides without heating. A particularly preferred embodiment of the process is one in which the dissolved amino acids and / or peptides are dissolved cationic amino acids and / or peptides.

[0274] No heating means that a temperature of 60°C is not exceeded.

[0275] A neutral fat-free protein fraction is preferred.

[0276] In this context, neutral fat-free means a mass weight fraction of < 0.l wt%.

[0277] Surprisingly, the aqueous digestion process according to the invention results in a spontaneous phase separation of the neutral lipids and the aqueous phase. These lipid phases exhibited only slight emulsion formation at the phase boundary and were, in some cases, almost clear. Separation could be achieved by separately draining off the phases. No further neutral lipids could be extracted from samples of the aqueous phase below using organic solvents. This process effect is therefore particularly advantageous, as it eliminates the need for an additional step to remove neutral lipids with solvents. The sedimentative separation process can be accelerated by centrifugal separation techniques. Furthermore, the skimming of the lipid phase can be carried out in various process steps.In a preferred embodiment of the process, the spontaneously separating lipid phase is removed continuously or discontinuously in a container with a controllable outlet in the upper region, so that with continuous filling of the container, the accumulating lipid phase can be drained through the outlet, or, with discontinuous filling, the lipid phase is separated before the aqueous phase is drained. In a preferred embodiment of the process, the lipid phase is skimmed off after process step 2b) or 2), preferably after complete dissolution of the organic components has already occurred. In a further preferred embodiment, the lipid phase is skimmed off following the separation of the solids in process step 3). In a further preferred embodiment, the skimming takes place after a change in the pH value of the aqueous solution.This is particularly advantageous when, for the separation of a condensed protein phase, the entire aqueous phase is fractionated using a centrifugal field separator; separation of the phases with a tricanter is especially beneficial. This allows the three phases present—solid, aqueous phase, and lipid phase—to be separated in a single process step and obtained with a high degree of purity. If a neutral fat phase has been added to the aqueous process solution during a process step, it can be removed again in the same or in one of the subsequent process steps using the methods mentioned above.

[0278] The separation of the neutral fat phase is favored by a large dilution ratio of the aqueous phase of the aqueous process mixture in relation to the solid content contained therein, or by an increased process temperature.

[0279] Disintegration of plant starting material and obtainable products

[0280] The process according to the invention is also aimed at the complete material utilization of all constituents of the plant starting material. According to the prior art, efficient fractionation of constituents, such as the protein fraction with a protein content of > 80 wt%, requires mechanical disintegration of the plant starting material to obtain a very fine flour or powder. This process is energy-intensive and does not allow for the separation of all constituents from one another, thus failing to yield materially pure fractions.

[0281] Surprisingly, it was demonstrated that the process steps according to the invention also enable the disintegration of the plant starting material, thereby eliminating the need for complex mechanical digestion processes. Simultaneously, complete utilization of all constituents of the plant starting material can be achieved with a high degree of purity.It was thus demonstrated that it is not necessary to mechanically break down the plant material as finely as possible to ensure high efficiency of the material separation using the inventive method; finer mechanical division only reduced the duration of the soaking time of the plant material with the aqueous solutions according to the invention. The product results were no different when only coarse division of the plant material took place, as with grits or semolina, compared to fine flour. Furthermore, it was found that even large aggregates, which can be scaled down to the centimeter level, are completely permeated by the aqueous solutions according to the invention over time, which is not the case with aqueous solutions containing alkalis, acids, or surfactants.However, a prerequisite is that the plant material to be processed is permeable to water. Therefore, in a preferred embodiment, the plant sheath material, which forms a water-repellent and / or water-impermeable layer or layers, is first processed so that the plant material can be penetrated by the aqueous solutions according to the invention at room temperature. Using the methods described herein, it is easy to determine whether sufficient disintegration of the plant material has occurred and whether the constituents have separated from one another and can thus be isolated in a distribution volume.Thus, the process according to the invention is particularly advantageously suited for the disintegration of plant starting material that is not mechanically disintegrated or only slightly disintegrated, while simultaneously separating the constituents of the plant starting material, enabling the recovery of the constituents in pure form. Mechanical disintegration is particularly unnecessary if the aqueous solutions according to the invention, containing dissolved amino acids and / or peptides, can freely pass through the plant starting material. A preferred method is one for disintegrating plant starting material using an aqueous solution containing dissolved amino acids and / or peptides, by which the constituents of the starting material can be obtained in pure form. An embodiment of the process in which the dissolved amino acids and / or peptides are dissolved cationic amino acids and / or peptides is particularly preferred.

[0282] Another aspect of the invention aims at the complete utilization of all components of plant seeds, kernels, or grains. Prior art processes generally aim to obtain only one fraction of the constituents in the purest possible form; processes for the complete breakdown of plant starting materials are not available. Surprisingly, it has been shown that the processes according to the invention now make it possible to separate all constituents present in the plant starting materials from one another and to make them available for economic utilization in pure form. This applies particularly to the main constituents of the plant starting material, such as proteins, carbohydrates, cellulose-based fibers and lignin-rich hulls, as well as neutral lipids, but also to minor constituents such as phospholipids, glycolipids, glycoglycerolipids, pigments, antioxidants, vitamins, and minerals.

[0283] A preferred method is one in which complete utilization of plant starting materials takes place without further pretreatment, by obtaining the main components in pure form through aqueous digestion.

[0284] Thus, the invention relates to a process for the complete aqueous digestion of plant starting materials for complete material utilization.

[0285] The process according to the invention is also particularly suitable for obtaining, in unchanged form, thermolabile compounds that are present in the biogenic starting material and whose structure and / or function are destroyed by heating. The process according to the invention enables the breakdown and recovery of constituents at ambient temperatures. It is preferred that the process steps be carried out at a temperature of the aqueous phases between 1 and 60°C, more preferably between 5 and 40°C, further preferably between 10 and 40°C, and particularly preferably between 15 and 35°C.

[0286] Retainable protein fractions and minor fractions

[0287] Another aspect of the invention relates to odor and flavor compounds, which are found particularly in plant seeds and are predominantly bound to the proteins contained therein. These compounds, such as ketones or aldehydes, are difficult to separate using prior art techniques. An aqueous process for detaching and separating flavorings or colorings from proteins is not known. Prior art processes include first debittering the meal by treating it with acids before extracting the remaining components (DE 5 37 265). Such processes are complex and have limited efficiency.Surprisingly, it has now been found that the separation of the constituents of the biogenic starting materials, including aqueous solutions containing dissolved cationic amino acids and / or peptides, also allows the odor and taste compounds to be detached from their bonds and leached into the aqueous distribution solution. It can be assumed that the expansion of the proteins due to the hydration achieved by the process promotes the detachment of the odor and taste compounds and prevents their reattachment. The clarified aqueous solutions obtained after the separation of solid particles and the condensed / aggregated / complexed soluble constituents (proteins) exhibit the corresponding odor and taste components to a high degree. As a result, the recoverable protein fractions are completely or almost completely odorless and tasteless.In aqueous extraction trials conducted without the compounds according to the invention, the odor and flavor compounds (especially the bitter substances) remained associated with the protein fraction and were still present in a recoverable protein extract obtained by precipitation or centrifugal separation, leading to undesirable sensory and nutritional effects. Thus, in one embodiment of the process, protein fractions can be obtained that are low in or free of off-flavors. On the other hand, dissolved odor and flavor compounds, including the bitter substances, are obtained, which can be recovered separately. Methods for this are known in the prior art.

[0288] A preferred method involves detaching and separating odor and / or flavor substances and / or antinutritional compounds and / or endogenous or exogenous toxins from the constituents.

[0289] A preferred method is one for obtaining biogenic odor and flavor substances.

[0290] In one embodiment, the process steps according to the invention can also be used for the purification of protein fractions. It has been shown that not only odor or flavor compounds can be dissolved and separated from the constituents of the biogenic starting materials, but also other physiologically or non-physiologically occurring compounds. Physiological compounds include, among others, phytosterols, glycosides, alkaloids, inosites, polyphenols, flavonoids, vitamins, phytosterols, saponins, glucosides, phytoestrogens, monoterpenes, and endogenous toxins such as phorbol esters or certain fatty acids, such as erucic acid or phytic acid. Unphysiological compounds include, among others, pesticides, herbicides, fungicides or exogenous toxins, e.g. from fungi, such as aflatoxins, ochratoxins, Alternaria toxins, alternariol monomethyl ether (AME), altenuene and tenuazonic acid, fumonisins, Fusarium toxins or ergot alkaloids.As previously described, some physiologically occurring compounds are responsible for antinutritional properties, such as alpha-glucosidases, trypsin inhibitors, phytic acid, tannins, or oxidized phenols. It has been shown that the protein fractions produced according to the inventive methods exhibited practically no measurable traces of antinutritional or toxic compounds when these were present in the biogenic starting materials.

[0291] A preferred method is one for removing and separating odor and / or flavor substances and / or antinutritional compounds and / or endogenous or exogenous toxins. A protein fraction with few off-flavors and no or minimal residual levels of antinutritional compounds and / or toxins is preferred.

[0292] It was further found that even the already isolated fractions of constituents occurring in biogenic starting materials can be purified of impurities / minor components using one of the processes according to the invention. A particular advantage is that only the already separated protein fractions need to be treated with the aqueous digestion solutions disclosed herein. It was demonstrated that in a protein concentrate from an algal culture with a high proportion of chlorophyll, neutral lipids, and carboxylic acids, which was in powdered form and used instead of the biogenic starting material in process step 1) and treated with the consecutive process steps according to the invention, a practically complete separation of chlorophyll, neutral lipids, and carboxylic acids was achieved, such that the resulting protein concentrate contained no or practically no chlorophyll, neutral lipids, or carboxylic acids.Furthermore, a milk protein condensate, which had a high content of neutral lipids, phospholipids, and free fatty acids, but also soluble carbohydrates, was treated with process steps 2, 4, and 5. The resulting protein mass had a protein content (based on dry matter) that was 11 wt% higher than that of the starting material. Only a very small amount of carbohydrates was found in the protein fraction, no free fatty acids were present, and neutral lipids and phospholipids were present in a range of less than 1 wt% with respect to the protein mass. In a further investigation, a meal from an animal rendering plant, consisting of fish carcasses with a solids content of 32 wt%, a protein content of 51 wt%, and a lipid content of 12 wt%, was used as the starting material and treated with a process according to the invention. Step 2b) was carried out at a temperature of 60°C.At the end of the process step, a lipid fraction with a slight turbidity, which floated to the surface of the process fluid, was skimmed off. The solids obtained in step 3 were free of adhering soluble compounds. The protein mass obtained contained no solids and no free fatty acids or neutral lipids.

[0293] The protein fractions (PI) obtained from process step 5 according to Scheme 1), or other protein fractions obtained, are completely dissolved in one of the digestion solutions for purification, either again or for the first time, as required or to meet specific requirements. The proportions, concentrations, and compositions of the digestion solutions are to be selected analogously to those of process step 2a. The same applies to the pH of the process solution, which is preferably adjusted to a value between 6.5 and 13, more preferably between 7 and 12, and further preferably between 8 and 12. A shear mixer can be used to obtain a homogeneous solution or suspension. The process conditions and residence time can also be carried out analogously to those of process step 2a. The recovery of the dissolved protein fraction then takes place according to process steps 4 and 5.All protein fractions obtained from the described investigations were odorless and tasteless, whereas the starting materials had a distinct inherent taste. If deactivation and / or removal of antinutritional and / or toxic compounds from the obtainable protein fractions is desired or necessary, prior art methods can be used. For example, it is possible to homogenize the obtained protein mass with a suitable amount of water and heat it to a defined temperature at which deactivation, e.g., of enzymes, occurs. It is known from the literature that enzymes, when present in protein flour dissolved in water, are completely deactivated after just a few minutes at a temperature of 85–90°C. In contrast, such deactivation is not possible in dry protein flour or in grains.This method enables the inactivation or modification of thermosensitive compounds, such as toxins or enzymes, in an aqueous solution containing dissolved cationic amino acids and / or peptides by suspending the proteins containing the thermosensitive compounds in the aqueous solution and heating them. Heating to a temperature between 50 and 140°C is preferred, more preferably between 60 and 121°C, and even more preferably between 70 and 90°C. The duration of the heat treatment depends on the compound to be deactivated and must be determined experimentally.

[0294] A preferred method is one for deactivating enzymes and toxins in an aqueous protein fraction.

[0295] The aqueous digestion process advantageously separates the organic components of the starting material from one another, thus making them separable. Fibrous or particulate materials, which had been separated from the aqueous process mixture by simple sieving and freed from residual / adhering water, were practically pure; that is, further washing steps with aqueous solutions or organic solvents could not remove any or only minimal amounts of soluble organic compounds. The resulting digestion of the starting material's constituents can also be used to remove, in their dissolved state, components from the aqueous process mixture that would interfere with further processing and could be carried over into a product phase. This can be achieved using state-of-the-art methods.In an advantageous embodiment of the process, phenols and / or polyphenolic compounds are removed from the aqueous distribution mixture of process steps 2), 2b), 3), or 6.3) by binding them using adsorptive techniques. Suitable materials for this purpose include, for example, ion exchange resins, zeolites, activated carbon, and aluminas. Further preferred embodiments of the process, in which an immiscible organic phase is mixed into the aqueous reaction mixtures to bind amphiphilic and / or lipophilic compounds and separate them by phase separation, have already been described. Particularly suitable materials for this purpose are paraffinic oils, aliphatic or cyclic hydrocarbons, as well as methyl esters of fatty acids or paraffin compounds. Preferably, the phases are then thoroughly mixed or brought into contact.This method is particularly suitable for binding and carrying away lipophilic and / or amphiphilic organic compounds that are to be removed from the aqueous reaction mixture. The separation of the organic phase preferably occurs through spontaneous phase separation, and the phases can then be separated using one of the methods described herein. The organic compounds removable by such a method include, among others, lipophilic pigments such as carotenoids or chlorophylls, lipophilic vitamins such as etiol, calciferol, or tocopherol, phytosterols, polyphenols, saponins, glucosides, phytoestrogens, and monoterpenes. It has been demonstrated that the amphiphilic or lipophilic compounds carried out into a lipid phase can be extracted from it using established techniques and utilized.For example, chlorophylls with a purity level of > 80% or glycoglycerolipids with a purity level of > 70% could be extracted from the lipid phases. Furthermore, a recirculation of the lipid extraction solvent phase can also be implemented here.

[0296] A preferred method involves separating and recovering amphiphilic and / or lipophilic compounds by mixing an organic mixture with an aqueous solution containing dissolved amino acids and / or peptides, and subsequently separating a lipid phase. A particularly preferred embodiment of the method is one in which the dissolved amino acids and / or peptides are dissolved cationic amino acids and / or peptides. This method also aims to obtain a protein fraction that is low in odor and taste. In this context, low in odor and taste means that, compared to the starting material, the sensory odor and taste components are reduced by, preferably, > 70%, more preferably > 85%, and further preferably > 95%.In other words, a protein fraction is obtained by one of the processes according to the invention which contains < 30%, more preferably < 15%, and further preferably < 5% of sensorially perceptible odor or taste substances compared to the starting material. Furthermore, the process also aims to obtain a protein fraction that is free of off-flavors.

[0297] A preferred method is a process for producing protein fractions that are free from off-flavors. A preferred method is a process for obtaining a protein fraction with low odor and taste. A preferred method is a protein fraction with low odor and taste.

[0298] Surprisingly, toxins from the seeds, such as erucic acid or phorbol esters, and hazardous substances absorbed by the seeds, such as pesticides, herbicides, and fungicides, could also be dissolved using the digestion process. These compounds were no longer bound to proteins in the distribution phase. It turned out that, analogous to the behavior of odor and flavor compounds, the dissolved toxins or hazardous substances remained in solution and were present only in minimal quantities or not at all in the recoverable protein fraction. Therefore, the process aims to dissolve toxins and hazardous substances from the starting material. In this context, "dissolving" means that > ​​70 wt%, preferably > 85 wt%, and furthermore > 95 wt% of the toxins or hazardous substances present in the starting material are completely dissolved in the aqueous solution of the distribution phase, i.e., not bound to a protein.In other words, a protein fraction low in toxins and hazardous substances is obtained by one of the processes according to the invention, which contains < 30%, more preferably < 15%, and further preferably < 5% of the toxins or hazardous substances compared to the starting material. A process for producing protein fractions that are low in toxins and hazardous substances is preferred.

[0299] A preferred method is one for obtaining a protein fraction low in toxins and hazardous substances. Protein isolation

[0300] In investigations into the isolation of dissolved proteins from aqueous solutions containing other dissolved soluble constituents, obtained by separation in aqueous solutions containing dissolved amino acids and / or peptides, it was found that the hydration of the proteins achievable through this process allows for the recovery of a very pure fraction by appropriately selecting the process parameters. "Pure" in this context means that the protein fractions have a protein content of preferably > 60 wt%, more preferably > 70 wt%, further preferably > 80 wt%, and even more preferably > 85 wt%, and most preferably > 90 wt%. This was particularly true for the use of cationic amino acids and / or peptides.

[0301] It was found that such pure protein fractions can be produced in particular by achieving a large distribution volume after the constituents were digested according to the invention. Proteins dissolved in this way pass, for example, through a membrane filter with a pore permeability of minimal Iμιτι. This allows for size-selective separation of dissolved proteins. Furthermore, it was shown that, especially in this situation of optimal hydration of the dissolved proteins and the presence of a physiological pH range, a very rapid and pronounced interaction with the condensing agents listed herein occurs, resulting in the hydrated proteins aggregating and displacing or excluding the process water.This can be recognized, for example, by the formation of three-dimensional structures visible to the naked eye, accompanied by partial or complete clarification of the process fluid, which then settle only very slowly. The process fluid is subsequently moderately to intensely colored and contains odor and taste compounds as well as soluble carbohydrates. Thus, the hydration and condensation process ensures that the compounds previously detached from the proteins remain in a dissolved state in the process water phase and do not bind with or are carried away by the condensing proteins.

[0302] Furthermore, the process opens up the possibility of using very different compounds as condensing agents for the dissolved proteins, thereby achieving further highly advantageous effects on the obtainable pure protein fractions. For example, condensing agents can be used that bind to the proteins and remain in the obtainable protein fraction. This allows, for example, antioxidants such as ascorbic acid or compounds with surfactant properties such as glycoglycerolipids or calcium compounds such as calcium carbonate to be incorporated into the obtainable protein fraction in a targeted and dosable manner and in various combinations. Advantageously, the obtained protein fractions retain the excellent solubility properties obtained with the inventive processes.

[0303] It has proven particularly advantageous that the protein fractions obtainable by these methods exhibit a very homogeneous consistency and a pH between 6.0 and 7.5. After centrifugal removal of binding water, the resulting paste-like mass remains homogeneous and is very easily soluble in water. This can be used to great advantage to completely dissolve the obtainable condensed protein fraction in a washing step with water or a protic solvent and subsequently separate it by further centrifugation. It is also very easy to obtain a suspension in a slightly or completely nonpolar solvent, which allows even strongly hydrophobic compounds to be extracted from the dissolved protein mass. Thus, the process technology according to the invention ensures a sequenced removal of organic compounds from the obtainable protein fractions.Furthermore, polar compounds, such as electrolytes contained in the remaining residual water, can also be removed. A protein fraction obtained from the process according to the invention is particularly suitable for this purpose. This fraction is preferably produced by filtration techniques in the form of a highly dehydrated protein mass, which is placed in a filter fabric and immersed in or subjected to deionized water. It was found that practically no relevant amounts of protein are lost from the protein mass.

[0304] Thus, the process steps and techniques allow for the obtaining of highly purified protein fractions that meet the product specifications of protein condensates, protein concentrates and protein isolates.

[0305] A preferred method is a process for producing protein condensates and / or protein concentrates and / or protein isolates from organic starting material using aqueous solutions containing dissolved amino acids and / or peptides. A particularly preferred embodiment of the process is one in which the dissolved amino acids and / or peptides are dissolved cationic amino acids and / or peptides.

[0306] Further advantages arise from the consistency of the obtainable protein fractions, which can be controlled by the process. Protein fractions can be obtained that are liquid, pasty, solid, or granular. It is also advantageous that even thickened protein fractions can be readily dissolved in water and fed in a free-flowing form, for example, into a spray-drying process to produce a powder.

[0307] Retainable carbohydrate fractions

[0308] Carbohydrates in plant seeds, kernels, or grains are predominantly present in the form of amyoplasts, the so-called starch granules. These largely break down during pressing and milling, releasing glycogen. These polysaccharides, suitable for human nutrition, are predominantly present in high-molecular-weight form as starch. Starch consists of microscopically small, polymeric solid particles that exhibit characteristic sizes and shapes, as well as varying proportions of amylose and amylopectin, depending on the plant species or variety. Native starch granules are insoluble in water. They swell reversibly in cold water by up to 28% by volume, with the free hydroxyl groups of the starch molecules forming hydrogen bonds. Above a certain temperature, which depends on the type of starch, the starch gelatinizes within a very narrow temperature range.This gelatinization is irreversible and is based on a softening of the amorphous starch structure through the gradual absorption of water and the breaking of hydrogen bonds.

[0309] The inventive method makes it very advantageous to dissolve and separate dissolved and undissolved as well as insoluble carbohydrates from other organic and inorganic compounds in order to make them available for further use.

[0310] In one embodiment, process steps 2), 2a), 2b), and 3) are carried out under cold or cooled conditions (<10°C). This allows the breakdown of complex carbohydrates to be reduced to the necessary level, depending on the process time, so that, for example, the release of amylopectins does not occur or occurs only to a minimal extent. Furthermore, the swelling capacity of complex carbohydrates is minimized, allowing the complex carbohydrates to be obtained in a largely unchanged state compared to the initial state, but freed from other components of the starting mixture. Particularly advantageously, undissolved complex carbohydrates, corresponding, for example, to a starch granule or parts thereof, can be separated from the remaining solids and soluble compounds using simple filtration or eddy current techniques. After drying, e.g.,In a drying oven, they can be put to use, e.g. in the production of starch flour.

[0311] Insoluble carbohydrates exist, for example, in the form of polysaccharides, which exhibit different sedimentation rates depending on their molecular weight. It has been found that polysaccharides that cannot be removed by filtration from the process mixture of process step 2b), 2), or 3) sediment only very slowly. Surprisingly, with the appropriate selection of a condensing agent for the condensation / aggregation / complexation of the proteins present in the mixture, these compounds are not incorporated into or bound to the condensates / aggregates / complexes. Therefore, this carbohydrate fraction remains in the clarified process water after the condensed soluble proteins have been separated using a suitable filter material. It has been found that following the separation of the proteins, or possibly other fractions, e.g.,From lipids or amphiphilic compounds, the higher molecular weight carbohydrates present in the process water can be separated using centrifugal techniques, such as a decanter or separator. The solid obtained in this way can be further purified using a simple process technique. Surprisingly, it was found that the same aqueous solutions containing dissolved amino acids and / or peptides can be used to purify the obtainable higher molecular weight carbohydrates. Cationic amino acids / peptides were particularly suitable for this purpose. For this, the carbohydrate fraction, preferably freed from free liquid, is placed in a container with one of the aqueous solutions according to the invention, containing dissolved amino acids and / or peptides, in one of the concentrations specified therein, and dissolved therein.After a residence time of preferably between 2 minutes and 3 days, more preferably between 5 minutes and 24 hours, and further preferably between 15 minutes and 3 hours, phase separation is carried out, preferably by filtration techniques or by centrifugal processes. The resulting mass can be dried using prior art methods and processed into a flour that can be used immediately. It has been shown that a high product purity is achieved. It has also been shown that when using centrifugal processes, a larger proportion of dissolved proteins is removed with the solid phase; therefore, only filtration or eddy current separation processes are suitable to enable the most complete possible separation of dissolved proteins from solids. This was not known in the prior art, as can be illustrated, for example, by Chinese patent application CN 106 720 920 A.The text does not describe how the fibers are detached and separated from the proteins. In particular, it is unclear how the protein phase is separated. On the other hand, the method makes it possible to selectively integrate soluble carbohydrates into a obtainable protein fraction. It has been found that, under certain conditions, the dissolved carbohydrates can be incorporated into a forming condensate / agglomerate / complex of proteins, resulting in a very homogeneous combination product. Further advantages arise from the possibility of heating the digestion mixture and / or the partition mixture. This allows complex carbohydrates to be completely or partially digested or hydrated, producing water-soluble carbohydrate fractions. This makes it possible to generate soluble carbohydrates, such as...Pectins, which can then be incorporated into the recoverable protein fraction and separated together with it, but also separately.

[0312] A preferred method involves separating and utilizing the water-insoluble and / or insoluble carbohydrates from organic components.

[0313] A preferred method is one in which dissolved carbohydrates are condensed / agglomerated / complexed together with dissolved proteins, resulting in protein-carbohydrate condensates / agglomerates / complexes.

[0314] A preferred method is one in which, in step 4), dissolved carbohydrates and / or phospholipids and / or glycoglycerolipids are condensed / agglomerated / complexed together with dissolved proteins, yielding protein condensates / agglomerates / complexes containing carbohydrates and / or phospholipids and / or glycoglycerolipids.

[0315] A preferred method involves converting insoluble carbohydrates into a soluble form and condensing / agglomerating / complexing them with dissolved proteins, resulting in a homogeneous mixture of proteins and carbohydrates.

[0316] Another aspect of the invention relates to the separation of carbohydrates from milled products. It has been found that in coarse or fine-grained flour, which, for example, results from an impact or milling process and in which the starch granules remain predominantly intact, the adhering soluble constituents, and in particular the soluble proteins, can be removed practically without residue using the method according to the invention. This allows the intact starch granules to be obtained and separated in pure form using a simple sieving technique. Since these have a different sieve size than cellulose-based fibers and lignin-rich bran components, a practically pure fraction of starch granules or carbohydrate aggregates can be obtained directly. After drying, these can be further processed. It has been shown that the removal of proteins from the starch granules or carbohydrate aggregates is particularly effective.The addition of complex carbohydrates has a very positive effect on the baking properties of the resulting flours. It was demonstrated that they exhibit a greater volume during the dough preparation and subsequent baking process than flours from which the protein content had not been removed. Furthermore, they showed less sticking to the baking surface. Additionally, the resulting flours made from complex carbohydrates were free of off-flavors, including unpleasant odors and / or tastes.

[0317] A preferred method is one in which protein-free complex carbohydrates and / or starch granules can be separated in pure form from vegetable pressed or milled products. In one embodiment of the present invention, the methods described herein further comprise step 4a) after step 4) and before step 5).

[0318] Separation of the aggregated proteins and subsequent addition of further aggregating agent to aggregate the carbohydrates according to step 3).

[0319] A preferred method is one in which protein-free flours are obtained from complex carbohydrates or starch granules, which exhibit improved baking properties compared to flour containing protein.

[0320] Improved baking properties mean, for example, increased leavening volume or reduced stickiness of a dough preparation or fermentation product.

[0321] Particularly preferred is a process wherein, in step 3), after the separation of solid solids from the distribution mixture of step 2b), obtaining a fiber-free aqueous solution of the water-soluble and dissolved compounds of the starting material, protein-free complex carbohydrates and / or starch granules are separated from the separated solid solids in a step 3a).

[0322] The present invention is also directed to protein-free complex or complexed carbohydrates and / or starch granules obtainable by a method described herein.

[0323] In a preferred embodiment, the protein-free complex or complexed carbohydrates and / or starch granules are obtained by a process wherein, in step 3), after the separation of solid solids from the distribution mixture of step 2b), obtaining a fiber-free aqueous solution of the water-soluble and dissolved compounds of the starting material, protein-free complex carbohydrates and / or starch granules are separated from the separated solid solids in step 3a).

[0324] In a preferred embodiment of the process according to the invention, in step 3) after the separation of solid solids from the distribution mixture of step 2b) to obtain a fiber-free aqueous solution of the water-soluble and dissolved compounds of the starting material, in a step 3a") decomplexed cellulose-based fibers and / or decomplexed lignin-rich shell fragments, and / or complex / complexed carbohydrates, which are free of dissolved soluble compounds, are obtained from the separated solid solids.

[0325] Furthermore, the present invention relates to cellulose-based fibers with a water binding capacity of >200 vol% and / or lignin-rich shells with a fat binding capacity of >200 wt%, obtainable by a method described herein.

[0326] Particularly preferred are cellulose-based fibers with a water binding capacity of >200 vol% and / or lignin-rich shells with a fat binding capacity of >200 wt%, obtainable by a process wherein, in step 3), after the separation of solid solids from the distribution mixture of step 2b), obtaining a fiber-free aqueous solution of the water-soluble and dissolved compounds of the starting material, in step 3a) decomplexed cellulose-based fibers and / or decomplexed lignin-rich shell parts, and / or complex / complexed carbohydrates, which are free of dissolved soluble compounds, are obtained from the separated solid solids.

[0327] Particularly preferred is a process in which, in step 4), dissolved carbohydrates and / or phospholipids and / or glycoglycerolipids are aggregated together with dissolved proteins, and, after step 5), in a step 5a), protein aggregates containing carbohydrates and / or phospholipids and / or glycoglycerolipids are obtained.

[0328] The present invention is therefore also directed towards protein aggregates containing carbohydrates obtainable according to a method according to the invention.

[0329] Particularly preferred are protein aggregates containing carbohydrates obtainable by a process in which, in step 4), dissolved carbohydrates and / or phospholipids and / or glycoglycerolipids are aggregated together with dissolved proteins, and, after step 5), in a step 5a), protein aggregates containing carbohydrates and / or phospholipids and / or glycoglycerolipids are obtained.

[0330] Cellulose-based fibers and lignin-rich shell parts

[0331] The type and composition of bran materials naturally vary depending on the type of plant material. For flour production, the bran is usually separated before milling, as it is generally undesirable in the resulting products. This typically requires significant processing effort and results in the loss of grain / seed material due to mechanical breakdown. Fibers, which are present as structural components in seeds, kernels, and grains, as well as in other plant materials, cannot be completely separated or isolated using state-of-the-art methods, as they are fully bound or compacted with the constituents. In particular, mechanical separation of these fibers is not possible with current technology.

[0332] It was therefore completely surprising that both the lignin-rich shell components and the cellulose-based fibers of the plant starting materials could be separated and obtained in a directly pure form. After extensive removal of bound water, no or virtually no proteins, soluble carbohydrates, odor or taste compounds, or other detachable organic or inorganic compounds were found. Microscopic examination revealed no traces of other organic components.

[0333] The lignin-rich shell fragments have a lignin content of 50–95 wt%. They occur as submillimeter-sized platelets or in an amorphous form. After drying, they are free-flowing and pourable. They possess a considerable water retention capacity, which can exceed 40%. Microscopically, the cellulose-based fibers have a cotton-like, three-dimensional structure with mean diameters between 50 and 500 μm and an aspect ratio (length / diameter) of 1:1 to 100:1. These are isolated / discrete structures that are not interconnected and have a very low linear density of < 70 mg / 100 m. It was found that such cellulose-based fibers differ significantly from cellulose fibers in chemical composition, secondary and tertiary structure, and physicochemical properties.Furthermore, it was found that both the recoverable cellulose-based fibers and the lignin-rich shell components exhibited a significant water binding capacity, exceeding 200 vol%.

[0334] Furthermore, it was found that both the lignin-rich shell components and the cellulose-based fibers are free or virtually free of odors, flavors, or dyes that are soluble in an aqueous medium. Therefore, the lignin-rich shell components and cellulose-based fibers obtainable by the process are, in the form in which they can be obtained and produced by the processes according to the invention or after drying, which can be carried out using prior art techniques, immediately usable or can be subjected to further processing.

[0335] A preferred method is one in which pure lignin-rich shell parts and / or cellulose-based fibers are obtained from a biogenic starting material, with a water binding capacity of > 200 vol%.

[0336] Surprisingly, dried lignin-rich shell particles exhibit not only a high water binding capacity and high water retention capacity, but also an extremely high binding capacity for oils and fats. In tests with various lignin-based shell particles, this capacity ranged from 250 to 550 wt%. Remarkably, hydrophobic interactions between the surfaces resulted in very rapid transport of oils and fats along the outer surfaces of the granules. This allows oils and fats to be transported against a pressure gradient through a poured lignin-rich shell granulate via capillary forces on the inner and outer surfaces. The delivery head in tests using riser pipes exceeded 5 cm.

[0337] Furthermore, it was shown that the dried and powdered cellulose-based fibers also exhibited a very high binding capacity for oils and fats, ranging from 220 to 360 wt%. A preferred method is one in which pure lignin-rich shell fragments and / or cellulose-based fibers are obtained from a biogenic starting material, with an oil and / or fat binding capacity of > 200 wt%.

[0338] Surprisingly, it was found that the lignin-rich hull components and the cellulose-based fibers, which were present in the filter residue of process step 3 for many of the investigated plant starting materials, such as press residues of rapeseed and jatropha, can be separated very easily using prior art techniques. Eddy current processes, such as hydrocyclones, are preferred for this purpose, but filtration techniques can also be used. It was demonstrated that this makes it possible to obtain pure fractions of cellulose-based fibers on the one hand and lignin-rich hull components on the other, in which no or virtually no proteins, soluble carbohydrates, odor or flavor compounds, or other organic or inorganic leachable compounds are present, or from which dyes leach in an aqueous medium.

[0339] The resulting shell or fiber fractions are preferably freed from any remaining bound water by a pressing process. Alternatively, centrifugal processes can be used. The dewatered shell or fiber fractions can be used in their obtained form or completely dried. Drying methods are known from the prior art. Warm air drying is preferred. Advantageously, the lignin-rich shell components obtained after drying are immediately available in a readily separable and free-flowing form.

[0340] It was found that the produced cellulose-based fibers differ in their chemical composition compared to cellulose fibers and cellulose derivatives. While practically no elements other than C, H, and O could be identified in cellulose fibers and cellulose derivatives, numerous elements such as N, S, P, Fe, Cl, Na, Ca, K, Ni, Cl, Cu, and others were present in cellulose-based fibers. Based on the bonding properties observed in the cellulose-based fibers, it can be assumed that these elements belong, at least in part, to functional groups that are covalently linked, either directly or indirectly, to the polymeric backbone structures. A covalent indirect link can occur, for example, via a sugar residue or a peptide.However, it is also conceivable that non-covalently bonded compounds are connected to the polymer backbone via electrostatic interactions exhibited by these functional groups or elements. The presence of functional groups on the surfaces of cellulose-based fibers is responsible for many of the effects observed so far.

[0341] Surprisingly, it was demonstrated that the obtainable cellulose-based fibers are ideally suited for various applications in humans and animals. For example, it was shown that cellulose-based fibers are excellent for incorporating, formulating, transporting, or storing substances / compounds or even microorganisms. They are particularly suitable for formulating proteins in dry or water-soluble form. Furthermore, cellulose-based fibers can also be used as a substitute for carbohydrates or fats in food preparations. They are also suitable as calorie-free dietary fiber and have stool-regulating effects. In addition, weight loss was achieved with diets using the cellulose-based fibers produced according to the invention.In addition, it was shown that further positive effects can be achieved, e.g. on the formulation of creams / lotions / ointments or pastes, or on the reduction of off-flavors in food, or also on the cultivation and increase in the activity of microorganisms such as yeasts or algae.

[0342] Introducing compounds into sustainable products

[0343] Another aspect of the invention relates to a method for the controlled introduction and / or contacting of compounds into / onto the protein fraction / proteins obtainable by the methods according to the invention. This method variant is made possible by the advantageous dissolution of the compounds used for aqueous separation. It may be necessary to increase the concentration of these compounds in subsequent process steps. For example, free fatty acids, phospholipids, glycolipids, antioxidants, or water-soluble vitamins can be stably dissolved in the aqueous process mixtures. Compounds already present in the reaction mixture can be used for this purpose, or compounds can be added to the reaction mixture in a suitable concentration. Preferably, this process step is carried out before the condensation / aggregation / complexation of the proteins.In one embodiment, adhesion of one or more dissolved compounds to the dissolved proteins is preferably achieved by changing their solubility in a spatial arrangement that also occurs physiologically, e.g., via hydrophilic and / or hydrophobic molecular domains, thereby binding the proteins. Preferably, the solubility of one or more of these compounds is changed before condensation / aggregation / complexation of the dissolved proteins, thereby preferably resulting in adhesion of the one or more compounds to the dissolved proteins. Particularly advantageously, the one or more compounds can be assembled in a region of the proteins that is highly expanded due to hydration and the physiological conditions under which condensation / aggregation / complexation of the dissolved proteins takes place, and which is also physiologically the preferred binding site of the protein.This achieves a "physiological loading" of the dissolved proteins, leading to particularly advantageous functional effects of the recoverable protein fractions. However, a change in the solubility of one or more compounds brought into contact with the dissolved proteins is also preferred; this change occurs during the initiation of protein condensation / aggregation / complexation. This allows for incorporation into the resulting condensates / aggregates / complexes.

[0344] Preferably, the solubility of one or more dissolved compounds is changed by adjusting the pH and / or salinity and / or temperature of the reaction mixture and / or by introducing a gas and / or adding further compounds, such as divalent cations. It has been shown that this method binds phospholipids, e.g., phosphotidylcholine, or fatty acids, e.g., linolenic acid, to the proteins, resulting in a weight ratio of 0.2 to 1.6 wt% with the recoverable protein fraction.This method is particularly advantageous because the loading of proteins with other organic compounds, preferably generated by electrostatic interactions, occurs through self-assembly. This results in a physiological alignment and arrangement of the compounds relative to one another, enabling stable incorporation of the introduced compounds and simultaneously stabilizing the proteins. In this context, "stabilized" means, among other things, that they exhibit greater stability against physical influences. It is particularly noteworthy that, for example, the formability of such protein fractions produced by self-assembly can be significantly improved with phospholipids or glycolipids in an aqueous medium. Furthermore, protein fractions produced in this way and loaded with free fatty acids exhibit a significantly improved mouthfeel.Furthermore, oxidation-labile compounds can be homogeneously incorporated and stabilized within such arranged protein fractions. These properties have been documented particularly for incorporated free fatty acids.

[0345] Available products

[0346] Surprisingly, the processes according to the invention yielded protein fractions free of off-flavors. Off-flavors are defined as odor and taste substances that lead to a reduction in the quality of the product. Furthermore, it is advantageous that the obtainable protein fractions were practically or completely free of any taste and odor substances, thus resulting in a tasteless and odorless protein product.

[0347] A preferred method is one in which a protein fraction is obtained that is free from off-flavors and / or is practically odorless and tasteless.

[0348] A highly advantageous aspect of this invention lies in the possibility of enriching the recoverable protein fractions with other compounds / substance groups, thereby producing higher-quality products. Higher product quality refers, for example, to a higher nutritional value achievable compared to a pure protein fraction. This is the case, for instance, when a combination of proteins and soluble carbohydrates is present. Further possibilities for a higher nutritional value in a combination product include the inclusion of vitamins or antioxidants, which preferably originate from the related starting material itself, but can also be added before condensation / aggregation / complexation of the solution with dissolved proteins. Higher quality also refers, among other things, to the achievable product properties.For example, in one of the embodiments according to the invention, phospholipids and / or glycolipids can adhere to or aggregate with the dissolved proteins during condensation / aggregation / complexation, resulting in a highly homogeneous product of proteins and phospholipids and / or glycolipids. Such a product is characterized by very good protein solubility and excellent interfacial properties, enabling the production and stabilization of improved quality, e.g., food foams and emulsions. A protein fraction with a protein solubility index (PDI) of > 80% is preferred. A protein fraction that enables high foam stability is also preferred.

[0349] Preferred, therefore, are aggregated proteins with low odor and taste and / or low toxin and hazardous substance content, obtainable according to step 5) by a process according to the invention with a protein solubility index (PDI) > 80%. Furthermore, improved storage stability can be achieved by incorporating one or more compounds, i.e., that no sensory changes occur, e.g., during storage. Another aspect of the invention also aims at the production of a storage-stable protein-containing food ingredient. It has been shown that a protein fraction obtainable by condensation / aggregation / complexation of proteins and / or glycolipids and / or phospholipids and / or antioxidants and / or vitamins using one of the processes according to the invention exhibits highly advantageous storage stability.In this context, storage stability means that storage at room temperature does not lead to any functional or sensory changes compared to the initial state over a period of 12 months.

[0350] Surprisingly, cellulose-based fibers were obtained in pure and isolated form in the submillimeter range, ready for immediate use. The three-dimensional spatial structure of the fibers results in a very large surface area with remarkable binding properties. In addition to their enormous water-binding capacity, they also adsorb oleophilic compounds. Surprisingly, the cellulose-based fibers exhibited particularly excellent coating properties with proteins obtained through the extractions according to the invention. This allowed the spatial structures of the cellulose-based fibers, after their extraction by one of the processes described herein, to be completely filled with proteins, resulting in spherical discrete particles with very good solubility.In contrast to a similar coating of cellulose fibers made from chaff or stem pulp with proteins, the adhering proteins detached during drying and after mechanical shearing, whereas this did not occur with the coated cellulose-based fibers.

[0351] Baking trials have demonstrated excellent stabilization of doughs through the addition of cellulose-based fibers, as well as when replacing flour with these fibers. Due to their large surface area, the cellulose-based fibers swell very quickly, resulting in a very pleasant mouthfeel. The cellulose-based fibers obtained and produced according to the invention are completely soft after soaking in water and do not impart any graininess, unlike cellulose fibers produced from chaff or stem pulp, even though these were significantly smaller (with average maximum diameters of < 10⁻⁵ µm) than the cellulose-based fibers.Comparative studies, in which extraction methods according to the prior art or alternative methods for extracting proteins from flours and press residues were carried out, showed that the cellulose-based fibers obtainable and producible with the methods according to the invention, with the properties achievable by one of the methods according to the invention, cannot be obtained by means of these methods.

[0352] Due to their large surface area, cellulose-based fibers are very well suited as stabilizers or carriers for, for example, dissolved proteins, but also dissolved carbohydrates. Furthermore, a stabilization of consistency in cheese production has been observed. Therefore, their use as a fat substitute is also possible. It has also been shown that cellulose-based fibers are excellent as a dietary fiber additive in food preparations. In addition, weight loss was observed in individuals who followed a high-fiber diet prepared with the cellulose-based fibers obtained and produced according to the invention.

[0353] The preferred use is cellulose-based fibers as a low-calorie dietary fiber for human or animal nutrition.

[0354] The use of cellulose-based fibers as a substitute for fats and / or binders in food preparation is preferred.

[0355] Due to the achievable removal of proteins and carbohydrates, the obtainable cellulose-based fibers have no caloric value for humans and, because of their origin and approval as food, can be used as a calorie-free dietary fiber. Low-calorie plant cellulose fibers are produced according to current technology from the husks and stems of various crops, such as corn, wheat, oats, and potatoes, and are used as dietary fiber and as a structuring or thickening agent in the food industry. For this purpose, fibers with a length of 30 to 90 µm and a high length-to-width ratio are produced by finely grinding the plant structural cellulose, a process that requires significant energy input. Furthermore, it is essential to ensure that any externally applied compounds such as pesticides, herbicides, or fungicides are completely removed from the starting material.Due to their origin as a biopolymer optimized for support and retention functions, cellulose fibers are fibers consisting of bundled fibrils and thus differ completely morphologically from the cellulose-based fibers produced according to the invention. Furthermore, the cellulose-based fibers obtainable by the process according to the invention differ in their structural composition, chemical constituents, and original physiological function.It can therefore be assumed that the significantly improved functional and sensory properties found in various food preparations for the cellulose-based fibers produced with the inventive method, compared to cellulose fibers produced from milling husk and stem material, are due to differences in spatial structure as well as different surface properties. Thus, cellulose-based fibers that can be obtained and produced using the inventive method differ from cellulose fibers produced from milling husk or stem material in both their structural and functional properties.

[0356] The lignin-rich husk components, like the cellulose-based fiber components, exhibit large internal surface areas, which account for their enormous water-binding capacity. This makes them particularly suitable for water retention and storage in arable soils. In their dried state, they are exceptionally easy to store and transport. They exhibit optimal miscibility with all soil types tested (e.g., clay, humus). The water absorption and water retention index of all soils tested were significantly increased by the addition of lignin-rich husk components.

[0357] The use of lignin-rich husk particles is preferred for improving the water-binding and retention capacity of cultivation soils. In their dried state, lignin-based husk particles exhibit excellent oil and grease absorption properties and are therefore very well suited for absorbing oils and fats, e.g., from surfaces or from air / gas mixtures containing oils and fats. The absorbed oils and fats do not spontaneously leach from the lignin-based husk particles, and at the same time, the oil- or grease-saturated material does not "clump," thus maintaining very good transportability. Furthermore, it has been shown that the adsorbed oils and fats can be completely removed from the lignin-based husk particles using solvents, and that the particles retain their original capacity to reabsorb oils and fats.Lignin-based shell components have a low bulk density and can be easily permeated by air or gas streams. This has been shown to enable the virtually complete removal of oil and grease droplets from air or gas mixtures containing oil and fat vapors, such as the exhaust air from deep fryers. Therefore, lignin-rich shell components are ideally suited as oil separators or oil absorbers for surface applications or for capturing oil from air / gas mixtures.

[0358] The use of lignin-rich shell parts for the absorption and binding of oils and fats from surfaces and from air / gas mixtures is preferred.

[0359] Reuse of process solutions and procedures

[0360] The processes according to the invention offer a particularly advantageous way to recover, purify, and reuse the liquids used, as well as any unused compounds or those discharged with the product(s). This completely eliminates wastewater streams and the pollution of the environment with organic material. Recycling can occur at various points in the process, both before and after the removal of dissolved substances, and in some cases, even in an unchanged manner, providing synergistic benefits in the respective process step.Furthermore, reuse is particularly resource-efficient, since the process solutions obtained after a separation process still contain the compounds used and / or dissolved products. When this process water phase is reused, the compounds / products can be returned to the process at the same or a different point and thus reused or recovered as a product. This applies especially to the reuse of the clarified process water phase after process step 5), which is obtained after the separation of the condensates / agglomerates / complexes.In this solution, the dissolved amino acids and / or peptides are still present, depending on the process parameters, in a concentration / amount that separates a solution from soluble constituents of the starting material, as found in studies conducted with this process water phase without further purification when reused with an identical starting material. However, it may be necessary to adjust the pH of this recycled process water phase to ensure protonation and / or deprotonation of the compounds used.Surprisingly, it was found that the clarified process water phase of process step 5) is very well suited to achieve a complete removal of dissolved compounds located in the bound water fraction of the cellulose-based fibers and lignin-rich shell fractions when these are rinsed with the clarified process water phase of step 5), thereby completely or almost completely separating the soluble components with the water phase that results from water removal from the rinsed cellulose-based fibers and lignin-rich shell fractions.This advantageously allows, on the one hand, the complete or near-complete removal of soluble constituents from the starting material and, on the other hand, the dissolved soluble constituents to be fed into one of the process steps in a subsequent process run along with the recoverable process water phase, thus making the dissolved constituents recoverable as a product. It was found that residues of condensing agents, which, depending on the process procedure, were still present in the clarified process water phase of process step 5), were no longer present, or nearly so, in these clarified and reused process water phases when this process water phase was used for a rinsing process of the filter residue from process step 3) and after the separation of the process water from the cellulose-based fibers and / or lignin-rich shell components in process step 3-1), depending on the process procedure.

[0361] In another preferred embodiment of the process, the clarified water phase of process step 5) is first purified in process step 6).

[0362] It was demonstrated that by using the clarified process water phase of process step 5) and the clarified and purified process water of process step 6) for rinsing the cellulose-based fibers and / or lignin-rich shell components in the sidestream process step 3-1), dissolved amino acids and / or peptides, which are flushed into the process water phase by the rinsing process in the bound water component of the cellulose-based fibers and lignin-rich shell components and thus enter the obtainable process water phase, which is obtained after dewatering the cellulose-based fibers and / or lignin-rich shell components, were present in a significantly higher concentration than was the case in the initially used clarified and / or clarified and purified process water phase.Furthermore, small amounts of condensed proteins were present in the resulting process water phase, and the concentration of condensing agents was either undetectable or only measurable at minimal levels. Preferably, this process fluid, low in condensing agents and rich in amino acids / peptides and proteins, is used as the aqueous phase in subsequent process steps 2a) and / or 2b) or 2). This process minimizes the loss of recoverable products, particularly the constituents of the starting material, the dissolved amino acids and / or peptides used in the process, and the condensing agents, thus avoiding wastewater streams contaminated with organic components.

[0363] The clarified and / or purified process water phases are stored in storage containers (V 5a and V 5b, according to Scheme 1) under suitable conditions until they are reused. Suitable conditions may include, for example: cooling, UV irradiation, exposure to a protective gas, or darkening.

[0364] A preferred method is one in which the process fluids are completely recycled and reused for the process.

[0365] It was demonstrated that the process water phases obtained, for example, after the bypass process step 3-111) can be reused without further purification in process steps 2a) and / or 2b), or 2) and / or 3) on the one hand, and / or in process step 3-1) on the other, by adding the clarified or clarified and purified process water phases to the reaction mixture(s) of these process step(s). Even with repeated reuse, no changes occurred in the process parameters or the product qualities obtained. It is also advantageous that the costs for disposing of the process water are eliminated. Furthermore, it is advantageous that both the compounds / substances used for separating the starting material and the condensing agents, and possibly other components, can be reused.Any remaining dissolved proteins or other organic compounds can be reintroduced into the process and thus recovered or obtained as a product from one of the process steps. This significantly contributes to the efficiency of the process.

[0366] The aforementioned process descriptions can also be used to remove compounds that fall under the general category of toxins and substances of concern to health, such as pesticides, herbicides, and insecticides. In a particularly advantageous embodiment, the compounds adsorbed or precipitated from the clarified process water phase can be used for further applications by separating and, if necessary, further purifying them. For example, the precipitated glycolipids and / or phospholipids can be separated from the process water phase by centrifugal separation and subsequently further purified or used directly. In principle, all compounds obtainable from the process fluid can thus be made available for further use.

[0367] In a preferred embodiment of the process, nanofiltration of one or more process water phases is carried out. Preferably, small molecular compounds, such as dyes or carbohydrates, are retained and thereby removed from the process water phase, which is then reused.

[0368] Advantages of the products that can be manufactured and the process technology

[0369] The inventive method makes it extremely advantageous to both completely break down plant starting materials into their main constituents and to obtain pure fractions of these constituents, with improved product properties compared to prior art products.

[0370] The process steps according to the invention enable the recovery of pure phases of the ingredients, such as proteins, carbohydrates, fibers, and shell components, in a low-energy closed-loop process in which the compounds used for product manufacturing are almost completely recovered from the various process steps and reused both during the same process and in subsequent applications. This also applies to the process water phases used.

[0371] Particularly advantageous is the production of pure products. The process allows the production of protein fractions with a high protein content, comparable to that of a concentrate or isolate. Furthermore, functionalized proteins with improved product properties, such as higher water solubility, high foaming capacity, or improved emulsifying properties, can be produced using the processes according to the invention. In particular, hydrated proteins can be produced that can be combined with other compounds within a physiological pH range. Moreover, the process techniques enable the recovery of complex undissolved and dissolved carbohydrates, which can then be used directly.Furthermore, the process technologies make it possible to obtain and separate cellulose-based fibers and lignin-rich shell components that are free of residues of other constituents, such as proteins or carbohydrates, and thus acquire special product properties. For example, the obtainable cellulose-based fibers and lignin-rich shell components exhibit a very high water and oil binding capacity. The latter, in particular, are therefore especially suitable for improving the soil quality of arable land. The obtainable cellulose-based fibers, which can be obtained according to one of the processes according to the invention, can be used in many areas of life. They are particularly suitable as substitutes and / or supplements in food products or preparations, especially as substitutes for sugar, flour / starch, or fats / oils.This results in a very broad range of applications in food preparation and as a food additive. Furthermore, the available cellulose-based fibers are suitable for formulation and stabilization in applications for skin and mucous membranes, as well as for the cultivation and production improvement of microorganisms.

[0372] Furthermore, the process according to the invention enables the production of protein fractions with high product quality. Protein fractions are obtained that are low in taste and odor or completely free of odor or flavor substances. In particular, they contain no bitter substances or other compounds that are perceptible as off-flavors. Furthermore, toxins or harmful compounds present in the biogenic starting materials can be dissolved and removed without entering the obtainable protein fraction. The same process can also be used to remove the oil from the starting material, yielding the separated oil fraction. Moreover, the process allows for the recycling of digestion compounds and process water for repeated applications, thus enabling economical process operation.Furthermore, compounds that are only present in low concentrations in the aqueous digestion solution can also be removed using the provided methods and recovered for further applications.

[0373] A process is therefore particularly preferred in which, in step 2b) and / or 3) and / or 4), a separation of lipophilic constituents of the starting material takes place by additionally adding one or more lipophilic compound(s) to the reaction mixture in step 2a) and / or 2b) and mixing with it, and / or by de-oiling plant proteins at room temperature and / or elevated temperature.

[0374] It was demonstrated that the presence of soluble organic compounds in and on cellulose-based fibers significantly impairs the achievable product quality. Specifically, a protein content of > 0.5 wt% was found to cause a noticeable reduction in water absorption after prior drying of the fiber mass. This is most likely due to the remaining proteins, which exhibit hydrophobic properties in the dried state, causing the surfaces of the cellulose-based fibers to stick together. Depending on the amount of protein remaining in the fiber mass, the dried fibers were no longer swellable in water and exhibited an unpleasant mouthfeel when consumed. This was generally not the case when product phase 2 was post-treated with process water phase 1.It was found that the protein content of the fiber mass could be significantly reduced by process water phase 1, to a considerably greater extent than with a fresh water phase added in the same volume. This result correlated with the reduction of the residual protein content of the subsequently dewatered fibers. Therefore, the use of process water phase 1 for the post-treatment of product phase 2 is particularly advantageous and simultaneously enables the production of sensorially flawless cellulose-based fibers. Furthermore, it was found that the process water phase used for the post-treatment of product phase 2 becomes enriched with the proteins extracted from the fiber mass during this treatment step, and the pH of the solution is raised to a neutral to slightly alkaline range. Therefore, neutralization of this process water phase is not necessary before its reuse in steps 2a) and / or 2b).It was found that, over the course of three or more process cycles, reusing the process water phase 1 after treatment of the product phase 2 in process step 2a) leads to a reduction in the concentration of amino acids in the supplied digestion solution, as these compounds become concentrated. Thus, an improvement in the process economy of the inventive process can also be achieved by saving on digestion compounds. Furthermore, it was shown that the process water phase 1, after use for purifying the product phase 2, is suitable for diluting the water phase in process step 4). Dilution of the water phase is particularly advantageous when a very small volume of water was used in the preceding process steps and a high protein concentration is present.The sedimentation of the organic compounds initiated by the aggregation compounds is then slow, as is the dewatering of the separated aggregate phase in step 5). By adding the process water phase, obtained after the purification of product phase 2 in step 2b), the concentration of the aggregable compounds can be adjusted to ensure optimal aggregation by the aggregation compounds. This can be achieved without additional water consumption and without the otherwise necessary addition of a basic compound or recycling of aggregable organic compounds. This results in further advantageous effects on process economy.

[0375] Definitions:

[0376] Plant-based raw materials

[0377] The term "starting materials," as used herein, encompasses all biogenic products containing one or more of the main constituents: proteins, carbohydrates, fiber / shells, or fats / oils. In principle, the starting materials may contain any proportion of the main constituents as well as other components and compounds. The preferred starting materials are plant-based, such as seeds, grains, kernels, nuts, beans, beets, tubers, vegetables, fruits, or roots. These may be in the form of immature, ripe, mature, overripe, aged, or damaged starting materials. The particularly preferred plant-based starting materials are non-lignified, meaning they contain a low proportion of lignin. Specifically, the non-lignified plant materials referred to herein have a lignin content of less than 10% by weight.Contaminated or spoiled plant materials are also suitable. The term "non-lignified," as used here, refers to a protein-containing biogenic starting material with a lignin content of less than 10% by weight. Lignification is the process of lignin deposition in the cell walls of plants.

[0378] The term "biogenic", as used herein, is defined as follows: of biological or organic origin, produced by life or by living beings.

[0379] The plant-based starting material can be in completely intact form, damaged, crushed, peeled, pressed, ground, or otherwise disintegrated. This includes grits or flours, such as those produced after mechanical oil extraction, known as press cakes. It also includes starting materials, and in particular plant-based starting materials, that have previously undergone a thermal and / or liquid extraction process, e.g., with an alcohol or an organic solvent such as hexane. Furthermore, it includes plant-based starting materials that have undergone thermal treatment. Finally, it includes plant products obtainable from a pulping and / or fermentation process, especially residues such as brewery residues (e.g.,...).in the form of spent grain or spent grain flour) or pomace from cider production, or olive pomace, or beet pulp. Furthermore, residues of cocoa beans. Additionally, residues of vegetable or fruit preparations, such as the core of cabbage vegetables or peels, e.g., from potatoes.

[0380] Furthermore, residues from press residues, such as those obtained during the production of juices (e.g. apple, tomato or carrot juice) or pomace, e.g. of grapes or apples, or extracts such as those obtained during the production of jellies or liqueurs (e.g. blackberry jelly, cassis), are preferred.

[0381] Furthermore, peeling, revetting or coring products from plant-based raw materials can be used.

[0382] This definition includes, in particular, all plant seeds, such as flaxseed, poppy, chia, amaranth, chili, tomatoes, anise, and field peas; grains, e.g., from rapeseed, camelina, oats, hemp, wheat, buckwheat, rye, barley, corn, sunflowers, green spelt, and jatropha; kernels, e.g., from apples, pears, grapes, oranges, cherries, plums, apricots, peaches, serviceberries, medlars, mirabelle plums, rowan berries, pumpkins, melons, and avocados; beans, such as soybeans, broad beans, moth beans, mung beans, or kidney beans, peas, lentils, such as duckweed, lupins, and sesame; vegetables, such as cauliflower, broccoli, kohlrabi, celery, zucchini, peppers, artichokes, or okra; and root vegetables, such as carrots or sugar beets. Fruits such as apples, pears, quinces, bananas, breadfruit, mango, kiwi, passion fruit, melons, passion fruit, figs, pumpkin, pineapple, avocado, olives, mango, chayote, guava, papaya, tamarillo, marmay apple, grapefruit, oranges, lemons or grapes;Berries such as rosehips, gooseberries, blueberries, blackberries, strawberries, elderberries, currants, cranberries, mulberries, chokeberries, raspberries, blackberries, and sea buckthorn; also tubers and roots such as potatoes, beetroot, sweet potatoes, turmeric, cassava, horseradish, celery, radishes, ginger, araqash, taro, wasabi, yacon, black salsify, asparagus, parsnips, turnips, Jerusalem artichokes, cattails, swedes, Siberian angelica, yam, sunflower root, devil's claw, or ginkgo; likewise cucumbers such as salad or gherkins, and also eggplants or zucchini; nuts such as almonds, hazelnuts, peanuts, walnuts, cashews, Brazil nuts, percan nuts, pistachios, chestnuts, marrons, dates, or coconuts. Also sugar cane. Dried raw materials are preferred. Pre-shredding by a mechanical process is preferred. A GMO-free plant-based starting material for the production of GMO-free products is preferred.

[0383] Proteins

[0384] The term "proteins," as used herein, refers to macromolecules composed of amino acids linked together by peptide bonds. The proteins referred to here contain more than 100 amino acids. They can exist in their primary, secondary, or tertiary structure, as well as in a functionally active form. The secondary structure can have a spatial geometry such as an α-helix, β-sheet, β-loop, or be disordered as anatomical coil structures. Also included are supramolecular compounds of proteins, such as collagen, keratin, enzymes, ion channels, membrane receptors, genes, antibodies, toxins, hormones, or coagulation factors.Due to their ubiquitous occurrence in all life forms and environments, the proteins referred to herein can be macromolecular compounds in one of the specified forms, whose physiological function was, for example, shaping, supporting, transporting, or defending, or serving for reproduction, energy production or metabolism, or promoting / transforming reactions. This includes, in particular, proteins according to the given definition that can be extracted from the starting materials described herein.

[0385] carbohydrates

[0386] The term "carbohydrates," as used herein, encompasses all sugar molecules from C3 to C6, as well as compounds composed of these molecules. This includes, but is not limited to: monosaccharides, such as hexoses (including glucose and fructose), pentoses (including ribose and ribulose), and trioses (glyceraldehyde and dihydroxyacetone); disaccharides, such as maltose, sucrose, and lactose; and polysaccharides, such as dextrans, cyclodextrins, starch, and cellulose. A distinction must be made between amylose and amylopectin in the case of starch.

[0387] While monosaccharides, disaccharides, and some polysaccharides are water-soluble, higher molecular weight carbohydrates are water-insoluble. Higher molecular weight carbohydrates, which are preferably linked to one another via alpha-1,4-glycosidic and / or alpha-1,6-glycosidic bonds, are classified here as complex carbohydrates. Besides starch and cellulose, these include, among others, glycogen, chitin, callose, fructans, and pectins. This category also encompasses complex structures composed of carbohydrate agglomerates, such as a starch granule.

[0388] Cellulose-based fibers

[0389] The term “cellulose-based fibers”, as used herein, encompasses all corpuscular structures of plant starting materials consisting of a primary cellulose backbone that exhibit at least 2 of the following characteristics:

[0390] - an origin from a plant-based starting material

[0391] - an aspect ratio of a longitudinal and transverse diameter of 1:1 to 1,000:1

[0392] - a water binding capacity of > 200 wt%

[0393] - a proportion of chemical compounds and functional groups of > 2.5 wt% that do not correspond to the elements C, H or O.

[0394] The cellulose-based fibers according to the invention exhibit three-dimensional spatial and surface structures. They can exist in a composite structure that can be divided into spherical or particulate fragments by physical means, such as mechanical comminution and / or thermal treatment. This can be verified in a decompacted state of the cellulose-based fibers using analytical methods.

[0395] The cellulose-based fibers can already be present in a loosely compacted composite with other compounds or components, such as in a matrix that has been broken apart by a pressing or impact process, as is the case with pressed oilseeds or ground grains, or they can be present in a stable composite structure that prevents the cellulose-based fibers from being released, as is the case, for example, with vegetables or fruits. The fibers falling under this definition are characterized by structural features and physical properties that they share. In particular, they exhibit spatial structures in the form of free fibers, networks, or spatial tissue structures, which become microscopically visible after decompacting and hydrating. The decompacted cellulose-based fibers according to the invention preferably have a planar and / or corpuscular geometry.In particular, they are characterized by a low fiber length weight, or coarseness, which is preferably < 70 mg / 100 m, more preferably < 50 mg / 100 m, more preferably < 30 mg / 100 m, and even more preferably < 20 mg / 100 m, more preferably < 15 mg / 100 m, and most preferably < 10 mg / 100 m. They can encapsulate, surround, or contain pigments, or these can be structural components of the fibers according to the invention. Other organic or inorganic compounds can also be components of the cellulose-based fibers or be permanently bonded to them in an aqueous medium.

[0396] The decompacted cellulose-based fibers obtained by process step 3) or 3-111 exhibit these properties, which can be verified using state-of-the-art methods.

[0397] Lignin-rich shell components

[0398] The term "lignin-rich hull components," as used herein, encompasses all cladding and supporting structures of the plant starting material that have a lignin content of > 30 wt%. Preferred lignin-rich hull components have a lignin content of > 40 wt%, more preferably > 50 wt%, further preferably > 60 wt%, and even more preferably > 80 wt%. They have no specific external shape, ranging from flat and polymorphic to corpuscular and round. Their dimensions depend on the manufacturing process and can range from a few micrometers to several millimeters. Lignin-rich hull components are present, for example, in the press residues of rapeseed or jatropha seeds at a wt% of 8 to 15 wt%.

[0399] Oils / fats

[0400] The term "oils / fats" encompasses all lipid compounds present in the starting material. Preferred lipid compounds include aryl glycerides, particularly mono-, di-, and triglycerides; carboxylic acids, especially free fatty acids and fatty acid compounds such as fatty acid methyl esters; glycolipids and glyceryl glycolipids; and hydrocarbon compounds with a carbon number > 5.

[0401] Disintegration

[0402] The term "disintegration" encompasses all processes that lead to the separation of water-impermeable tissue structures or textures of the starting material, thereby enabling complete contact of the main constituents contained therein with an aqueous solution according to the invention, containing disintegration compounds. This definition thus includes all processes that create cracks, gaps, or fissures in the covering or shell materials of the plant starting material, up to and including complete disintegration with exposure of the surfaces of the constituents of the plant starting material. Crucially, disintegration enables the wetting of the surfaces of the constituents of the plant starting material with the dissolved compounds for the separation of the starting material.A disintegration, by definition, is therefore synonymous with making the constituents of the starting material wettable for the aqueous digestion solutions and the compounds contained therein.

[0403] Aqueous digestion solution

[0404] The term "aqueous digestion solution" herein refers to an aqueous solution of dissolved compounds for the separation of constituents of the starting material. In a preferred embodiment of the process, the compounds for the separation of constituents of the starting material are one or more amino acids and / or peptides present in water in a completely dissolved form. In a particularly preferred embodiment, the dissolved amino acids and / or peptides are dissolved cationic amino acids and / or peptides. The water may be clarified, clarified and purified process water, deionized, partially deionized, well water, or municipal water. The preferred compounds present in dissolved form for the separation of constituents of the starting material are naturally occurring amino acids and / or peptides consisting of or containing these amino acids.The particularly preferred compounds, which are present in solution for the separation of constituents of the starting material, are naturally occurring amino acids and / or peptides consisting of or containing these amino acids. The aqueous digestion solutions according to the invention are preferably solutions of one, two, or more amino acid(s) and / or peptide(s) present in the individual and / or total concentration in a range of 10 μιμιον to 3 mol / l, more preferably between 1 mol / l and 1 mol / l, and further preferably between 0.1 mol / l and 0.5 mol / l. These can be L- or D-forms or racemates of the compounds. The use of the L-form is preferred. The amino acids arginine, lysine, and histidine are preferred. Derivatives of the aforementioned amino acids are also preferred. Cationic amino acids and peptides with cationic groups are particularly preferred.The peptides that can be used according to the invention can be di-, tri-, and / or polypeptides. The peptides according to the invention have at least one functional group that binds or can bind a proton. The preferred molecular weight is below 500 kDa, more preferably < 250 kDa, further preferably < 100 kDa, and particularly preferably < 100 kDa. The preferred functional groups are, in particular, a gunanidine, amidine, amine, amide, hydrazino, hydrazono, hydroxyimino, or nitro group. The amino acids can have a single functional group, several of the same class of compounds, or one or more functional groups of different classes of compounds. Preferably, the amino acids and peptides according to the invention have at least one positive charge group or have an overall positive charge.Particularly preferred peptides contain at least one of the amino acids arginine, lysine, histidine, and glutamine in any number and sequential order. Particularly preferred are amino acids and / or derivatives thereof containing at least one guanidino and / or amidino group. The guanidino group is defined as the chemical residue H₂N-C(NH)-NH— and its cyclic forms, and the amidino group as the chemical residue H₂N-C(NH)— and its cyclic forms. These guanidino and amidino compounds preferably have a partition coefficient K₀w between n-octanol and water of less than 6.3 (K₀w < 6.3). Arginine derivatives are particularly preferred. Arginine derivatives are defined as compounds comprising a guanidino group and a carboxylate group or an amidino group and a carboxylate group, wherein the guanidino group and carboxylate group or the amidino group and the carboxylate group are separated by at least one carbon atom, i.e.At least one of the following groups is located between the guanidino group or the amidino group and the carboxylate group: -CH2-, -CHR-, -CRR'-, where R and R' independently represent any chemical residues. Of course, the distance between the guanidino group and the carboxylate group or the amidino group and the carboxylate group can also be more than one carbon atom, for example in the following groups -(CH2)n-, -(CHR)n-, -(CRR')n-, with n = 2, 3, 4, 5, 6, 7, 8, or 9, as is the case, for example, in amidinopropionic acid, amidinobutyric acid, guanidinopropionic acid, or guanidinobutyric acid. Compounds with more than one guanidino group and more than one carboxylate group include, for example, oligoarginine and polyarginine. Other examples of compounds that fall under this definition are guanidinoacetic acid, creatine, and glycocyamine.

[0405] Preferred compounds share the general formula (I) or (II) as a common feature.

[0406]

[0407] Formula (I) Formula (II)

[0408] Where

[0409] R, R', R", R'" and R"" independently of each other -H, -CH=CH2, -CH2-CH=CH2, -C(CH3)=CH2, — CH— CH — CH3, — C2H4- CH— CH2 / — CH3, — C2H5, — CgHy, — CH(CH3)2 ; — C4.H9, — CH2 — CH(CH3)2 ; -CH(CH3)-C2H 5, -C(CH3)3, -C5H n , -CH(CH3)-C3H7, -CH2-CH(CH3)-C2H5, -CH(CH3)-CH(CH3)2, -C(CH3)2-C2H5, -CH2-C(CH3)3, -CH(C2H5)2, -C2H4-CH(CH3)2, -C6H 13 , -C7H 15 , Cyclo-C3H5, cyclo-C4H7, cyclo-CsHg, Cyclo-C6H u,-CECH, -CEC-CH3, -CH2-CECH, -C2H4-CECH, -CH2-CEC-CH3 represent, or ' and R" together form the residue -CH2-CH2-, -CO-CH2-, -CH2-CO-, -CH=CH-, -CO-CH=CH-, -CH=CH-CO-, -CO-CH2-CH2-, -CH2-CH2-CO-, -CH2-CO-CH2- or -CH2-CH2-CH2-; X represents -NH-, -NR""-, or -CH2- or a substituted carbon atom; and

[0410] L represents a C x up to C8 linear or branched and saturated or unsaturated carbon chain with at least one substituent selected from the group comprising or consisting of -NH2, -OH, -PO3H2, -PO3H " , -PO3 2" , -OP03H2, -OPO3H " , -OP03 2" , -COOH, -COO " , -CO-NH2, -NH3 + , -NH-CO-NH2, -N(CH3)3 + , -N(C2H5)3 + , -N(C3H7)3 + , -NH(CH3)2 + , -NH(C2H5)2 + , -NH(C3H7)2 + , -NHCH3, -NHC2H5, -NHC3H7, -NH2CH3 + , -NH2C2H5 + , -NH2C3H7 + , -S03H, -S03 ", -S02NH2, -C(NH)-NH2, -NH-C(NH)-NH2, -NH-COOH, or It is preferred that the carbon chain L is in the range from C1 to C7, more preferably in the range from C1 to C6, and further preferably in the range from C1 to C6. x up to C5, and preferably in the range of C x up to C4.

[0411] Preferably L represents -CH(NH2)-COOH, -CH2-CH(NH2)-COOH, -CH2-CH2-CH(NH2)-COOH, -CH2-CH2-CH2-CH(NH2)-COOH, -CH2-CH2-CH2-CH2-CH(NH2)-COOH, or -CH2-CH2-CH2-CH2-CH2-CH(NH2)-COOH.

[0412] Compounds of general formula (III) as shown below are also preferred: where the remainders X and L have the meanings revealed herein.

[0413] Digestion solutions according to the invention may contain further compounds that are completely dissolved therein. These may be compounds for adjusting the pH of the solution, in particular an acid or base, such as urea or triethylamine, or acetic acid or uric acid, or compounds with surfactant properties, such as DMSO or SDS. Furthermore, stabilizers, such as antioxidants or reducing agents, may be included. Compounds that enable the disinteraction of constituents of the starting material are also preferred; compounds from the group of sulfites and sulfates are particularly favored. These are preferably present in the digestion solution at a concentration between 0.01 and 30 wt%.

[0414] Also suitable are di-, tri-, or oligopeptides, as well as polypeptides composed of one, two, or more amino acids. Short-chain peptides, e.g., RDG, are preferred. Particularly preferred are peptides consisting of amino acids possessing both hydrophobic and hydrophilic side chains, such as (listed alphabetically by amino acid name) GLK, QHM, KSF, ACG, HML, SPR, EHP, or SFA. Peptides possessing both hydrophobic and cationic and / or anionic side chains, such as DG, BCAA, NCR, HIS, SPR, EHP, or SFA, are also particularly preferred. Further examples with four amino acids are NCQA, SIHC, DCGA, TSVR, HIMS, or RNIF, or with five amino acids are HHGQC, STYHK, DCQHR, HHKSS, TSSHH, and NSRR. RDG, SKH, or RRC are particularly preferred.

[0415] Aqueous process mixture

[0416] The term "aqueous process mixture" or the synonymous terms "process mixture" or "reaction mixture" refers to an aqueous solution, emulsion, suspension, or solids with a water content of < 20 wt%. The solids can be in a fully hydrated state or in a barely wetted state. Specifically, this refers to mixtures produced by an aqueous solution used in the process, the starting material, and the intermediate and end products obtained during the process from the separated constituents and components.

[0417] reaction vessel

[0418] The term “reaction vessel” or “reaction container” refers to containers in which aqueous process mixtures / reaction mixtures are produced by contacting, combining or mixing aqueous solutions used in the process flow with the starting material and the intermediate and end products obtained during the process from the constituents and components separated from it.

[0419] Distribution solution

[0420] The term "partitioning solution," used synonymously with "partitioning volume" herein, refers to an aqueous phase added to a reaction mixture that enables the distribution and separation of soluble, dissolved, soluble solid, and complex insoluble components of the starting material. In a distribution volume according to the invention, these components are present in a readily separable form. The presence of a sufficiently large distribution volume can be verified by taking a sample and determining the separability of the dissolved and suspended components using techniques and methods as described herein.

[0421] Condensation / Aggregation / Complexation

[0422] The terms "condensation / aggregation / complexation" encompass all physical and / or chemical processes that lead to the combination of similar and / or dissimilar organic and / or inorganic compounds, resulting in condensates, aggregates, or complexes that can be separated from the aqueous phase of an aqueous process mixture as solids using suitable separation methods. The term "condensate" refers to a spatial approximation of macromolecular structures, forming a measurable three-dimensional structure. The bonding forces are electrostatic, resulting from hydrophobic or hydrophilic interactions. In general, "aggregation" means the accumulation or aggregation of atoms, molecules, and / or ions into a larger unit, the aggregate. This accumulation or aggregation is caused by van der Waals forces, hydrogen bonding, and / or other types of chemical or physicochemical bonding.In this context, "complexes" are understood to be macroscopically visible formations that are linked together by condensates and / or aggregates to form a larger composite structure. Due to the low bond energies of the condensates / aggregates and complexes, the individual compounds can be easily extracted from the composite structures, for example, through a mixing process, and isolated. In contrast, coagulates are three-dimensional structures of small- to macromolecular compounds that arise from a chemical reaction in which covalent bonds between the molecular structures are formed and / or broken. In a coagulate, the individual compounds cannot be separated or isolated from one another, or only to a limited extent, by a dissolution process in water.The condensation / aggregation / complexation referred to here is distinct from coagulation, which occurs primarily through a precipitation reaction with a (strong) acid, resulting in denaturation where at least part or all of the original tertiary structure of the proteins is no longer present. This is recognizable, for example, by a reduced water-binding capacity.

[0423] Condensant

[0424] The terms "condensing agent" or "aggregating agent" are used here to refer to one or more organic and / or inorganic compounds that initiate, maintain, and / or accelerate the condensation, aggregation, or complexation of constituents / compounds dissolved in water within an aqueous process mixture. They may exert, among other effects, a catalytic, destabilizing, displacing, and / or releasing effect on the constituents to be condensed, aggregated, or complexed, leading to a combination of these constituents / compounds. The compounds may also cause this effect by altering the pH and / or salinity and / or may themselves participate in the aggregation process.

[0425] Organic compounds

[0426] The term organic compounds encompasses all organic compounds of biogenic origin that can be extracted from biogenic starting materials using one of the methods described herein. Corresponding to the different possible origins, organic compounds from various substance groups are found, occurring individually, but mostly in different combinations and in varying proportions.Therefore, only the essential groups of substances to which organic compounds can be assigned are listed below, without being limited to them: waxes, wax acids, lignins, hydroxy and mycolic acids, fatty acids with cyclic hydrocarbon structures, such as shikimic acid or 2-hydroxy-1-cycloheptylundeicanoic acid, mannosterylerythritol lipid, pigments such as carotenes and carotenoids, chlorophylls, and their degradation products, as well as phenols, phytosterols, in particular β-sitosterol and campesterol, as well as sigmasterol, sterols, sinapines, and squalene. Phytoestrogens, such as isoflavones or lignans. Furthermore, steroids and their derivatives, such as saponins, as well as glycolipids, glycoglycerolipids, and glycerosphingolipids, as well as rhamnolipids, sophrolipids, trehalose lipids, and mannosterylerythritol lipids.Likewise, polysaccharides, including pectins such as rhamnogalacturonans and polygalacturonic acid esters, arabinans (homoglycans), galactans and arabinogalactans, as well as pectic acids and amidopectins. Also included are phospholipids, in particular phosphotidylinositol, phosphatides such as phosphoinositol, long-chain or cyclic carbon compounds, fatty alcohols, hydroxy and epoxy fatty acids. Likewise, glycosides, lipoproteins, lignins, phytate or phytic acid, and glucoinosilates. Proteins, including albumins, globulins, oleosins, vitamins such as retinol (vitamin A), and derivatives such as... B. Retinoic acid, riboflavin (vitamin B2), pantothenic acid (vitamin B5), biotin (vitamin B7), folic acid (vitamin B9), cobalamins (vitamin B12), calcitriol (vitamin D) and derivatives, tocopherols (vitamin E) and tocotrienols, phylloquinone (vitamin K) and menaquinone. Also tannins, terpenoids, curcuminoids, xanthones.But also sugar compounds, amino acids, peptides, including polypeptides, and carbohydrates such as gluconeogenesis. Also included are related carboxylic acids, flavorings (or odor and taste substances), colorants, phospholipids and glycolipids, waxes (or wax acids), and fatty alcohols.

[0427] Odor and flavor compounds

[0428] The terms odorant and flavoring agent are used synonymously with flavoring agent here. Organic compounds that lead to sensory perception in the form of taste or smell are present in virtually all organic mixtures of biogenic origin. There is an extremely high degree of heterogeneity among the possible organic compounds. The structural composition of these carbon-based compounds is diverse. Some typical classes of compounds are alkaloids, alcohols, aldehydes, amino acids, aromatic hydrocarbons, esters, lactones, cyclic ethers, furans, furanoids, free fatty acids, flavonols, glycosides, ketones, saturated and unsaturated hydrocarbons, enamine ketones, ketopiperazines, isoprenoids, monoterpenes, terpenes, cyclic terpenes, triterpenes, triterpenoids, tetraterpenes, sesquiterpenes, sesquiterpenoids, sterols, phytosterols, purine derivatives, and phenylpropanoids.Phenols and / or hydroxycinnamic acid derivatives. These classes of compounds can occur individually or in any combination. These include in particular 1,5-octadien-3-ol, butanal, hexanal, octanal, nonenal, nonadineal, decanal, dodecanal, piperonal, cysteine, cystine, methionine, phenantrene, anthracene, pyrene, benzopyrene, 4-hydroxybutyric acid, ethyl hexanoate, coumarin, maltol, diacetylfuran, pentylfuran, perillense, rosenfuran, caprylic acid, capric acid, hydroxy fatty acids, amygdalin, progoitrin, 2-heptanone, 2-nonanone, decatrienal, 10cten-3-one, vinyl amyl ketone, 4-(4-hydroxyphenyl)-butan-2-one, mycosporin, diketopiperazine, humulones and lupulones (bitter acids), mono-terpenes: myrcene, ocimene and cosmene, linalool, Myrcenol, Ipsdienol, Neral; Citronellol and Geranial, Citronellal, Myrcene, Limonene, Linalool, Nerol, Geraniol, Terpinolene, Terpinene and p-Cymene, Carvone and Carvenone, Thymol, Dihydroxycarveol, 2-Pinene, α and β-Pinene, Limonene, Phellandrene, MenthaneCamphor; fenchone, xanthophyllins, bisabolanes, germacranes, elemanes and humulanes, farnesenes, rotundone, sterols, phytosterols; also p-cresol, guaiacol, ferulic acid, lignin, sinapine, catechins, eugenol, vanillin, 3-butenyl isothiocyanate, 4-petenyl isothiocyanate, 4-pentenitrile, 5-hexenitrile, camphene, dodecane, cinnamyl alcohol, fenchyl alcohol, 1R,2S,5R-isopulegol, 2-ethylfenchol, menthol, 4-hydroxy-3,5-dimethoxybenzyl alcohol, (R)-(-)-lavandulol

[0429] Piperonyl alcoholjhujyl alcohol, 1,8-cineole, 4-ethylguaiacol, N-[[(lR,2S,5R)-5-methyl-2-(l-methylethyl)cyclohexyl]carbonyl]-glycine ethyl ester, (lR,2S,5R)-N-cyclopropyl-5-methyl-2-isopropylcyclohexanecarboxamide, L-alanine, aspartic acid, 2,4-Dimethylthiazole, Lenthionine, (+)-Cedrol, 3-Methylphenol, Anisole, l-Methoxy-4-propylbenzene, 4-Allyl-2,6-dimethoxyphenol, 2,6-Dimethoxy-4-vinylphenol, Ethyl-4-hydroxy-3-methoxybenzyl ether, Vetiverol, 2-Butylethyl ether, Ethylgeranyl ether, Carvacrol, 2-methylpropanal, cinnamaldehyde, p-toluene aldehyde, 2-Methylbutyraldehyde, salicylaldehyde, acetic acid, lactic acid, 3-methylbutyric acid, hexanoic acid, 1-malic acid and / or anethole. These compounds can occur individually or in any combination.

[0430] Plant pigments and dyes

[0431] The term "dyes" encompasses organic compounds that typically occur in varying quantities and compositions in source materials of biogenic origin. Within this context, the term "plant pigments" refers to all color-imparting compounds. The most dominant pigment, and by far the most abundant in plant oils, is the group of chlorophylls and their degradation products, such as pheophylins, chlorophyllides, pheophorbides, phyropheophytins, chlorins, rhodines, and purpurins. Compounds classified as carotenes or carotenoids are also present. Other classes of compounds are also found, including flavonoids, curcumins, anthrocyanins, betaines, xanthophylls (which include carotenes and lutein), indigo, kampnerol, and xanthophyllins such as neoxanthin and zeaxanthin.These dyes can be present in different proportions in the lipid phases.

[0432] Phospholipids

[0433] The term "phospholipids," as used herein, includes amphiphilic lipids containing a phosphate group, belonging either to the phosphoglycerides or the phosphosphingolipids. It also includes acidic glycoglycerolipids, such as sulfoquinovosyl diacylglycerol or sulfoquinovosyl diacylglycerol. Phosphoglycerides (also called glycerophos-pholipids or phosphoglycerolipids) consist of a diacylglyceride whose remaining terminal hydroxyl group is bonded to a phosphate group, which is either unmodified (phosphatidic acid) or esterified with an alcohol. The most common representatives of the latter group are phosphatidylcholines (also called lecithins), phosphatidylethanolamines, and phosphatidylserines. "Glycophosphatidylinositols" are compounds that are saccharide glycosidically linked to the inositol group of phosphatidylinositols.

[0434] Glycolipids

[0435] The term "glycolipid", as used herein, encompasses compounds in which one or more monosaccharide residue(s) are linked to a hydrophobic acyl residue via a glycosidic bond.

[0436] Glycoglycerolipids

[0437] The term glycoglycerolipids used herein refers to phosphoglycosphingolipids, phosphonoglycosphingolipids, glycosphingolipids, sulfoglycosphingolipids, sialoglycosphingolipids, mono-, oligo-, and polyglycosylsphingoids, and mono-, oligo-, and polyglycosylceramides. Further examples include rhamnolipids, sophorlipids, trehalose lipids, and lipopolysaccharides.

[0438] Residual moisture content

[0439] The residual moisture content is determined by measuring the difference in weight between an initial measurement and a measurement after complete drying in a vacuum oven. The determined value is expressed as a percentage relative to the initial weight. Alternatively, automated methods for determining the moisture content can be used. Clarified aqueous phase

[0440] In this context, a "clarified aqueous phase" or "clarified process aqueous phase" refers to the aqueous phase obtained after a condensation / aggregation / complexation of organic and / or inorganic components according to the invention, as well as their separation. The term "clarified" refers to an optically clear solution containing no or only isolated suspended solids. This is quantifiable, for example, by turbidity measurement, provided that a value of 20 FTU is not exceeded. The term "clarified" also implies the removal of dissolved organic compounds. Methods that allow for the quantification of any remaining organic compounds include, for example, HPLC and / or MS.

[0441] Purified water phase

[0442] A "purified aqueous phase" is understood herein to mean a clarified aqueous phase or clarified process aqueous phase, as defined herein, in which the reduction of organic and / or inorganic compounds contained therein to < 0.5 wt% has been achieved. This can be verified, for example, by elemental analysis (e.g., ICP) or atomic absorption spectroscopy of a drying residue.

[0443] Process economy

[0444] The term "process-efficient," as used here, means that the execution / management of a particular process offers quantifiable economic advantages compared to other process execution methods. These economic advantages can affect various economic sectors, which may overlap and combine to form an overall process efficiency.

[0445] Inventive process economy is ensured by one or more of the process steps that relate to the utilization / usability of resources and / or energy requirements and / or the avoidance of environmental pollution and / or process costs, and thus affects the following economic areas, without being limited to them:

[0446] Raw material economy - for example, with the inventive method all constituents of the plant starting material can be obtained as valuable material fractions.

[0447] Energy economy - for example, the methods according to the invention can be carried out at room temperature.

[0448] Environmental economics - for example, the aqueous process phases can be completely reused in a particularly advantageous way with the process designs, so that the amount of fresh water and wastewater is considerably lower (> 50 vol%) compared to a process that is not carried out with fresh water in the various process stages according to the invention, and no wastewater with organic loads is produced, which is the case with a process not carried out according to the invention.

[0449] Production cost efficiency – for example, a process implementation according to the invention leads to a reduction in the required digestion compounds and in fresh and wastewater compared to a non-inventive process implementation, so that the total process costs are reduced by > 15%. In addition, the process ensures improved product quality of obtainable products through the reuse of process water phases.

[0450] The process achieves its economic advantages particularly through the reuse, and especially the unlimited reuse, of a clarified aqueous phase. The aspect of "economic efficiency" is particularly significant because the process according to the invention produces no wastewater, i.e., no aqueous phases as waste or aqueous wastewater. This offers a considerable process advantage, especially with regard to costs and environmental impact, given the relatively large volume of aqueous solutions used in the invention.

[0451] Decompacting

[0452] The term "decompacting" refers to the disruption of compacted compounds, resulting in the previously gap-free separation of these compounds in an aqueous medium. Methods

[0453] Method for providing plant-based starting material.

[0454] Depending on the different origins and methods of obtaining the biogenic starting materials usable according to the invention, these can be present in different forms and states. For example, they can be whole / intact seeds, grains, kernels, nuts, vegetables, fruits, flowers, ovaries, or roots, and / or plant materials that are wholly or partially degraded, broken open, crushed, ground, smashed, or pressed, and / or plant materials in which a fermentative or disintegrative process, in particular through autolysis / microbial degradation / physical-chemical reaction, has partially or completely taken place, and / or they are residues from agricultural production / food manufacturing or processing.The broken, divided, crushed, pulverized, liquidated, or dissolved plant starting materials can be in the form of cohesive or fragmented pieces, or compacted, e.g., as pellets or pressed mass, or in a loose form, such as granules or bulk material, or in isolated forms, such as flour or powder, or as a suspension. The consistency, shape, and size of the plant starting materials are generally irrelevant; however, crushed plant starting materials that facilitate digestion are preferred. Preferably, the maximum diameter of the dispersible particles of the biogenic starting materials is between 100 μm and 100 cm, more preferably between 0.5 mm and 50 cm, further preferably between 1 mm and 20 cm, and even more preferably between 2 mm and 5 cm.The form of the suitable plant-based starting materials is arbitrary, as is their consistency, which can be hard or soft, or they can be in a liquefied form. The starting material can be at any temperature; a heated starting material, such as that obtained after a pressing process, is preferred. If the plant-based starting material does not meet the suitable properties / requirements for one of the processes according to the invention, these conditions can be achieved using methods available from the prior art. These include, in particular, methods that enable and / or facilitate the processing of the plant-based starting material according to the invention. These include, in particular, mechanical methods for comminuting the plant-based starting material.For process optimization, it may be necessary to first shred and dry plant material, or to dry it and then shred it. In one embodiment of the process, the shredded and then dried plant material is further reduced to a specific particle size before process step 1). Particle sizes between 1 mm and 2 cm are preferred, and more preferably between 30 mm and 5 mm. In another embodiment, lignin-containing components of the plant materials are first removed. These can be, for example, covering materials of the plant materials, such as skins, husks, or shells, like those of apple or grape seeds. Mechanical methods for this removal are known in the prior art.In a further preferred embodiment of the process, a method for the breakdown and / or dissolution of lignin can be carried out before process step 1). Such methods are known in the prior art, for example as the "Kraft process". For instance, the breakdown or dissolution of lignin is achieved by boiling with an alkali. However, mechanical disintegration can also take place during or after process step 2a). The use of shear mixers or colloid mills is advantageous.

[0455] The starting materials are placed in a suitable container, which can preferably be filled from the top and has a closable outlet at the bottom.

[0456] A preferred method is therefore one in which plant-based starting materials are provided in a container for the additional absorption of a liquid.

[0457] The container must comply with the regulatory requirements for the respective product manufacturing process. This also applies to subsequently used containers, system components, and piping systems. A container design with a conical bottom is preferred. A mixing device for thoroughly blending the container contents is preferred. A cooling / heating device for the container or its contents is also preferred. Preferably, the digestion solution is added to, for example, the press residues / milled products in this container, mixed, and stored for the required time. For use in the next process step, the solution is discharged by draining it through the bottom outlet.

[0458] Methods for the preparation and use of digestion solutions

[0459] The digestion solutions according to the invention are prepared with the compounds according to the invention for the separation of constituents of the starting material, as defined herein. For this purpose, one or more of the compounds are completely dissolved in water, which may be clarified or clarified and purified process water, completely ion-free water, or well water or municipal water. Dissolving the compounds may require increasing the temperature and / or continuing the mixing process for up to two days. Preferably, the pH of the solution of amino acids or peptides is in the range of 7.5 to 13.5, more preferably between 8 and 13, and further preferably between 8.5 and 12.5. This is particularly the case when using cationic amino acids / peptides. In one embodiment, the pH can be adjusted to any desired pH range between 7.5 and 13.5 by adding an acid or a base.Acids and bases known in the prior art can be used.

[0460] Additives may be added to the solutions to improve or accelerate the digestion and recovery of cellulose-based fibers, or to disintegrate and / or dissolve other components of the starting material. Such compounds include, but are not limited to, urea, NH3, triethylamine; ionic or non-ionic surfactants, such as SDS or DMSO; antioxidants, or NaSO3, sodium bisulite, or NaSO4. These compounds may be present individually or in combination in the digestion solution at concentrations between 0.01% w / w and 50% w / w.

[0461] Furthermore, the digestion solutions according to the invention can be provided with additives that particularly improve the solubility of certain compounds of the starting material, including, among others, alcohols, fatty alcohols, fatty acid esters or lactones.

[0462] The digestion solutions can be prepared at any temperature and added to the starting material in process step 2a), or 2), and, if necessary, also in process step 2b). Application can be dropwise, intermittently, or in a jet, continuously or discontinuously, to, into, and / or onto the starting material. In a preferred embodiment, this is carried out under conditions of exclusion of air and / or inert gas. Application is achieved by feeding a prepared digestion solution from a storage container to the starting material in an adjustable quantity via a feed line.

[0463] Methods for the disintegration of starting material.

[0464] For the inventive separation of constituents of the starting material, it is necessary that the compounds according to the invention completely penetrate the starting material and that, subsequently, the constituents are present in a hydrated state, at least at the interfaces. This requires penetrability of the aqueous digestion solution. In the case of insufficient penetrability, a mechanical and / or physicochemical disintegration process can be used. While mechanical disintegration processes should preferably be carried out before or at the time of process step 1, in a preferred embodiment, physicochemical disintegration can take place in process step 2a) or 2). Thermal disintegration is preferred in this case.A temperature of preferably 80°C to 150°C, more preferably between 90°C and 140°C, and further preferably between 99°C and 121°C is preferred. Pressurization occurring simultaneously with heating is preferred; the use of an autoclave for simultaneous heating and pressurization is preferred. In a particularly preferred embodiment, the digestion solutions used in process steps 2a), 2b), and 2) are used for the disintegration of the starting material; the use of amino acid and / or peptide solutions for disintegration, involving mechanical and / or physicochemical disintegration of the starting material, is preferred. A solution containing dissolved cationic amino acids and / or derivatives containing at least one guanidino and / or amidino group is preferred for the physicochemical disintegration of the starting material.Particularly preferred is a solution containing arginine and / or arginine derivatives in dissolved form for the thermal disintegration of starting materials. Also preferred is a digestion solution containing at least one compound comprising urea, NH3, triethylamine; ionic or non-ionic surfactants, such as SDS or DMSO, or NaSO3 or sodium bisulite.

[0465] A preferred method is the disintegration of starting materials with a solution of dissolved amino acids and / or peptides. A particularly preferred embodiment of the process is one in which the dissolved amino acids and / or peptides are dissolved cationic amino acids and / or peptides. In principle, thermal disintegration is advantageous when the plant-based starting material has a high water content, as is the case with fresh fruits and vegetables. Mechanical disintegration is particularly advantageous when the plant-based starting materials have a low water content and / or are enclosed in husks / shells that are impermeable to water. Furthermore, a mechanical process is preferable if another fraction of the plant-based starting material, such as oil, is to be removed first.

[0466] In a preferred embodiment of the process, plant raw materials undergo disintegration by placing the raw material, whole, in parts, or mechanically crushed, into a water bath and heating it until it is so soft that it disintegrates into a pulpy or liquid phase under slight pressure, e.g., by crushing with the fingers. This is particularly advantageous when, due to the different degrees of hardness of various structures, the different structures, such as the mesosperm and the peel, can be easily differentiated and mechanically separated as layers following one of the aforementioned disinteration processes. In a preferred embodiment, the heating is carried out in conjunction with pressure increase in an autoclave.In a preferred embodiment, plant sheath materials are removed before and / or after disintegration of the plant starting material.

[0467] In a particularly preferred embodiment, the plant starting material is disintegrated by immersion in one of the aqueous solutions according to the invention, containing an aqueous digestion solution according to the invention. In principle, the volume or weight ratio can be freely selected; however, it is advantageous if the plant starting material is completely wetted by the digestion solution. The duration of exposure to the digestion solution depends on the plant starting materials used. A duration between 1 minute and 48 hours is preferred, more preferably between 10 minutes and 14 hours, and even more preferably between 20 minutes and 6 hours. The temperature at which the plant starting material is exposed to the aqueous digestion solutions is, in principle, freely selectable.A temperature between 5° and 140°C is preferred, more preferably between 10° and 120°C, and even more preferably between 15° and 90°C. Prior and / or simultaneous and / or subsequent treatment of the plant starting material with compounds that cause disintegration or chemical reaction of lignin compounds is also preferred. The use of sulfites and sulfate compounds is preferred. Sodium bisulfite is particularly preferred.

[0468] Methods for carrying out process step 2a): Mixing the plant starting material of step 1 with an aqueous solution containing dissolved amino acids and / or peptides to separate the constituents of the starting material.

[0469] In this process step, the wetting of the surfaces of the constituents within the preferably biogenic starting material must be ensured. This means that even constituents present in a compacted aggregate must be wetted and thus hydrated. In the preferred economical embodiment of the process, the compounds are used to separate constituents from a dry starting material by dosing only the minimum amount of the digestion solution required to ensure complete saturation of the starting material. This can be verified, for example, by determining the moisture content, which is preferably > 20 wt% when complete saturation is achieved. Furthermore, saturation can be detected, for example, visually, e.g., by a change in color, or analytically, e.g., by a change in electrical conductivity.In another preferred embodiment, a volume of the digestion solution is added to the starting material, achieving complete swelling of the starting material. Complete swelling can be recognized, for example, by the fact that the swollen material can no longer bind any further amount of water, as evidenced by the fact that further addition of water does not lead to any further increase in the volume of the swollen homogeneous material and that only minimal free liquid phase separates during centrifugation (2,000 g). A test to determine whether further water binding is possible can be carried out by adding a 0.3 molar solution of the amino acid and / or peptide solution in small volume units to a sample of the swollen material whose mass is determined.If a free water phase forms, the swelling process is complete; otherwise, the addition of the amino acid and / or peptide solution to the mixture should be continued.

[0470] The volume of aqueous solutions containing dissolved amino acids and / or peptides is added to the starting material in a mass ratio of 0.5:1 to 10:1, more preferably between 1:1 and 8:1, and further preferably between 1.2:1 and 4:1. A process embodiment at a temperature between 6 and 90°C is preferred, more preferably between 10 and 60°C, and even more preferably between 18 and 40°C.

[0471] The application of aqueous solutions can be carried out using state-of-the-art methods. Suitable containers for this process step are reaction containers, which may be open, closable, or heated, and preferably equipped with a stirring or mixing device, such as a stirred tank, to ensure complete circulation of the mixture. The aqueous digestion solution is added continuously or discontinuously until complete saturation is observed in a representative sample. In another embodiment of the process, the starting material is distributed on a conveyor belt or a conveyor screen belt, and the distributed starting material is sprayed with the aqueous solution, thereby becoming saturated.

[0472] The duration of the penetration phase naturally depends on the type and properties of the starting material. A duration between 5 minutes and 24 hours is preferred, more preferably between 10 minutes and 12 hours, and further preferably between 20 minutes and 6 hours. A simple test procedure can be used to determine whether a mixture from this process step is suitable for feeding into the next process step. For this purpose, a representative sample is taken from the mixture and added to water (25°C) in a mass ratio of 1:20 and agitated for 2 minutes at 200 rpm. Subsequently, the entire suspension is filtered (sieve size Iommi). The sieve residue is examined visually or microscopically for the presence of aggregates of constituents from the biogenic starting material. If no aggregates are present, sufficient separation of the constituents of the starting material has occurred and the process step is complete.

[0473] In one process variant, the starting material is impregnated with one of the digestion solutions during or immediately after the application of one of the disintegration processes. This process variant is particularly advantageous for starting materials with a high water content, such as raw vegetables, tubers, or roots. In another process variant, the impregnation occurs directly together with compounds that enable / accelerate the disintegration of the plant starting material. This can also be the case, for example, if the aqueous digestion solution is used for disintegration in a thermal process. In this case, the plant material is also impregnated with the compounds of the digestion solution during the disintegration process. In a preferred process variant, the disintegration and impregnation take place under negative or positive pressure conditions in a suitable container.Preferably, a pressure of 100 to 50 bar is applied, more preferably 100 to 10 bar, and further preferably 100 to 5 bar. In principle, impregnation can take place at any temperature. Simultaneous heating of the starting material is preferred to accelerate the impregnation process. Therefore, it is preferred to carry out the process step at a temperature between 5 and 150°C, more preferably between 8 and 140°C, further preferably between 10 and 120°C, and even more preferably between 15 and 90°C. It is preferred to carry out the process step with simultaneous temperature increase and application of either negative or positive pressure. The preferred duration of the process step depends on the penetrability and the degree of disintegration achieved.A duration between 10 seconds and 10 days is preferred, more preferred between 1 minute and 2 days, more preferred between 10 minutes and 24 hours, still more preferred between 15 minutes and 8 hours, and most preferred between 20 minutes and 4 hours.

[0474] The completeness of disintegration and penetration can be easily verified by suspending, for example, a 1 ml sample of the digested plant material in 1000 ml of water and agitating it with a magnetic stirrer for 10 minutes at a speed of 300 rpm. If, after stopping agitation, fibrous materials with a slow sedimentation tendency are visible to the naked eye, and if, at the same time, any shell fragments or other solid const...

Claims

Claims Methods for the process-economical separation and / or splitting of all constituents encompassing - water-soluble and dissolved compounds, including proteins and carbohydrates and / or flavorings and / or colorings and / or fats and / or toxins; - optional water-soluble and insoluble compounds, including starch; - solid solids comprising cellulose-based fibers and / or lignin-rich shells, present in compacted form; a protein-containing biogenic starting material, wherein the process comprises the following steps: 1) Providing the protein-containing biogenic starting material, 2a) Mixing the starting material of step 1) with an aqueous solution having a pH between 7.5 and 13.5, containing at least one dissolved amino acid with a molar mass of less than 400 g / mol and a solubility of at least 35 g / L in water at 20°C and / or a peptide consisting of 2 to 50 of these amino acids to completely saturate the constituents of the protein-containing biogenic starting material, until hydrated soluble compounds and solid solids are obtained. 2b) Addition of an aqueous distribution volume with a weight ratio to the dry mass of the protein-containing biogenic starting material of 5:1 to 500:1 and mixing to obtain a distribution mixture of the separated and / or separated constituents from step 2a), yielding dissolved soluble compounds and decompacted solids. 3) Separation of the solid decompacted solids and optionally the undissolved water-soluble compounds from the partition mixture of step 2b) to obtain an aqueous solution of the water-soluble and dissolved compounds, without solid solids and without the optional water-soluble and undissolved compounds, 4) Addition of an aggregating agent comprising an aqueous solution containing at least one organic acid and aggregation of the water-soluble and dissolved compounds, comprising proteins and / or carbohydrates of the aqueous solution of step 3), until a suspension of the aggregated compounds, comprising the proteins and / or carbohydrates, and an aqueous phase, comprising the non-aggregated, water-soluble and dissolved compounds, is obtained. 5) Separation of the suspension from step 4) and dehydration of the aggregated compounds by separation of water, yielding dehydrated aggregated compounds and a clarified aqueous phase, and optionally purification of the clarified aqueous phase. 6) Addition of the clarified aqueous phase from step 5) as an aqueous solution to step 2a) and / or as an aqueous distribution volume to step 2b), or Use of the clarified aqueous phase from step 5) to purify the separated solids from step 3), or 1. Use of the clarified aqueous phase from step 5) for purification of the separated solids from step 3) obtaining an aqueous wash phase and addition of the aqueous wash phase as an aqueous solution to step 2a) and / or as an aqueous distribution volume to step 2b).

2. Method according to claim 1, wherein the protein-containing biogenic starting material is non-lignified plant starting material.

3. A method according to claim 1 or 2, wherein the at least one amino acid and / or the one peptide is / are a cationic amino acid and / or a peptide containing at least one cationic amino acid.

4. The method according to claim 1 further comprising step 4a) after step 4) and before step 5). Separation of the aggregated proteins and subsequent addition of one or more further aggregating agent(s) to aggregate the dissolved carbohydrates according to step 3).

5. Method according to one of claims 1 - 4, wherein the mixing to obtain a distribution mixture of the separated and / or separated constituents from step 2a) is carried out by means of an intensive mixer.

6. Method according to any one of claims 1-5, wherein the pH of the aqueous solutions is not undercut during the method.

7. Method according to any one of claims 1-6, wherein in step 4) compounds comprising carbohydrates, phospholipids, glycolipids, glycoglycerolipids, antioxidants, vitamins are added to and / or already contained in the aqueous solution of step 3), which are bound to the dissolved proteins and aggregated together with the proteins.

8. Method according to any one of claims 1 - 7, wherein in step 3) the separation of the solid materials from the distribution mixture of step 2b) is carried out by means of filtration or sedimentation.

9. Method according to any one of claims 1-8, wherein the aqueous solution with a pH between 7.5 and 13.5 contains no further amino acids besides the at least one cationic amino acid and / or peptides consisting of 2 to 50 of these amino acids.

10. Method according to any one of claims 1-9, wherein in step 5) the separation of the suspension of step 4) is carried out using a filtration method.

11. A method according to any one of claims 1-9, wherein in step 2b) and / or 3) and / or 4) a separation of lipophilic constituents of the starting material is carried out by additionally adding one or more lipophilic compound(s) to the reaction mixture in step 2a) and / or 2b) and mixing with it and / or de-oiling of plant proteins at room temperature and / or elevated temperature.

12. Method according to any one of claims 1-10, wherein in step 3) after the separation of solid solids from the distribution mixture of step 2b) to obtain a fiber-free aqueous solution of the water-soluble and dissolved compounds of the starting material, in step 3a) protein-free complex carbohydrates and / or starch granules are separated from the separated solid solids.

13. A method according to any one of claims 1-11, wherein in step 3) after the separation of solid solids from the distribution mixture of step 2b) to obtain a fiber-free aqueous solution of the water-soluble and dissolved compounds of the starting material, in a step 3a") decomplexed cellulose-based fibers and / or decomplexed lignin-rich shell fragments, and / or complexed carbohydrates, which are free of dissolved soluble compounds, are obtained from the separated solid solids.

14. Method according to any one of claims 1-12, wherein in step 4) the pH value of the aqueous solution of step 3) is adjusted to a pH value in the range between 5.5 and 8.

15. A method according to any one of claims 1-13, wherein in step 4) dissolved carbohydrates and / or phospholipids and / or glycoglycerolipids are aggregated together with dissolved proteins, and in step 5a) protein aggregates containing carbohydrates and / or phospholipids and / or glycoglycerolipids are obtained.

16. A method according to any one of claims 1-15, wherein step 4 of the method is carried out without the use of organic solvents.

17. Odorless and tasteless and / or toxin- and hazardous substance-free aggregated proteins obtainable according to step 5) according to the method according to any one of claims 1 - 16 with a protein solubility index (PDI) > 80%. Cellulose-based fibers with a water-binding capacity of >200 vol% and / or lignin-rich hulls with a fat-binding capacity of >200 wt%, obtainable by the process according to claim 13.

19. Protein-free complex or complexed carbohydrates and / or starch granules, obtainable by the process according to claim 12.

20. Protein aggregates containing carbohydrates available according to claim 15.

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