New components for clarification of sugar cane juice in processes for the production of crystal sugar or raw sugar

Abstract

The present invention relates to new components for clarifying sugar cane juice in a process for the production of crystal sugar or raw sugar. In particular, the present invention generally relates to the use of quaternary ammonium salts and cationic (co)polymers for clarifying sugar cane juice during the production of crystal sugar or raw sugar. The present invention also relates to a new process for the production of crystal sugar or raw sugar from sugar cane juice. More specifically, the present invention describes a process for improving the phosphatation clarification of crystal sugar or raw sugar by adding quaternary ammonium salts and cationic (co)polymers before, during or just after the clarification step. A kit comprising quaternary ammonium salts and cationic (co)polymers is also provided.

Description

[0001] This application is a divisional application of the following application: Application date: August 4, 2017; Application number: 201780047486.6; Invention title: "A novel component for clarifying sugarcane juice in a method for producing crystalline sugar or raw sugar". Technical Field

[0002] This invention generally relates to the use of quaternary ammonium salts and cationic (co)polymers in clarifying sugarcane juice during the production of crystalline or raw sugars. The invention also relates to a novel method for producing crystalline or raw sugars from sugarcane juice. More specifically, the invention describes a method for improving the phosphate clarification of crystalline or raw sugars by adding quaternary ammonium salts and cationic (co)polymers before, during, or immediately after a clarification step. A kit comprising quaternary ammonium salts and cationic (co)polymers is also provided. Background Technology

[0003] According to the Food and Agriculture Organization of the United Nations (FAO, 2015), global sugar production in 2014 / 2015 was estimated at 181 million tons, a modest increase of 0.2% compared to the 2013 / 2014 season, but still the second largest harvest in history, with Brazil remaining the largest producer, with an estimated output of 37.5 million tons.

[0004] Sugarcane is the primary sugar-producing crop, with global sugar production from sugarcane approximately six times greater than that from sugar beets (another major sugar source). Sugarcane is one of the few tall, perennial true grass species identified as a field crop in all tropical and subtropical countries of the world, and sugar production methods are steadily improving.

[0005] Currently, there is considerable interest in the sugarcane milling industry in finding effective technologies to remove impurities from sugarcane juice during manufacturing. These efforts reflect the growing demand for food products containing minimal amounts of chemicals, and consequently, a focus has been placed on improving sugar quality and providing white crystalline substances.

[0006] Because color is one of the most important standards for sugar quality, this aspect has been evaluated and new methods have been studied to reduce sugar color without leaving any trace of chemicals in the final product.

[0007] Conventional methods for producing crystalline and raw sugars from sugarcane involve extracting sugarcane juice from harvested sugarcane. The juice is then purified (often referred to as clarification) to produce crystalline or raw sugars. Raw sugars can be remelted to give syrups or sugar solutions, which are used as raw materials for the production of refined sugars.

[0008] At the outset of sugar production methods, sugarcane juice clarification was the most crucial step in supplying the market with sugar of optimal quality. In the 1950s, a sugarcane juice clarification technique known as sulfitization was developed in India for sugar production. This typical clarification method involves adding sulfur dioxide (SO2) to the juice to separate non-sugar components, including colored substances. Sugar produced through this method can contain approximately 20 ppm or more of sulfur, and this contaminant causes health and environmental problems, making it unacceptable in the food and beverage market.

[0009] In the beet sugar industry, another method for clarifying beet juice is known, known as carbonation. This method involves adding calcium hydroxide to a slurry and bubbling carbon dioxide gas to precipitate calcium carbonate. When applied to sugarcane, this type of method suffers from several problems, particularly the excessive consumption of lime, which makes the method economically unsustainable. Indeed, the two sugar sources have different compositions, especially different non-sugar properties, and beets do not contain any reducing sugars. In some cases, this method can be applied to the clarification of refined sugar, but not to the production of raw / crystalline sugar from sugarcane. WO 2014 / 011496 and FR 2578238 disclose such carbonation methods using polymeric color precipitants.

[0010] In the refined sugar industry, a common clarification method is phosphate clarification. This method is based on the principle of precipitating calcium phosphate by adding phosphoric acid and lime.

[0011] Numerous chemical additives have been proposed to precipitate impurities during sugar purification via phosphate treatment. However, these innovative initiatives have primarily been developed in the refining steps of the sugar industry. For example, U.S. Patent No. 3,698,951, WO 2011 / 060168, and U.S. Patent No. 5,865,899 describe sugar refining methods in which syrups and sugar solutions are decolorized by adding a dialkyldimethyl quaternary ammonium surfactant.

[0012] According to the Food and Drug Administration, HHS § 173.400 Pt. 174 21 CFR Ch. I (4-1-00 edition), dimethyl-bis(octadecyl)ammonium chloride (DHT) is known to be " Used as a decolorizing agent in the clarification of sugar solutions in refineries under the following limitations: 1) The food additives described in paragraphs (a)(1) of this section are added only during the purification / clarification stage of sugar refining, and in no particular quantity. More than 700 parts per million by weight of sugar solids. " However, even at these very high levels, the performance is not satisfactory enough for industrial implementation when applied to methods for producing crystalline sugars.

[0013] Therefore, a primary approach has been taken to optimize refining methods through clarification processes to reduce sugar color from syrups and solutions that have already been clarified in previous steps of producing raw or crystalline sugar and thus exhibit fewer impurities and a lower initial color intensity. Indeed, there is a difference between syrups and solutions and cane juice. Syrups and solutions are molten raw sugars that are more concentrated and have fewer impurities that are removed in the preliminary steps of sugar refining processes. On the other hand, cane juice is the juice extracted directly from crushed whole or peeled sugarcane in a grinder.

[0014] According to the Food and Drug Administration, HHS, 21 CFR Ch. I (4-1-12 edition), paragraph 173.60, dimethylamine-epimylohydrin copolymer (DMA-Epi) is known as "a food additive used as a decolorizing agent and / or flocculant in the clarification of sugar solutions and juices in refineries. It is added only during the purification / clarification stage of sugar solution refining, and in a concentration not exceeding 150 parts per million by weight of the copolymer of sugar solids." However, for amounts exceeding regulatory limits, good performance has been achieved in the clarification of sugarcane juice in methods for producing crystalline sugar or raw sugar.

[0015] In view of the above, to date, there is no solution for improving the clarification method of sugarcane juice to obtain crystalline sugar or raw sugar.

[0016] Therefore, the object of the present invention is an optimized solution for clarifying sugarcane juice using the phosphate principle when producing crystalline sugar or raw sugar.

[0017] Another object of the present invention is to provide an improved method for producing crystalline sugar or raw sugar with low coloring and thus acceptable to the food, pharmaceutical and beverage industries.

[0018] Another objective of this invention is to propose a more efficient method that consumes less chemicals, causes less corrosion, and is easier to control. Summary of the Invention

[0019] Therefore, this invention proposes the use of quaternary ammonium salts and cationic (co)polymers in clarifying sugarcane juice during the production of crystalline or raw sugar. Preferably, the object of this invention is the use of quaternary ammonium salts and cationic (co)polymers in clarifying sugarcane juice by phosphate treatment during the production of crystalline or raw sugar.

[0020] The present invention also provides a method for producing crystalline sugar or raw sugar, the method comprising the following steps: a) Extracting sugarcane juice from sugarcane; b) Clarifying sugarcane juice, preferably by phosphate treatment; c) Evaporation and clarification of sugarcane juice; d) To crystallize the clarified sugarcane juice; e) Centrifugation and drying.

[0021] The quaternary ammonium salt and cationic (co)polymer are added before, during, or immediately after the clarification step.

[0022] Another object of the present invention is a kit comprising: - Quaternary ammonium salts, - Cationic (co)polymers, and - Optional phosphorus source. Detailed Implementation

[0023] definition In the context of this invention, the term "sugarcane juice" or "mixed juice" refers to any juice containing sugar and extracted by grinding and crushing whole or peeled sugarcane in a grinder. The typical color intensity of sugarcane juice is between 5000 and 50000 IU (ICUMSA units), more frequently between 10000 and 25000 IU, and even more frequently between 12000 and 20000 IU. The method for measuring the color intensity of juice in IU is described in the experimental section below.

[0024] "Decanted juice" refers to juice obtained from sugarcane juice after a clarification step using the quaternary ammonium salt and cationic (co)polymer according to the invention. Decanted juice with a color intensity of less than 10,000 IU is preferred.

[0025] The percentage of discoloration obtained from the mixture of clarified sugarcane juice during the production of crystalline or raw sugar using the quaternary ammonium salt and cationic (co)polymer according to the invention is typically as follows: - Mixed juices with initial color below 30,000 IU, color reduction %: 10-60 - Mixed juice with an initial color of over 30,000 IU, color reduction %: 20-70.

[0026] According to the present invention, the term "crystalline sugar," also known as plant-grown white sugar, is sugar produced essentially directly from sugarcane juice obtained from sugarcane by means of extraction, clarification, evaporation, and crystallization. Examples of crystalline sugar may include those having sucrose crystals having an average size of 0.4 to 0.8 mm, preferably 0.5 to 0.7 mm, a color intensity between 50 and 400 ICUMSA units, preferably 90 to 150 ICUMSA units, and notably for domestic and industrial purposes.

[0027] According to the present invention, the term "raw sugar," also known as VHP (very high polarization) sugar, is minimally processed cane sugar. Examples of raw sugar may include those having a color intensity between 400 and 1200 ICUMSA units, preferably 700 to 900 ICUMSA units, and which are commonly used as raw materials for refining processes to obtain refined sugar.

[0028] According to method ICUMSA GS 9 / 1 / 2 / 3-8 (2011) - Determination of the color of sugar solutions at pH = 7 by MOPS buffer method, the color of crystalline sugars or raw sugars in ICUMSA units is obtained.

[0029] The term "phosphated" refers to the removal of at least some of the impurities that cause the color of sugarcane juice by using a phosphorus source to precipitate phosphate.

[0030] For example, the term “a / a(a)” used in the text below is as follows: “quaternary ammonium salt” or “cationic (co)polymer” is the plural of the class. This means that it must be interpreted as “a / a kind or a plurality of / kinds” or “at least one / kind”.

[0031] Applications of quaternary ammonium salts and cationic (co)polymers - Quaternary ammonium salts The quaternary ammonium salt is advantageously a compound having formula (I): in: R1 and R2 are chosen independently from the group consisting of: C8 to C 36 Straight-chain or branched, saturated or unsaturated aliphatic groups, optionally containing heteroatoms or ester or amide groups; R3 and R4 are chosen independently from the group consisting of: C1 to C 18 Straight-chain or branched, saturated or unsaturated aliphatic groups, optionally containing heteroatoms or ester or amide groups; X is, for example, an anion selected from halide ions, nitrate ions, phosphate ions, or acetate ions; preferably, X is a halide ion; more preferably, X is a chloride ion.

[0032] In one embodiment, R1 and R2 are selected independently from a group consisting of: C 12 To C 20 Straight-chain or branched, saturated or unsaturated aliphatic groups, optionally containing heteroatoms or ester or amide groups, preferably C 16 To C 18 Straight-chain alkyl groups.

[0033] In another embodiment that can be combined with the previous one, R3 and R4 are selected independently from the group consisting of: C1 to C 12 Straight-chain or branched, saturated or unsaturated aliphatic groups, optionally containing heteroatoms or ester or amide groups, preferably C1 to C4 straight-chain alkyl groups.

[0034] In a preferred embodiment, the quaternary ammonium salt is dimethyl-bis(octadecyl)ammonium chloride.

[0035] The quaternary ammonium salts according to the invention can be derived from plants or animals, or can be synthesized under well-known classical conditions via a reaction between a trialkylamine and a haloalkane. In a preferred embodiment, the dimethyl dioctadecylammonium chloride is the result of a reaction between methyl dioctadecylamine and methyl chloride.

[0036] The quaternary ammonium salt may be present in amounts ranging from 10 ppm to 700 ppm by weight, preferably from 10 ppm to 160 ppm, more preferably from 20 ppm to 100 ppm, even more preferably from 20 ppm to 60 ppm, notably 40 ppm to 60 ppm or 20 ppm to 40 ppm, based on the amount of solids in the sugarcane juice. This amount is the "active content" by weight based on the amount of solids in the sugarcane juice.

[0037] The quaternary ammonium salt can be added in the form of an aqueous solution, an alcoholic solution, or a water-alcoholic solution. A preferred embodiment is to use a solution containing ethanol and / or isopropanol (as a solvent for the quaternary ammonium salt) and water.

[0038] - Cationic (co)polymer The cationic (co)polymer can be a cationic homopolymer or a copolymer.

[0039] Advantageously, it can be selected from the group consisting of: polyquaternary ammonium salts, preferably homopolymers of dimethylaminoethyl acrylate methyl chloride quaternary ammonium salt and / or homopolymers of diallyl dimethyl ammonium chloride (PolyDADMAC), cationic copolymers of dialkylamines and epichlorohydrins, and mixtures thereof.

[0040] According to a first embodiment, the cationic (co)polymer is a cationic copolymer of dialkylamine and epichlorohydrin, wherein the alkyl portion is a straight-chain or branched alkyl group containing 1 to 6 carbon atoms, preferably 1 to 4 carbon atoms. A preferred cationic copolymer is a cationic copolymer of dimethylamine and epichlorohydrin (DMA-Epi). The preferred copolymer of dimethylamine and epichlorohydrin, CAS Registry No. 25988-97-0, may have no more than 5 mol% of dimethylamine that can be replaced by an equimolar amount of ethylenediamine, and its total amine to epichlorohydrin molar ratio is preferably about 1:1. Advantageously, the nitrogen content of the copolymer of dimethylamine and epichlorohydrin is 9.4 to 10.8% by weight on a dry weight basis. Suitable molar masses of DMA-Epi can vary from 6,500 to 30,000 g / mol, preferably from 7,000 to 25,000. The cationic copolymer of dimethylamine and epichlorohydrin can be prepared by a stepwise reaction synthesis of 2-hydroxy-3-dimethylaminopropyl (a monomer formed by the reaction of epichlorohydrin and dimethylamine), as disclosed in Water Science and Technology: Water Supply, Vol. 1, No. 1, pp. 43-50, IWA Publishing, 2001. It is also available under the commercial name Glokill PQ60 from Solvay SA and Barquat PQ from Lonza Group AG.

[0041] According to another embodiment, the cationic (co)polymer is polydiallyl dimethylammonium chloride (PolyDADMAC). The molecular weight of the polydiallyl dimethylammonium chloride (PolyDADMAC) can vary from 100,000 to 200,000 g / mol, preferably from 140,000 to 180,000 g / mol, and more preferably from about 160,000 g / mol.

[0042] PolyDADMAC can be prepared by the free radical polymerization of diallyl dimethyl ammonium chloride (DADMAC), more precisely, by the free radical addition polymerization of diallyl dimethyl ammonium chloride (DADMAC) using persulfate or organic peroxide as initiators. It is also available under the commercial names Mirapol 100 from Solvay, Percol 1697 from Allied Colloids Ltd, and Merquat 100 from Lubrizol Corporation.

[0043] The cationic (co)polymer is advantageously present in an amount of 10 ppm to 150 ppm, preferably 10 ppm to 70 ppm, and more preferably 15 ppm to 40 ppm by weight, based on the amount of solids in the sugarcane juice. The amount is the "active content" by weight based on the amount of solids in the sugarcane juice.

[0044] The cationic (co)polymer can be added in the form of an aqueous solution.

[0045] - Additional components During the production of crystalline or raw sugar, preferably before, during, or immediately after the clarification step, a phosphorus source is also added. In this case, it is preferably selected from the group consisting of any salt containing a phosphate anion and a cation, wherein the phosphate anion is preferably selected from hydrogen phosphite (HPO3). 2- ), dihydrogen phosphate (H2PO4) 4- ), orthophosphate (PO4) 3- HPO4 2- H2PO4 - ), diphosphate (H2P2O6) 2- ), metaphosphate (PO3) - ) or pyrophosphate (P2O7) 4- The cation is preferably selected from ammonium (such as R4N). + 、R3NH + R2NH2 + RNH3 + NH4 + R is typically a straight-chain or branched C1 to C6 alkyl group, sodium (Na) + ) or calcium (Ca 2+ ).

[0046] In a preferred embodiment, the phosphorus source is phosphoric acid. Advantageously, the phosphoric acid is used as an aqueous solution typically at a concentration between 50% and 95% by weight, preferably 70% to 85%.

[0047] The phosphorus source may be added together with the quaternary ammonium salt and / or together with the cationic copolymer and / or separately from the quaternary ammonium salt and the cationic copolymer. We prefer to add the phosphorus source together with the quaternary ammonium salt and together with the cationic copolymer, and optionally also separately from the quaternary ammonium salt and the cationic copolymer.

[0048] The total amount of the phosphorus source is advantageously from 50% to 400% by weight of the total weight of the quaternary ammonium salt and the cationic copolymer, preferably from 50% to 200%, more preferably from 100% to 200%.

[0049] When a phosphorus source (especially phosphoric acid) is added together with the cationic polymer (notably DMA-Epi), the relative amounts of DMA-Epi and phosphorus source are about 20% to 30% by weight of DMA-Epi and 35% to 60%, preferably 35% to 50% by weight of phosphorus source, with the remainder being water.

[0050] When a phosphorus source (especially phosphoric acid) is added together with the quaternary ammonium salt (notably DHT), the relative amounts of DHT and phosphorus source are about 30% to 60% by weight of DHT and 5% to 30%, preferably 10% to 30% and more preferably 15% to 25% by weight of phosphorus source, with the remainder being water and / or alcohols such as ethanol or isopropanol.

[0051] When the phosphorus source (especially phosphoric acid) is added separately from the quaternary ammonium salt and the cationic copolymer, it is in the form of an aqueous solution of phosphoric acid at a weight of between 50% and 95%, preferably 70% to 85%.

[0052] Particularly preferred embodiments include the use of two or three solutions: - An aqueous-alcoholic solution of a quaternary ammonium salt and a phosphorus source, preferably an aqueous-alcoholic solution of DHT and phosphoric acid. - An aqueous solution of a cationic (co)polymer and a phosphorus source, preferably an aqueous solution of DMA-Epi and phosphoric acid. - Optionally, the phosphorus source is preferably an aqueous solution of phosphoric acid to clarify the sugarcane juice during the production of crystalline sugar or raw sugar.

[0053] According to this particularly preferred embodiment, the amount of each of the two or three solutions is as follows: - An aqueous-alcoholic solution of a quaternary ammonium salt and a phosphorus source, ranging from 20 ppm to 300 ppm, preferably from 20 ppm to 100 ppm, and more preferably from 50 ppm to 95 ppm (based on the total weight of the mixed juice), preferably an aqueous-alcoholic solution of DHT and phosphoric acid. - An aqueous solution of a cationic (co)polymer and a phosphorus source, preferably an aqueous solution of DMA-Epi and phosphoric acid, at a concentration of 50 ppm to 150 ppm, preferably 50 ppm to 100 ppm (based on the total weight of the mixed juice by weight). - Optionally, the phosphorus source is an aqueous solution of phosphoric acid, ranging from 20 ppm to 200 ppm, preferably from 20 ppm to 100 ppm, and more preferably from 50 ppm to 95 ppm (based on the total weight of the mixed juice).

[0054] According to this particularly preferred embodiment, the concentrations of each of the two or three solutions are as follows: - An aqueous-alcoholic solution comprising 30% to 60% of a quaternary ammonium salt and 5% to 30% (preferably 10% to 30%) of a phosphorus source, preferably 40% to 60% of DHT and 5% to 30% (preferably 10% to 30%) of an aqueous-alcoholic solution of phosphoric acid at a concentration between 50% and 95% by weight. - An aqueous solution comprising 40% to 60% by weight of a cationic (co)polymer aqueous solution at a concentration between 50% and 70% and 35% to 60% preferably 40% to 60% of a phosphorus source, preferably 40% to 60% of DMA-Epi at a concentration between 50% and 70% and 40% to 60% by weight of a phosphoric acid aqueous solution at a concentration between 50% and 95%. - Optionally, an aqueous solution of a phosphoric acid source, preferably an aqueous solution of phosphoric acid with a concentration between 50% and 95% by weight, preferably 70% to 85% by weight.

[0055] The most preferred embodiment of the present invention is when two or three solutions are used in the following concentrations and amounts: - An aqueous-alcoholic solution containing 30% to 60% quaternary ammonium salt and 5% to 30% (preferably 10% to 30%) of phosphorus source, from 20 ppm to 300 ppm, preferably 20 ppm to 100 ppm, more preferably 50 ppm to 95 ppm (based on the total weight of the mixed juice), preferably 30% to 60% (preferably 40% to 60%) of DHT and 5% to 30% (preferably 10% to 30%) of an aqueous solution of phosphoric acid at a concentration between 50% and 95% by weight. - An aqueous solution comprising, by weight, 40% to 60% of a cationic (co)polymer aqueous solution at a concentration between 50% and 70% and 35% to 60% (preferably 40% to 60%) of a phosphorus source, preferably 40% to 60% of DMA-Epi at a concentration between 50% and 70% and 40% to 60% of a phosphoric acid aqueous solution at a concentration between 50% and 95%, from 50 ppm to 150 ppm, preferably 50 ppm to 100 ppm (based on the total weight of the mixed juice), and preferably 40% to 60% of DMA-Epi at a concentration between 50% and 70% and 40% to 60% of phosphoric acid at a concentration between 50% and 95%. - Optionally, an aqueous solution of a phosphorus source of 20 ppm to 200 ppm, preferably 20 ppm to 100 ppm, preferably 50 ppm to 95 ppm (based on the total weight of the mixed juice), preferably an aqueous solution of phosphoric acid at a concentration between 50% and 95% by weight, preferably 70% to 85% by weight.

[0056] Preferably, the above three solutions are used.

[0057] Methods for producing crystalline sugar or raw sugar This invention provides a method for producing crystalline sugar or raw sugar from sugarcane juice, the method comprising the following steps: a) Extracting sugarcane juice from sugarcane; b) Clarifying sugarcane juice, preferably by phosphate treatment; c) Evaporation and clarification of sugarcane juice; d) To crystallize the clarified sugarcane juice; e) Centrifugation and drying.

[0058] The quaternary ammonium salt and cationic (co)polymer are added before, during, or immediately after the clarification step.

[0059] Initially, the selection of the most suitable sugarcane variety is preferred. The overall quality of crystalline or raw sugar depends on several aspects of the selected sugarcane, such as agronomic practices, ripening stage, and climate change. Preferably, an extremely sweet, soft, and flavorful sugarcane variety is selected, which is essentially acid-free, has sucrose content ranging from 13% to 22%, and glucose content ranging from 0.1% to 1.0%. In particular, it is preferred that the selected sugarcane yields a sucrose level of at least 20% for processing.

[0060] Sugarcane is harvested by manual or mechanized cutting, both of which have positive aspects. Mechanical harvesting equipment can cut whole sugarcane stalks or shred the sugarcane. On the other hand, manual cutting avoids introducing foreign matter that is usually carried into the processing mill along with the sugarcane. Foreign matter, which typically accounts for ten percent or more of the sugarcane's weight, mainly consists of soil, mud, ash, leaves, minerals, and the top of the sugarcane. The introduction of foreign matter has the undesirable effect of altering the natural flavor of the subsequently extracted sugarcane juice.

[0061] Extracting sugarcane juice from sugarcane In step (a), the cut sugarcane stalks may be subjected to a standard washing step to remove the aforementioned foreign matter and reduce impurities on the stalk surface. Subsequently, the sugarcane stalks are typically reduced to smaller individual pieces using a rotary cutter or hammer mill, and leaves and nodes are advantageously removed.

[0062] Sugarcane juice extraction includes any conventional extraction methods suitable for destroying sugarcane cells, methods well known to those skilled in the art, such as crushing by tandem milling and extraction by diffusion. A tandem mill is a special type of modern rolling mill in which rolling is completed in a single pass and several stands (roll sets) are present. In conventional extraction, sugarcane stalks are fed through a standard rolling mill to extract sugarcane juice at temperatures ranging from 30ºC to 90ºC, more preferably from 60ºC to 85ºC, as is well known to those skilled in the art.

[0063] In a preferred embodiment, the sugarcane juice obtained by the above extraction step (a) has a pH level between 4 and 6, 10% to 30% sucrose by weight, 60% to 80% water by weight, 5% to 20% insoluble material by weight, and 10% to 30% soluble solids by weight.

[0064] In a more preferred embodiment, the sugarcane juice obtained by the above extraction step (a) has a pH level between 4.5 and 5.5, 13% to 22% sucrose by weight, 68% to 76% water by weight, 8% to 16% insoluble material by weight, and 18% to 25% soluble solids by weight.

[0065] Clarified sugarcane juice According to the present invention, the method for producing crystalline sugar or raw sugar from sugarcane juice includes clarifying the sugarcane juice, wherein a quaternary ammonium salt and a cationic (co)polymer are added before, during or immediately after the clarification step (b).

[0066] According to various embodiments, the quaternary ammonium salt is advantageously as described above.

[0067] Prior to the addition of the quaternary ammonium salt in clarification step (b), the quaternary ammonium salt is advantageously dissolved or dispersed in water or an organic solvent (preferably ethanol or isopropanol). The quaternary ammonium salt can be added in the amounts described above.

[0068] According to various embodiments, the cationic (co)polymer is as described above.

[0069] The cationic (co)polymer can be added in the amounts described above.

[0070] The clarification step is advantageously a phosphate step.

[0071] In this particularly preferred embodiment, a phosphorus source is therefore added before, during, or immediately after the clarification step.

[0072] According to various embodiments, the phosphorus source is as described above.

[0073] The phosphorus source can be added in the amounts described above.

[0074] In a particular embodiment of the invention, the quaternary ammonium salt, the cationic (co)polymer, and optionally the phosphorus source are added as a homogeneous blend, either before, during, or immediately after the clarification step (b), or added separately but simultaneously, or separately and at different stages. For solubility reasons, we prefer to add the quaternary ammonium salt and the cationic (co)polymer separately but simultaneously. When adding, it is preferred that, before, during, or immediately after the clarification step (b), a portion of the phosphorus source is added separately but simultaneously with the quaternary ammonium salt, another portion is added with the cationic (co)polymer, and optionally the remaining portion is added.

[0075] As a highly preferred embodiment, before, during, or immediately after clarification step (b), a total amount of phosphorus source ranging from 3% to 25% is added together with the quaternary ammonium salt, a total amount of phosphorus source ranging from 10% to 70% is added together with the cationic (co)polymer, and a total amount of phosphorus source ranging from 0% to 80% is added.

[0076] In one embodiment of the invention, the clarification step (b) includes preheating (b1), pH correction (b2), and heating (b3) steps.

[0077] In step (b1), the sugarcane juice is preferably preheated at a temperature of 40ºC to 75ºC, more preferably from 60ºC to 70ºC.

[0078] While preheating, the juice is advantageously subjected to a pH correction step (b2) to promote subsequent chemical reactions and improve the precipitation of colloids and finely dispersed substances from the clarified sugarcane juice. The standard procedure in sugar mills is to add any source of lime, but calcium oxide, also known as milk of lime, is preferred. The addition of lime raises the pH and serves to form a calcium phosphate precipitate, which carries away impurities present in the juice during settling.

[0079] In step (b2), calcium oxide or lime milk is advantageously added to the sugarcane juice in an amount sufficient to bring the pH level of the juice to 6.0 to 8.0, preferably 6.8 to 7.4, more preferably 6.8 to 7.2. The amount of calcium oxide used in this invention is reduced compared to existing methods. Minimizing the amount of additives (such as calcium oxide) during this clarification process is essential to maintaining the natural flavor of the sugarcane juice and thus the final product.

[0080] Then, according to step (b3), in the second heating stage, the sugarcane juice is preferably heated at a temperature of 90ºC to 120ºC, more preferably from 98ºC to 110ºC.

[0081] Steps (b1) and (b3) are performed using standard heating equipment, as this is well known in the sugar industry.

[0082] In one embodiment of the invention, the quaternary ammonium salt, the cationic (co)polymer, and optionally the phosphorus source are added during these steps b1, b2, and / or b3.

[0083] In a preferred embodiment, the quaternary ammonium salt, the cationic (co)polymer, and optionally the phosphorus source are added between steps b2 and b3, and even more preferably during step b3.

[0084] evaporation Once the sugarcane juice has been substantially clarified, it is subjected to an evaporation step (c) to concentrate it. The clarified juice is typically transferred to a standard evaporator and preferably heated at a temperature of 60ºC to 95ºC, more preferably from 80ºC to 85ºC. Preferably, the juice is then extracted from the evaporator with a soluble solids content of 50 to 70º Brix, preferably 55 to 65º Brix.

[0085] crystallization Following the evaporation step (c), the clarified sugarcane juice is directed to the subsequent crystallization step (d), which is typically carried out in a vacuum pot to form solid crystals. In this crystallization step, the juice is then boiled, preferably at a temperature from 50ºC to 90ºC, more preferably from 60ºC to 75ºC, under vacuum. This causes the development and growth of solid crystals, and the result is referred to as "sugar paste" (a mixture of crystals and mother liquor, also known as molasses, produced by crystallization).

[0086] Centrifugation and drying Then, according to step (e), the crystalline sugar or raw sugar and molasses obtained from the crystallization are separated after centrifugation, and preferably dried at a temperature from 65ºC to 95ºC, more preferably from 70ºC to 80ºC.

[0087] In a preferred embodiment of the present invention, the method for producing crystalline sugar or raw sugar includes the following steps: a) Extracting sugarcane juice from sugarcane; b) Clarifying sugarcane juice, preferably by phosphate treatment; b1) Preheating b2) pH correction b3) Heating c) Evaporation and clarification of sugarcane juice; d) To crystallize the clarified sugarcane juice; e) Centrifugation and drying.

[0088] The quaternary ammonium salt, cationic copolymer, and optionally phosphorus source are added before, during, or immediately after the clarification step.

[0089] All steps a) to e) and their preferred embodiments have been described in detail above.

[0090] In a preferred embodiment, the method according to the invention is sulfur-free, which means that no sulfur compounds or derivatives are added during the method.

[0091] Furthermore, it is particularly preferred that the method according to the invention does not include a carbon dioxide addition step. Of course, very small amounts of CO2 can dissolve in water, but we mean that no voluntary addition of CO2 is performed during the method according to the invention.

[0092] The resulting crystalline sugar obtained according to the present invention has a color intensity between 50 and 400 ICUMSA units, preferably between 90 and 150 ICUMSA units.

[0093] The raw sugar obtained according to the present invention has a color intensity between 400 and 1200 ICUMSA units, preferably 700 to 900 ICUMSA units.

[0094] This invention offers advantages over existing methods for obtaining crystalline or raw sugars. The invention proposes an improved method for clarifying sugarcane juice by adding a quaternary ammonium salt and a cationic (co)polymer at the beginning of the method. This method exhibits increased decolorization properties, reduced sugar color, and leaves no trace chemicals in the final product. Crystalline and raw sugars produced using the method according to the invention have low coloration and are acceptable for use in the food, pharmaceutical, and beverage industries.

[0095] Reagent test kit The present invention also provides a kit comprising: - Quaternary ammonium salts, - Cationic (co)polymers, and - Optional phosphorus source.

[0096] In the kit according to the invention, the quaternary ammonium salt advantageously corresponds to Formula I and the above preferred embodiments, and it is preferably dimethyl-bis(octadecyl)ammonium chloride.

[0097] In the kit according to the invention, the cationic (co)polymer advantageously corresponds to the preferred embodiment described above; it is preferably a cationic copolymer of dimethylamine and epichlorohydrin (DMA-Epi).

[0098] For the optional phosphorus source of this kit, one of the phosphorus sources described in the above specification may be used. It is preferably phosphoric acid.

[0099] This kit advantageously contains two or three solutions of no more than: - An aqueous-alcoholic solution comprising 30% to 60% of a quaternary ammonium salt and 5% to 30% (preferably 10% to 30%) of a phosphorus source, preferably 40% to 60% of DHT and 5% to 30% (preferably 10% to 30%) of an aqueous solution of phosphoric acid with a concentration between 50% and 95% by weight. - An aqueous solution comprising 40% to 60% by weight of a cationic (co)polymer aqueous solution at a concentration between 50% and 70% and 35% to 60% preferably 40% to 60% of a phosphorus source, preferably 40% to 60% of DMA-Epi at a concentration between 50% and 70% and 40% to 60% by weight of a phosphoric acid aqueous solution at a concentration between 50% and 95%. - Optionally, an aqueous solution of a phosphoric acid source, preferably an aqueous solution of phosphoric acid with a concentration between 50% and 95% by weight, preferably 70% to 85% by weight.

[0100] The kit preferably contains the above three solutions.

[0101] The kit is available in the method according to the invention.

[0102] In summary, the present invention relates to the following embodiments: Implementation Scheme 1. Use of a composition comprising a quaternary ammonium salt and a cationic copolymer for clarifying sugarcane juice during the production of crystalline sugar or raw sugar. The quaternary ammonium salt is a compound having formula (I): in: R1 and R2 are independently selected from C12 to C20 straight-chain alkyl groups; R3 and R4 are independently selected from C1 to C4 straight-chain alkyl groups; and The cationic copolymer is a cationic copolymer of dialkylamine and epichlorohydrin, wherein the alkyl portion is a straight-chain alkyl group containing 1 to 6 carbon atoms; X is an anion selected from halide, nitrate, phosphate, or acetate ions.

[0103] Implementation Scheme 2. The use as described in Implementation Scheme 1, wherein X is a halide ion.

[0104] Implementation Scheme 3. The use as described in Implementation Scheme 1, wherein X is a chloride ion.

[0105] Implementation Scheme 4. The use according to Implementation Scheme 1, wherein the quaternary ammonium salt is dimethyl dioctadecyl ammonium chloride.

[0106] Implementation Scheme 5. The use according to Implementation Schemes 1 to 4, wherein the quaternary ammonium salt is present in an amount from 10 ppm to 700 ppm by weight based on the amount of solids in the sugarcane juice.

[0107] Implementation Scheme 6. The use according to Implementation Scheme 5, wherein the quaternary ammonium salt is present in an amount from 10 ppm to 160 ppm by weight based on the amount of solids in the sugarcane juice.

[0108] Implementation Scheme 7. The use according to Implementation Scheme 5, wherein the quaternary ammonium salt is present in an amount from 20 ppm to 100 ppm by weight based on the amount of solids in the sugarcane juice.

[0109] Implementation Scheme 8. The use according to Implementation Scheme 1, wherein the alkyl portion is a straight-chain or branched alkyl group containing 1 to 4 carbon atoms.

[0110] Implementation Scheme 9. The use according to Implementation Scheme 1, wherein the cationic copolymer is a cationic copolymer of dimethylamine and epichlorohydrin.

[0111] Implementation Scheme 10. The use according to Implementation Schemes 1 to 4, wherein the cationic copolymer is present in an amount from 10 ppm to 150 ppm by weight based on the amount of solids in the sugarcane juice.

[0112] Implementation Scheme 11. The use according to Implementation Scheme 10, wherein the cationic copolymer is present in an amount from 10 ppm to 70 ppm by weight based on the amount of solids in the sugarcane juice.

[0113] Implementation Scheme 12. The use according to Implementation Scheme 10, wherein the cationic copolymer is present in an amount from 15 ppm to 40 ppm by weight based on the amount of solids in the sugarcane juice.

[0114] Implementation Scheme 13. The use according to any one of Implementation Schemes 1 to 4, wherein a phosphorus source is also added during the production of crystalline sugar or raw sugar.

[0115] Implementation Scheme 14. The use according to Implementation Scheme 13, wherein the phosphorus source is selected from the group consisting of any salt containing phosphate anions and cations.

[0116] Implementation Scheme 15. The use according to Implementation Scheme 13, wherein the phosphorus source is selected from phosphoric acid.

[0117] Implementation Scheme 16. According to the use described in Implementation Scheme 14, wherein the phosphate anion is selected from hydrogen phosphite (HPO32-), dihydrogen phosphate (H2PO4-), orthophosphate (PO43-), orthophosphate (HPO42-), orthophosphate (H2PO4-), diphosphate (H2P2O62-), metaphosphate (PO3-), or pyrophosphate (P2O74-).

[0118] Implementation Scheme 17. The use according to Implementation Scheme 14, wherein the cation is selected from ammonium, sodium or calcium.

[0119] Implementation Scheme 18. The use according to Implementation Scheme 13, wherein the phosphorus source is present in a total amount from 50% to 400% by weight of the total weight of the quaternary ammonium salt and the cationic copolymer.

[0120] Implementation Scheme 19. The use according to Implementation Scheme 18, wherein the phosphorus source is present in a total amount from 50% to 200% by weight of the total weight of the quaternary ammonium salt and the cationic copolymer.

[0121] Implementation Scheme 20. A method for producing crystalline sugar or raw sugar, the method comprising the following steps: a. Extracting sugarcane juice from sugarcane; b. Clarified sugarcane juice; c. Evaporated and clarified sugarcane juice; d. To crystallize the clarified sugarcane juice; e. Centrifuge and dry; The quaternary ammonium salt and cationic copolymer are added before, during, or immediately after the clarification step. The quaternary ammonium salt has formula (I): in: R1 and R2 are independently selected from C12 to C20 straight-chain alkyl groups; R3 and R4 are independently selected from C1 to C6 straight-chain alkyl groups; and The cationic copolymer is a cationic copolymer of dialkylamine and epichlorohydrin, wherein the alkyl portion is a straight-chain alkyl group containing 1 to 6 carbon atoms; X is an anion selected from halide, nitrate, phosphate, or acetate ions.

[0122] Implementation Scheme 21. The method according to Implementation Scheme 20, wherein X is a halide ion.

[0123] Implementation Scheme 22. The method according to Implementation Scheme 20, wherein X is a chloride ion.

[0124] Implementation Scheme 23. The method according to any one of Implementation Schemes 20 to 22, wherein the quaternary ammonium salt is dimethyl dioctadecyl ammonium chloride.

[0125] Implementation Scheme 24. The method according to any one of Implementation Schemes 20 to 22, wherein the quaternary ammonium salt is present in an amount from 10 ppm to 700 ppm by weight based on the amount of solids in the sugarcane juice.

[0126] Implementation Scheme 25. The method according to Implementation Scheme 24, wherein the quaternary ammonium salt is present in an amount from 10 ppm to 160 ppm by weight based on the amount of solids in the sugarcane juice.

[0127] Implementation Scheme 26. The method according to Implementation Scheme 24, wherein the quaternary ammonium salt is present in an amount from 20 ppm to 100 ppm by weight based on the amount of solids in the sugarcane juice.

[0128] Implementation Scheme 27. The method according to any one of Implementation Schemes 20 to 22, wherein the cationic copolymer is a cationic copolymer of dialkylamine and epichlorohydrin, wherein the alkyl portion is a straight-chain or branched alkyl group containing 1 to 6 carbon atoms.

[0129] Implementation Scheme 28. The method according to Implementation Scheme 27, wherein the alkyl portion is a straight-chain or branched alkyl group containing 1 to 4 carbon atoms.

[0130] Implementation Scheme 29. The method according to Implementation Scheme 27, wherein the cationic copolymer is a cationic copolymer of dimethylamine and epichlorohydrin.

[0131] Implementation Scheme 30. The method according to any one of Implementation Schemes 20 to 22, wherein the cationic copolymer is present in an amount from 10 ppm to 150 ppm by weight based on the amount of solids in the sugarcane juice.

[0132] Implementation Scheme 31. The method according to Implementation Scheme 30, wherein the cationic copolymer is present in an amount from 10 ppm to 70 ppm by weight based on the amount of solids in the sugarcane juice.

[0133] Implementation Scheme 32. The method according to Implementation Scheme 30, wherein the cationic copolymer is present in an amount from 15 ppm to 40 ppm by weight based on the amount of solids in the sugarcane juice.

[0134] Implementation Scheme 33. The method according to any one of Implementation Schemes 20 to 22, wherein a phosphorus source is added before, during or immediately after the clarification step.

[0135] Implementation Scheme 34. The method according to any one of Implementation Scheme 33, wherein the phosphorus source is selected from the group consisting of any salt containing phosphate anions and cations.

[0136] Implementation Scheme 35. The method according to Implementation Scheme 33, wherein the phosphorus source is phosphoric acid.

[0137] Implementation Scheme 36. The method according to Implementation Scheme 34, wherein the phosphate anion is selected from hydrogen phosphite (HPO32-), dihydrogen phosphate (H2PO4-), orthophosphate (PO43-), orthophosphate (HPO42-), orthophosphate (H2PO4-), diphosphate (H2P2O62-), metaphosphate (PO3-), or pyrophosphate (P2O74-).

[0138] Implementation Scheme 37. The method according to Implementation Scheme 34, wherein the cation is selected from ammonium, sodium, or calcium.

[0139] Implementation Scheme 38. The method according to any one of Implementation Schemes 20 to 22, wherein the clarification step b includes preheating b1, pH correction b2 and heating b3 steps, during which the quaternary ammonium salt, the cationic copolymer and optionally the phosphorus source are added.

[0140] Implementation Scheme 39. The method according to Implementation Scheme 38, wherein the quaternary ammonium salt, the cationic copolymer, and optionally the phosphorus source are added between these steps b2 and b3.

[0141] Implementation Scheme 40. The method according to Implementation Scheme 38, wherein the quaternary ammonium salt, the cationic copolymer, and optionally the phosphorus source are added between and during steps b2 and b3.

[0142] Implementation Scheme 41. The method according to any one of Implementation Schemes 20 to 22, wherein the quaternary ammonium salt, the cationic copolymer, and optionally the phosphorus source are added as a homogeneous blend before, during, or immediately after the clarification step, or added separately but simultaneously, or separately and at different stages.

[0143] Implementation Scheme 42. A reagent kit comprising: - A quaternary ammonium salt having the formula (I): in: R1 and R2 are independently selected from C12 to C20 straight-chain alkyl groups. R3 and R4 are independently selected from C1 to C6 straight-chain alkyl groups; - A cationic copolymer, said cationic copolymer being a cationic copolymer of a dialkylamine and epichlorohydrin, wherein the alkyl portion is a straight-chain alkyl group containing 1 to 6 carbon atoms; and - Optional phosphorus source.

[0144] Implementation Scheme 43. The kit according to Implementation Scheme 42 comprises two or three solutions: - An aqueous-alcoholic solution containing 30% to 60% quaternary ammonium salts and 5% to 30% phosphorus sources. - An aqueous solution containing 40% to 60% by weight of a cationic copolymer at a concentration between 50% and 70% and 35% to 60% of a phosphorus source. - An aqueous solution of phosphoric acid source, optionally, with a concentration of phosphoric acid between 50% and 95% by weight.

[0145] Implementation Scheme 44. The kit according to Implementation Scheme 43, wherein it comprises an aqueous-alcoholic solution of 30% to 60% of a quaternary ammonium salt and 10% to 30% of a phosphorus source.

[0146] Implementation Scheme 45. The kit according to Implementation Scheme 43, wherein it comprises 40%-60% DHT and 5% to 30% an aqueous-alcoholic solution of phosphoric acid at a concentration between 50% and 95% by weight.

[0147] Implementation Scheme 46. The kit according to Implementation Scheme 43, wherein it comprises an aqueous-alcoholic solution of an aqueous phosphoric acid solution with a concentration of 10% to 30% by weight, which is between 50% and 95% by weight.

[0148] Implementation Scheme 47. The kit according to Implementation Scheme 43, wherein it comprises 40% to 60% by weight of an aqueous solution of a cationic copolymer at a concentration between 50% and 70% and an aqueous solution of a phosphorus source.

[0149] Implementation Scheme 48. The kit according to Implementation Scheme 43, wherein the kit comprises 40%-60% of DMA-Epi at a concentration of 50% to 70% and 40% to 60% of an aqueous solution of phosphoric acid at a concentration between 50% and 95% by weight.

[0150] Implementation Scheme 49. The kit according to Implementation Scheme 43, wherein the aqueous solution of the phosphorus source is an aqueous solution of phosphoric acid at a concentration of 70% to 85% by weight.

[0151] Other details or advantages of the invention will become clearer and more apparent from the examples given below.

[0152] Example Regulations DMA-Epi copolymer: 150 ppm by weight of sugar solids According to the Food and Drug Administration, the maximum dose under HHS § 173.60 Pt. 21 CFR Ch. I (4-1-11 version) is: “ c) Food additives are used as decolorizing agents and / or flocculants in the clarification of sugar solutions and juices in refineries. It is only used in sugar... It is added during the purification / clarification stage of liquid refining, and its concentration does not exceed 150 parts by weight of the copolymer of sugar solids. " DHT: 700 ppm by weight of sugar solids According to the Food and Drug Administration, the maximum dose under HHS § 173.400 Pt. 174 21 CFR Ch. I (version 4-1-00) is: “ c) Food additives are used as decolorizing agents in the clarification of sugar solutions in refineries under the following restrictions: 1) In this section The food additives described in paragraph (a)(1) are added only during the purification / clarification stage of sugar refining, and in amounts not exceeding the amount of sugar solids. 700 parts per million by weight. " Measurement methods Measure color and turbidity to control clarification.

[0153] The ICUMSA color of the mixed juice and the decanted juice was determined by measuring the absorbance of the juice solution at 420 nm and calculated using the following equation: Where A is the absorbance measured at 420 nm, b is the length of the cuvette, and C represents the concentration of the solution (g / 100 mL).

[0154] Juice turbidity was expressed as the difference between measurements at 720 nm before and after filtration through a 0.45 μm membrane. The turbidity before and after filtration was calculated using the following equation: in T is the transmittance measured at 720 nm, and b is the cuvette length.

[0155] Clarification performance was verified through clarification tests in order to evaluate the efficiency of sugarcane juice processing.

[0156] Example 1 Following the preheating step, the three compositions were metered into a fresh blend (15 Brix = 15% sugar solids by weight in the blend). Phosphoric acid was then added in the same manner for all treatments.

[0157] raw material The composition referred to herein as "DHT blend 1" is a solution comprising 53.3% by weight of dimethyl dioctadecyl ammonium chloride ("DHT") (dissolved in ethanol (75 / 25)), 25.9% by weight of an aqueous solution of phosphoric acid at a concentration of 85% by weight, 7.2% by weight of isopropanol, and 13.6% by weight of anhydrous ethanol. The ratio of the dimethyl dioctadecyl ammonium chloride to the phosphoric acid should be approximately 1.5 to 2.

[0158] The composition referred to herein as "DMA-Epi Mixture 1" is a solution comprising 50% by weight of an aqueous solution of dimethylamine-epimyl chloride copolymer and 50% by weight of an aqueous solution of phosphoric acid with a concentration of 85% by weight. The ratio between the dimethylamine-epimyl chloride copolymer and the phosphoric acid should be approximately 0.3 to 1.

[0159] Add lime in sufficient quantity to the mixture to bring the pH to 6.8-7.2, and heat the mixture at a temperature of 98ºC to 105ºC for 30 seconds.

[0160] High molecular weight anionic polyacrylamide (“polymer”) was also added to the mixture, and the treated juice was then stored for 10 minutes. Afterward, a sample of the supernatant was collected for analysis.

[0161] Color and turbidity were measured and compared between all tested compositions. For a fully successful treatment, the color of the decanted juice must be below 10,000 IU. Regarding turbidity, the lower the better.

[0162] Table 1. Clarification test results.

[0163] As shown in Table 1, the addition of 175 ppm of the DHT blend (Test #1.2) resulted in a 26% reduction in color. In this case, the color of the treated juice was worse than that obtained by sulfitization (Control; Test #1.5).

[0164] Treatment with DMA-Epi mixture 1 (Experiment #1.3) produced a clear juice with 9780 IU, representing a 46% reduction in color. A combination of 75 ppm DHT blend and 100 ppm DMA-Epi mixture 1 (Experiment #1.4) also resulted in good clarification, comparable to results obtained with 175 ppm DMA-Epi mixture alone. Both experiments resulted in better clarification compared to the control.

[0165] The turbidity values ​​of clarified juice treated with DHT blends and / or DMA-Epi mixtures were better than those obtained by sulfitization.

[0166] in conclusion The results above demonstrate that the method described in this invention improves the quality of the juice produced during the clarification step in the method for producing crystalline or raw sugar from sugarcane juice. The treatment proposed in Experiment #1.4 resulted in a 45% reduction in color and an 87% reduction in turbidity, which is considerably better than the 38% and 67% observed for sulfitization, respectively.

[0167] Example 2 Following the preheating step, the three compositions are metered into a fresh mixture. Phosphoric acid is then added in a manner consistent with the maximum authorized amount for each clarifying agent according to FDA regulations.

[0168] raw material The composition referred to herein as "DHT blend 2" is a solution comprising 53% by weight of dimethyl dioctadecyl ammonium chloride ("DHT") (dissolved in ethanol (75 / 25)), 40% by weight of anhydrous ethanol, and 7% by weight of an aqueous solution of phosphoric acid at a concentration of 85% by weight. The ratio of the dimethyl dioctadecyl ammonium chloride to the phosphoric acid should be approximately 5-8.

[0169] The composition referred to herein as "DMA-Epi Mixture 2" is a solution comprising 40% by weight of an aqueous solution of a dimethylamine-epimyl chloride copolymer and 60% by weight of an aqueous solution of phosphoric acid with a concentration of 85% by weight. The ratio of the dimethylamine-epimyl chloride copolymer to the phosphoric acid should be approximately 0.3-1.

[0170] Add lime in sufficient quantity to the mixture to bring the pH to 6.8-7.2, and heat the mixture at a temperature of 98ºC to 105ºC for 30 seconds.

[0171] High molecular weight anionic polyacrylamide (“polymer”) was also added to the mixture, and the treated juice was then stored for 10 minutes. Afterward, a sample of the supernatant was collected for analysis.

[0172] The color of ICUMSA was measured using the method described above.

[0173] Table 2. Clarification test results.

[0174] *Maximum authorized under US regulations in conclusion The results above demonstrate that the method described in this invention improves the quality of the juice produced during the clarification step in the method for producing crystalline or raw sugar from sugarcane juice, while adhering to the maximum authorized amount of each component. The treatment proposed in Test #2.4 resulted in a 42% reduction in color, and the successful treatment produced decanted juice with a color of less than 10,000 IU.

[0175] Example 3 - Crystal Sugar Production To evaluate the performance of the composition as a clarifying agent, industrial trials were conducted, and the results were compared with those obtained through sulfitization. The color of juice, syrup, and sugar was measured to control the clarification efficiency during the process.

[0176] As explained above, the CIUMSA color of the juice is determined by measuring the absorbance of the solution at 420 nm.

[0177] raw material Use DHT blend 2 and DMA-Epi mixture 2 as described in Example 2.

[0178] Tests and Results The industrial trials consisted of a 12-day test. It was conducted using "DHT blend 2" with an active content of 61 ppm, "DMA-Epi mixture 2" with an active content of 30 ppm, and H3PO4 at a dosage of 150 ppm. During the test, the proposed solution performed better than sulfitization, showing an average color reduction of 46% on the decanted juice. In the previous cycle, sulfitization provided an average color reduction of 30% on the decanted juice.

[0179] The final sugar color of the test according to the invention (measured according to method ICUMSA GS 9 / 1 / 2 / 3-8 (2011)) is 12% lower (better) than the final sugar color of the sugar obtained from sulfite.

[0180] Comparing the results of the sulfonation cycle with the solution tests presented herein, it is possible to see that the percentage reduction in color and sugar color are better during the tests according to the invention, reflecting laboratory results and enhancing the effectiveness of the developed solution in replacing sulfur in clarification methods.

[0181] in conclusion Based on the results of industrial trials, it is entirely possible to replace sulfur with the solution according to the invention in this method, and the replacement can bring benefits such as increased productivity, simplified methods and operations.

Claims

1. The use of a composition comprising a quaternary ammonium salt and a cationic copolymer for clarifying sugarcane juice during the production of crystalline sugar or raw sugar. The quaternary ammonium salt is a compound having formula (I): in: R1 and R2 are selected independently from C 12 To C 20 Straight-chain alkyl; R3 and R4 are independently selected from C1 to C4 straight-chain alkyl groups; and The cationic copolymer is a cationic copolymer of dialkylamine and epichlorohydrin, wherein the alkyl portion is a straight-chain alkyl group containing 1 to 6 carbon atoms; X is an anion selected from halide, nitrate, phosphate, or acetate ions.

2. The use according to claim 1, wherein X is a halide ion.

3. The use according to claim 1, wherein X is a chloride ion.

4. The use according to claim 1, wherein the quaternary ammonium salt is dimethyl dioctadecyl ammonium chloride.

5. The use according to claims 1 to 4, wherein the quaternary ammonium salt is present in an amount from 10 ppm to 700 ppm by weight based on the amount of solids in the sugarcane juice.

6. The use according to claim 5, wherein the quaternary ammonium salt is present in an amount from 10 ppm to 160 ppm by weight based on the amount of solids in the sugarcane juice.

7. The use according to claim 5, wherein the quaternary ammonium salt is present in an amount from 20 ppm to 100 ppm by weight based on the amount of solids in the sugarcane juice.

8. The use according to claim 1, wherein, The alkyl moiety is a straight-chain or branched alkyl group containing 1 to 4 carbon atoms.

9. The use according to claim 1, wherein, The cationic copolymer is a cationic copolymer of dimethylamine and epichlorohydrin.

10. The use according to claims 1 to 4, wherein the cationic copolymer is present in an amount from 10 ppm to 150 ppm by weight based on the amount of solids in the sugarcane juice.

11. The use according to claim 10, wherein the cationic copolymer is present in an amount from 10 ppm to 70 ppm by weight based on the amount of solids in the sugarcane juice.

12. The use according to claim 10, wherein the cationic copolymer is present in an amount from 15 ppm to 40 ppm by weight based on the amount of solids in the sugarcane juice.

13. The use according to any one of claims 1 to 4, wherein a phosphorus source is also added during the production of crystalline sugar or raw sugar.

14. The use according to claim 13, wherein the phosphorus source is selected from the group consisting of any salt containing phosphate anions and cations.

15. The use according to claim 13, wherein, The phosphorus source is selected from phosphoric acid.

16. The use according to claim 14, wherein, The phosphate anion is selected from hydrogen phosphite (HPO3). 2- dihydrogen phosphate (H2PO4) 4- phosphate PO4 3- orthophosphate HPO4 2- orthophosphate (H2PO4) - diphosphate H2P2O6 2- Metaphosphate PO3 - Or pyrophosphate P2O7 4- .

17. The use according to claim 14, wherein, The cation is selected from ammonium, sodium, or calcium.

18. The use according to claim 13, wherein the phosphorus source is present in a total amount from 50% to 400% by weight of the total weight of the quaternary ammonium salt and the cationic copolymer.

19. The use according to claim 18, wherein, The phosphorus source is present in a total amount ranging from 50% to 200% by weight of the total weight of the quaternary ammonium salt and the cationic copolymer.

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