Processes and apparatus for producing a dried carbohydrate preparation

Abstract

The present invention relates to processes and an apparatus for producing dried carbohydrate preparations starting from a carbohydrate starting preparation which is dissolved in water, and to dried carbohydrate preparations produced by these processes.

Description

[0001] DESCRIPTION

[0002] Method and device for producing a dried carbohydrate preparation

[0003] The present invention relates to methods and a device for producing dried carbohydrate preparations from a carbohydrate starting preparation dissolved in water, as well as to dried carbohydrate preparations produced by means of these methods.

[0004] For example, WO 01 / 19208 A1 describes processes for producing compressible raw materials, in particular isomaltulose and isomalt, by means of a spray dryer, wherein solutions or suspensions containing these components are sprayed into powders of these components with the addition of dry air and the resulting agglomerated products are subjected to subsequent drying and cooling.

[0005] Lipiäinen et al. (International Journal of Pharmaceutics, 510 (2016), 311-322) disclose spray-drying processes for the production of amorphous isomalt, sucrose, melibiose, and trehalose powders.

[0006] WO 2018 / 149707 describes processes for the production of solid isomaltulose- and trehalulose-containing materials, in which aqueous solutions containing isomaltulose and trehalulose are subjected to an evaporation process and then to a crystallization process in an extruder, whereby a solid product containing isomaltulose crystals and trehalulose is obtained following a subsequent cooling step.

[0007] The known drying processes for carbohydrate solutions are characterized by a number of disadvantages. These are often due to the fact that the products to be dried are multicomponent mixtures containing at least two components of different solubility in the solvent of the components to be dried.

[0008] This generally results in the less soluble component precipitating, particularly crystallizing, earlier in the drying process, while the more soluble, often hygroscopic, component remains in the residual solution and adheres as a syrup film to the less soluble components that have already crystallized. Such processes frequently lead to caking of the product to be dried and reduce the efficiency of the drying process, which may even lead to a production shutdown. Regular cleaning and maintenance work is therefore necessary, which can significantly impair the efficiency of continuously operated processes. Unwanted shutdown and restart of the dryer significantly reduces its availability and thus its cost-effectiveness. A syrup film adhering to hygroscopic products in particular can lead to undesired sticking of the products.Furthermore, the resulting products are often heterogeneous and exhibit undesirable, and often uncontrollable, sizes and size distributions of the resulting carbohydrate particles. However, it is desirable that the components of a carbohydrate solution to be dried be dried and obtained during the drying process in as homogeneous a form as possible, preferably in crystalline, especially semi-crystalline, form, with a desired, controllable crystal size distribution, and that the dried products exhibit high dimensional stability and correspondingly low stickiness.

[0009] The present invention is therefore based on the technical problem of providing a method and product that overcome the aforementioned disadvantages.

[0010] In particular, the present invention is based on the technical problem of providing a method for drying a carbohydrate starting preparation dissolved in water, which has at least two carbohydrates with different water solubility, in particular at least one poorly soluble carbohydrate and at least one readily soluble carbohydrate, which method leads to the provision of dried carbohydrate preparations efficiently and with as little disruption as possible and in particular enables the drying of carbohydrate preparations which are difficult or impossible to dry using conventional methods and which are also storage-stable.It is also a technical problem of the present invention to provide a process that leads to dried, at least partially crystalline carbohydrate preparations whose properties can be specifically adjusted and which can, in particular, provide particle sizes and particle size distributions, in particular crystal size distributions, of the resulting dried carbohydrate preparations that were previously unavailable, or at least could not be specifically adjusted. It is also a technical problem of the present invention to provide dried carbohydrate preparations whose properties can be specifically adjusted and which have advantageous properties that were previously unavailable.

[0011] The present invention solves the underlying technical problem by providing the teachings of the independent and dependent claims and the description. The present invention solves the underlying technical problem in particular by providing a process for producing a dried carbohydrate preparation from a carbohydrate starting preparation dissolved in water, comprising the steps: a1) Providing a carbohydrate starting preparation dissolved in water comprising at least one poorly soluble carbohydrate with a solubility of at most 50 g / 100 g and at least one readily soluble carbohydrate with a solubility of at least 66 g / 100 g (in each case g of dry matter in 100 g of solution, each measured at 50 °C in pure water), wherein the carbohydrate is a monomer or dimer,and a2) providing a dry product reservoir present in at least one injection area of ​​a vacuum mixing dryer having a dryer shaft, b) injecting the solution of the carbohydrate starting preparation at a temperature of 80 to 110 °C onto the dry product reservoir present in at least one injection area, c) drying and homogenizing the carbohydrate starting preparation sprayed onto the dry product reservoir at a temperature of 40 to 85 °C and a pressure of 30 to 600 mbar with mechanical agitation caused by the dryer shaft and transferring it from the injection area via a subsequent drying area into a subsequent discharge area of ​​the vacuum mixing dryer, d) obtaining the dried carbohydrate preparation, and e) discharging at least a portion of the dried carbohydrate preparation, in particular from the discharge area, and optionally from the drying area,especially from the discharge area of ​​the vacuum mixing dryer.

[0012] The present invention solves the technical problem underlying it in particular by providing dried carbohydrate preparations produced by the process according to the invention.

[0013] The present invention provides, in a first process step a), a solution of a carbohydrate starting preparation in water, wherein the carbohydrate starting preparation comprises at least one poorly soluble monomeric or dimeric carbohydrate with a solubility of at most 50 g / 100 g and at least one readily soluble monomeric or dimeric carbohydrate with a solubility of at least 66 g / 100 g (in each case g of dry substance in 100 g of solution, in each case measured at 50 °C in pure water). Furthermore, in this process step a), a dry product feedstock is provided in at least one injection area of ​​a vacuum mixer-dryer having one, in particular a single, dryer shaft. A dry product feedstock is a carbohydrate preparation that is in solid, preferably dried form, in particular at least partially crystalline form. This is located in at least one injection area of ​​a vacuum mixer-dryer.

[0014] In a particularly preferred embodiment, the dry product template provided in process step a2) has the same composition as the carbohydrate starting preparation provided in process step a1).

[0015] In a particularly preferred embodiment, the dry product template provided in process step a2) has a different composition than the carbohydrate starting preparation provided in process step a1).

[0016] In a particularly preferred embodiment of the present invention, the dry product template can be formed from one or more components that are present in the carbohydrate starting preparation to be dried.

[0017] In a particularly preferred embodiment, the dry product template can be isomalt, in particular semi-crystalline isomalt, in particular if the carbohydrate starting preparation is an isomalt starting preparation.

[0018] In a particularly preferred embodiment, the dry product template may be isomaltulose, in particular crystalline isomaltulose, especially if the carbohydrate starting preparation is a starting preparation containing isomaltulose and trehalulose.

[0019] In a process step b), the solution of the carbohydrate starting preparation, which has a temperature of 80 to 110 °C, is sprayed onto the dry product template present in at least one injection area.In this case, a part of the supplied solution is flashed directly in the injection area of ​​the dryer which is under reduced absolute pressure, i.e. the solvent water evaporates suddenly under reduced pressure, the carbohydrates dissolved therein are dried to fine particles immediately before they hit the dry product reservoir, possibly partly only after the primary particles have grown, and settle in dried form on the dry product reservoir present in the injection area, another significant part of the injected solution hits the dry product reservoir in liquid form and dries in the further course of the process, in particular in process step c), on its surface, in particular in layers or shell-like, together with the fine particles on the already existing solid and dry dry product reservoir.

[0020] In a subsequent process step c), the carbohydrate starting preparation sprayed onto the dry product template, i.e. the dry product template layered with liquid carbohydrate starting preparation and containing dried fine carbohydrate particles (hereinafter also referred to as drying material), is transferred, in particular continuously transferred, under mechanical agitation, i.e. in particular by means of the rotating dryer shaft, in a conveying flow direction starting from the upstream injection area via a subsequent drying area into a downstream discharge area of ​​the vacuum mixing dryer, and at the same time dried and homogenized at a temperature of 40 to 85 °C and a pressure of 30 to 600 mbar.The transfer through the rotating dryer shaft takes place under mechanical agitation, in particular by the dryer shaft present in the vacuum mixing dryer, which homogenizes, in particular mixes and kneads, the carbohydrate preparation during transport from the injection area via the drying area to the discharge area, in particular also in interaction with the additional mechanical elements present in the vacuum mixing dryer in a preferred embodiment, in particular disc elements and counter hooks. The preferably provided disc elements are preferably arranged on the dryer shaft in such a way that they serve to clean off drying material adhering to the inner wall of the dryer, to convey the drying material, and to precisely size the drying material.The preferably provided disc elements are also preferably arranged on the dryer shaft in such a way that, when the dryer shaft rotates about its longitudinal axis, they engage with the preferably provided counter hooks, which are preferably arranged on the inner wall of the dryer housing. This enables cleaning of the disc elements and defined comminution of the drying material. Furthermore, the counter hooks are preferably arranged and designed on the inner wall of the housing in such a way that they serve to clean drying material adhering to the dryer shaft and to achieve defined comminution of the drying material.In process step d), a dried carbohydrate preparation is obtained, in particular in the discharge area, and then in process step e) at least a portion of the dried carbohydrate preparation is discharged, in particular from the discharge area and optionally additionally from the drying area, in particular solely from the discharge area, of the vacuum mixing dryer.

[0021] The present invention enables controllable and efficient drying and crystallization of carbohydrate preparations containing carbohydrates with varying solubility under very mild conditions at temperatures of at most 85°C in an energy-saving manner. This extends the service life of the dryers, particularly in continuous drying processes, reduces their maintenance and repair costs, and provides dried carbohydrate preparations with advantageous product properties, in particular particle size distributions, particularly crystal size distributions. According to the invention, the liquid carbohydrate starting preparation is injected without spraying hot gas, as occurs, for example, in spray-drying processes. Advantageously, even highly concentrated, particularly highly evaporated carbohydrate preparations can be dried according to the invention.The drying of highly concentrated carbohydrate preparations enabled by the invention is energetically advantageous because less energy needs to be introduced into the evaporation process. The dried carbohydrate preparations obtained according to the invention are readily soluble and are in a flowable, storage-stable, non-sticky, and easily dosed state. In a preferred embodiment, the resulting carbohydrate preparations are at least partially crystalline, in particular completely crystalline. The particularly gentle drying process according to the invention reduces or prevents color formation and carbohydrate-specific decomposition reactions that may occur with conventional drying processes, in particular the formation of reducing substances such as HMF or GMF, which are undesirable in many applications.By targeted control of the process parameters, the dissolution rate, bulk density, angle of repose and / or flowability of the resulting crystalline and dried carbohydrate preparations can be specifically adjusted according to the invention and thus novel carbohydrate preparations can be obtained, in particular semi-crystalline carbohydrate preparations.

[0022] The partially crystalline dried carbohydrate preparations provided according to the invention in a preferred embodiment, preferably by means of the process according to the invention, in particular dried isomalt preparations or dried isomaltulose- and trehalulose-containing preparations, are particularly advantageous for applications in which the amorphous components present in these partially crystalline preparations, due to their hygroscopicity, remove and bind unwanted water from the immediate environment.

[0023] For example, it is known from EP0838529 that powdered sugar tends to absorb water and clump. Semi-crystalline products of the present invention can advantageously be used, for example, as an additive to powdered sugar to maintain and improve its shelf life and desired product properties, such as preventing clumping and thus increasing flowability. Compared to conventional excipients for improving flowability, such as starch, the preparations according to the invention, in particular the isomalt preparations, are also characterized by improved solubility and thus transparency in applications.The use of these preparations as components of, for example, powdered sugar preparations leads to advantages in many areas of powdered sugar application, such as an improved mouthfeel or reduced turbidity and improved transparency in solid, pasty and liquid products, for example in glazes or beverages.

[0024] In a particularly preferred embodiment, the present invention relates to an aforementioned process, wherein, following process step d), in a process step f), a first portion of the dried carbohydrate preparation obtained in process step d) is returned as a dry product feedstock under a pressure of 30 to 600 mbar from the discharge area and / or the drying area to the at least one injection area and / or dryer head of the vacuum mixer-dryer, and a second portion of the dried carbohydrate preparation obtained in process step d) is discharged from the vacuum mixer-dryer in process step e). This preferred embodiment is advantageously suitable for a continuous process.

[0025] The present invention therefore relates, in a preferred embodiment, to a continuously carried out process for producing a dried carbohydrate preparation from a carbohydrate starting preparation dissolved in water.

[0026] In a further embodiment, the present invention also relates to a semi-continuous or discontinuous, i.e. batch, process for producing a dried carbohydrate preparation from a carbohydrate starting preparation dissolved in water.

[0027] According to the invention, the dried carbohydrate preparation obtained in process step d) can preferably be removed from the drying area or discharge area, in particular from the drying area, in particular a region of the drying area located downstream of the conveyor stream, and returned.

[0028] In a particularly preferred embodiment of the present invention, the dry product template provided in process step a2) comprises, in particular consists of, a carbohydrate preparation having a water content of 0.0 to 10.0, in particular 0.1 to 8.0 wt.%, preferably 0.2 to 7.0 wt.% (in each case based on the total mass of the carbohydrate preparation).

[0029] In a particularly preferred embodiment of the present invention, the dry product template provided in process step a2) is a portion of the dried carbohydrate preparation obtained in process step d).

[0030] In a particularly preferred embodiment of the present invention, a vacuum mixing dryer is provided in process step a), wherein the vacuum mixing dryer comprises a housing with at least one injection opening, at least one discharge opening, at least one injection region spatially and functionally associated with the at least one injection opening, a discharge region spatially and functionally associated with the discharge opening and a drying region connecting the at least one injection region and the discharge region, in which drying region a dryer shaft having at least one disk element is arranged.

[0031] In a particularly preferred embodiment of the present invention, the dryer shaft has a length extending over the injection, drying and discharge area of ​​the vacuum mixing dryer.

[0032] In a particularly preferred embodiment of the present invention, the dryer shaft is located centrally in the housing of the vacuum mixer-dryer and along its longitudinal axis, which is preferably arranged horizontally relative to the ground. In a preferred embodiment, the entire dryer shaft is arranged in the housing of the vacuum mixer-dryer. Preferably, no additional dryer shaft is present in the vacuum mixer-dryer.

[0033] In a particularly preferred embodiment of the present invention, the dryer shaft has disc elements distributed along its longitudinal axis, in particular over its entire length, in particular over the entire length arranged in the dryer housing, preferably distributed at the same distance from one another.

[0034] In a particularly preferred embodiment of the present invention, each disc element has two bars arranged terminally and, as seen from the dryer shaft, distally, facing the inner wall of the housing, in particular arranged on the distal edge of the disc element.

[0035] In a particularly preferred embodiment of the present invention, the dryer shaft has disc elements along its entire length within the housing of the vacuum mixing dryer, with counter hooks spatially and functionally associated with the disc elements being arranged on the inner wall of the housing. The arrangement of disc elements and counter hooks is preferably provided such that the disc elements engage the counter hooks upon rotation of the dryer shaft, enabling cleaning of the disc element surfaces.

[0036] In a particularly preferred embodiment of the present invention, at least one counter hook is assigned to each disc element.

[0037] In a particularly preferred embodiment of the present invention, the housing has counter hooks over the entire length of the dryer shaft arranged in the housing.

[0038] In a particularly preferred embodiment of the present invention, it is provided that the vacuum mixing dryer has a housing on the inner wall of which at least one counter hook, in particular a plurality of counter hooks, are arranged, and wherein the at least one counter hook is spatially and functionally assigned to each disc element.

[0039] In a particularly preferred embodiment of the present invention, the vacuum mixing dryer has, in particular outside the housing, at least one return screw that functionally connects the drying area and / or discharge area, in particular the discharge area, with the at least one injection area and / or dryer head, in particular the dryer head.

[0040] In a preferred embodiment, the drying area and / or discharge area, in particular the discharge area, is connected to the return screw conveyor via a feed line for the return screw conveyor.

[0041] In a preferred embodiment, the return screw is connected to the dryer head and / or injection area, in particular to the dryer head, via a return pipe.

[0042] In a particularly preferred embodiment of the present invention, the vacuum mixing dryer is assigned a discharge lock connected to the discharge area, in particular the discharge opening, to which, in a preferred embodiment, at least one, in particular two discharge flaps are assigned.

[0043] In a particularly preferred embodiment of the present invention, a storage container, preferably under increased absolute pressure, is assigned to the vacuum mixing dryer, which is preferably connected to the vacuum mixing dryer via a feed line.

[0044] In a particularly preferred embodiment, the present invention relates to an aforementioned process, wherein the carbohydrate starting preparation provided in process step a1) is an isomalt starting preparation dissolved in water or an isomaltulose- and trehalulose-containing starting preparation dissolved in water.

[0045] In a particularly preferred embodiment of the present invention, the carbohydrate starting preparation dissolved in water provided in process step a1) has a water content of 5.0 to 95.0, in particular 15.0 to 87.0 wt.% (in each case based on the total mass of the carbohydrate starting preparation dissolved in water).

[0046] In a particularly preferred embodiment of the present invention, the water-dissolved carbohydrate starting preparation provided in process step a1) has a dry matter content of 5.0 to 95.0, in particular 13.0 to 85.0 wt.% (in each case based on the total mass of the water-dissolved carbohydrate starting preparation). In a particularly preferred embodiment of the present invention, the water-dissolved carbohydrate starting preparation, in particular Isomai t starting preparation, provided in process step a1) has a water content of 5.0 to 30.0, preferably 7.0 to 25.0, in particular 15.0 to 20.0 wt.% (in each case based on the total mass of the water-dissolved carbohydrate starting preparation).

[0047] In a particularly preferred embodiment of the present invention, the carbohydrate starting preparation, in particular isomalt starting preparation, dissolved in water provided in process step a1) has a dry matter content of 70.0 to 95.0, preferably 75.0 to 93.0, in particular 80.0 to 85.0 wt.% (in each case based on the total mass of the carbohydrate starting preparation dissolved in water).

[0048] In a particularly preferred embodiment of the present invention, the carbohydrate starting preparation dissolved in water provided in process step a1), in particular the starting preparation containing isomaltulose and trehalulose, has a dry matter content of 70.0 to 90.0, preferably 75.0 to 89.0, in particular 80.0 to 87.0 wt.% (in each case based on the total mass of the carbohydrate starting preparation dissolved in water).

[0049] In a particularly preferred embodiment of the present invention, the carbohydrate starting preparation dissolved in water provided in process step a1), in particular starting preparation containing isomaltulose and trehalulose, has a water content of 10.0 to 30.0, preferably 11.0 to 25.0, in particular 13.0 to 20.0 wt.% (in each case based on the total mass of the carbohydrate starting preparation dissolved in water).

[0050] In a particularly preferred embodiment of the present invention, the carbohydrate starting preparation provided in process step a1) comprises the poorly soluble carbohydrate 1,1-GPM (1-O-alpha-D-glucopyranosyl-D-mannitol) and the readily soluble carbohydrate 1,6-GPS (6-O-alpha-D-glucopyranosyl-D-sorbitol).

[0051] In a particularly preferred embodiment of the present invention, the isomalt starting preparation provided in process step a1) has a 1,1-GPM (1-O-alpha-D-glucopyranosyl-D-mannitol) and 1,6-GPS (6-O-alpha-D-glucopyranosyl-D-sorbitol) content of 90.0 to 100.0, in particular from 92.0 to 99.0, in particular from 93.0 to 98.0, in particular from 95.0 to 100.0 wt.% (based on the total dry mass of the isomalt starting preparation). In a particularly preferred embodiment of the present invention, the isomalt starting preparation provided in process step a1) has a 1,1-GPM (1-O-alpha-D-glucopyranosyl-D-mannitol) content of 35.0 to 60.0 wt.% and a 1,6-GPS (6-O-alpha-D-glucopyranosyl-D-sorbitol) content of 65 to 40 wt.% (each based on the total dry mass of the isomalt starting preparation).

[0052] In a particularly preferred embodiment of the present invention, the isomalt starting preparation provided in process step a1) has a 1,1-GPM (1-O-alpha-D-glucopyranosyl-D-mannitol) content of 15.0 to 30.0 wt.% and a 1,6-GPS (6-O-alpha-D-glucopyranosyl-D-sorbitol) content of 70.0 to 85.0 wt.% (each based on the total dry mass of the isomalt starting preparation).

[0053] In a particularly preferred embodiment of the present invention, the isomalt starting preparation provided in process step a1) comprises 1,1-GPS (1-O-alpha-D-glucopyranosyl-D-sorbitol), sorbitol, mannitol, or GPI or a mixture of two or more thereof.

[0054] In a particularly preferred embodiment of the present invention, the isomalt starting preparation provided in process step a1) comprises sorbitol, mannitol, or GPI in each case in an amount of 0.00 to 0.20, in particular of 0.04 to 0.17 wt.% (in each case based on the total dry mass of the isomalt starting preparation).

[0055] In a particularly preferred embodiment of the present invention, the isomalt starting preparation provided in process step a1) comprises 1,1-GPS in an amount of 0.20 to 0.70, in particular 0.30 to 0.60 wt.% (in each case based on the total dry mass of the isomalt starting preparation).

[0056] In a particularly preferred embodiment of the present invention, the isomalt starting preparation provided in process step a1) has a pH of 4.0 to 4.7, in particular 4.1 to 4.5.

[0057] In a particularly preferred embodiment, the present invention relates to an aforementioned process, wherein the poorly soluble carbohydrate provided in process step a1) is isomaltulose and the readily soluble carbohydrate is trehalulose, fructose and / or glucose.

[0058] In a particularly preferred embodiment, the present invention relates to an aforementioned process, wherein the isomaltulose- and trehalulose-containing starting preparation provided in process step a1) dissolved in water comprises isomaltulose and trehalulose, in particular optionally together with fructose, glucose, isomaltose or isomelezitose or a mixture of two or more thereof.

[0059] In a particularly preferred embodiment, the present invention relates to a process as mentioned above, wherein the carbohydrate starting preparation provided in process step a1) is a starting preparation containing isomaltulose and trehalulose dissolved in water, wherein the isomaltulose content thereof is from 65.0 to 98.0, in particular from 65.0 to 95.0, in particular from 65.0 to 90.0, in particular from 70.0 to 90.0, in particular from 75.0 to 88.0, in particular from 75.0 to 85.0 wt.% and the trehalulose content is from 2.0 to 35.0, in particular from 3.0 to 15.0, in particular from 5.0 to 15.0, in particular from 6.5 to 13.0, in particular from 6.0 to 12.0, in particular from 7.0 to 10.0 wt.% (each based on total dry mass the isomaltulose and trehalulose-containing starting preparation).

[0060] In a particularly preferred embodiment, the present invention relates to a process as mentioned above, wherein the carbohydrate starting preparation provided in process step a1) is a starting preparation containing isomaltulose and trehalulose dissolved in water, wherein the isomaltulose content thereof is from 65.0 to 98.0, in particular from 65.0 to 95.0, in particular from 65.0 to 90.0, in particular from 70.0 to 90.0, in particular from 75.0 to 88.0, in particular from 75.0 to 85.0 wt.% and the trehalulose content is from 2.0 to 35.0, in particular from 3.0 to 15.0, in particular from 5.0 to 15.0, in particular from 6.5 to 13.0, in particular from 6.0 to 12.0, in particular from 7.0 to 10.0 wt.% (each based on total dry mass the starting preparation containing isomaltulose and trehalulose), and which contains fructose, glucose and sucrose, and optionally isomelezitose and isomaltose.

[0061] In a particularly preferred embodiment of the present invention, the isomaltulose- and trehalulose-containing starting preparation provided in process step a1) comprises fructose, glucose, isomaltose or isomelezitose or a mixture of two or more thereof.

[0062] In a particularly preferred embodiment of the present invention, in process step b), the carbohydrate starting preparation is injected, in particular injected in a cyclic manner, from a storage container with an increased absolute pressure, in particular a pressure of more than 1 bar, in particular 1.5 to 3.0 bar, in particular 1.5 to 2.5 bar, in particular 2.0 to 3.0, into the injection region having a reduced absolute pressure, in particular a pressure of 30 to 600 mbar.

[0063] The injection provided in process step b) can be carried out in a clocked or non-clocked manner.

[0064] In a particularly preferred embodiment of the present invention, according to which an isomalt-containing starting preparation is dried according to the invention, process step c) is carried out for the provided isomalt starting preparation at a pressure of 30 to 150 mbar, in particular 35 to 130 mbar, in particular 40 to 150 mbar.

[0065] In a particularly preferred embodiment of the present invention, according to which an isomaltulose- and trehalulose-containing starting preparation is dried according to the invention, process step c) is carried out for the provided isomaltulose- and trehalulose-containing starting preparation at a pressure of 300 to 600 mbar, in particular 350 to 500 mbar.

[0066] In a particularly preferred embodiment of the present invention, following process step d), in a process step e), at least a portion of the dried carbohydrate preparation obtained in process step d) is discharged from the discharge area of ​​the vacuum mixing dryer.

[0067] In a particularly preferred embodiment of the present invention, following process step d), in a process step f), a first portion of the dried carbohydrate preparation obtained in process step d), in particular obtained from an isomalt starting preparation, is returned as a dry product feed to the at least one injection area and / or to the dryer head of the vacuum mixer-dryer under reduced absolute pressure, preferably at a pressure of 30 to 150 mbar, in particular 35 to 130 mbar, in particular 40 to 150 mbar, and a second portion of the dried carbohydrate preparation obtained in process step d) is discharged from the discharge area of ​​the vacuum mixer-dryer in process step e).

[0068] In a particularly preferred embodiment of the present invention, following process step d), in a process step f), a first portion of the dried carbohydrate preparation obtained in process step d), in particular obtained from a starting preparation containing isomaltulose and trehalulose, is returned as a dry product feed to the at least one injection area and / or to the dryer head of the vacuum mixer-dryer under reduced absolute pressure, preferably a pressure of 300 to 600 mbar, in particular 350 to 500 mbar, and a second portion of the dried carbohydrate preparation obtained in process step d) is discharged from the discharge area of ​​the vacuum mixer-dryer in process step e).

[0069] The present invention also relates in particular to a dried carbohydrate preparation, in particular producible according to one of the processes according to the invention.

[0070] In a particularly preferred embodiment of the present invention, the dried carbohydrate preparation obtained in process step d), in particular producible according to one of the processes according to the invention, has a water content of 0.0 to 10.0, in particular 0.1 to 8.0, in particular 0.1 to 7.9, in particular 0.1 to 7.5, preferably 0.2 to 7.5, in particular from 0.2 to 7.0 wt.% (in each case based on the total mass of the carbohydrate preparation, KF method).

[0071] The present invention also relates in particular to a dried carbohydrate preparation, in particular producible according to one of the processes according to the invention, which is characterized by a particle size distribution with a d50 value of 0.40 to 1.60 mm, in particular 0.45 to 0.90 mm, in particular 0.45 to 1.55 mm, in particular 0.71 to 1.44 mm.

[0072] The present invention also relates in particular to a dried carbohydrate preparation, in particular producible by one of the processes according to the invention, which is characterized by a dissolution rate of 80 to 105 seconds, in particular 80 to 102 seconds, in particular 81 to 102 seconds, in particular 94 to 101 seconds (each measured at 60°C and in 20 wt. % aqueous solution). The present invention also relates in particular to a dried carbohydrate preparation, in particular producible by one of the processes according to the invention, which is characterized by a bulk density of 0.70 to 0.90, in particular 0.70 to 0.89, in particular 0.76 to 0.89, in particular 0.84 to 0.86 g / ccm.

[0073] The present invention also relates in particular to a dried carbohydrate preparation, in particular producible according to one of the processes according to the invention, which is characterized by a flowability of 2.0 to 10.0, in particular from 5.0 to 9.5, in particular 5.2 to 9.3, in particular 6.7 to 8.3, in particular 6.8 to 8.0 seconds / 100 g (10 mm nozzle).

[0074] The present invention also relates in particular to a dried carbohydrate preparation, in particular producible according to one of the processes according to the invention, which is characterized by an angle of repose of 20.0 to 50.0, in particular of 30.0 to 40.0, in particular of 38.1 to 36.3, in particular of 37.8 to 37.6°.

[0075] The present invention also relates in particular to a dried carbohydrate preparation, in particular producible according to one of the processes according to the invention, which is characterized by a texture profile analysis (TPA) value of 5.0 to 30.0, in particular of 10.0 to 20.0, in particular 15.2 to 10.0, in particular 14.7 to 14.4 N / s.

[0076] The present invention also relates in particular to a dried carbohydrate preparation, in particular producible according to a process according to the present invention, wherein the dried carbohydrate preparation is semi-crystalline and in particular has a particle size distribution with a d50 value of 0.40 to 1.60 mm and / or a dissolution rate of 80 to 105 seconds (measured at 60 °C and in 20 wt. % aqueous solution) and / or a bulk density of 0.70 to 0.90 g / ccm and / or a flowability of 2.0 to 10.0 seconds / 100 g (10 mm nozzle) and / or an angle of repose of 20.0 to 50.0 ° and / or a texture profile analysis (TPA) value of 5.0 to 30.0 N / s.

[0077] In a particularly preferred embodiment of the present invention, the dried isomalt preparation obtained in process step d), in particular producible according to one of the processes according to the invention, has a water content of 0.0 to 10.0, preferably 0.1 to 5.0, in particular 0.2 to 4.0, in particular 3.5, in particular 2.8, in particular 1.6 to 1.9, in particular 0.5 to 0.8 wt. % (in each case based on the total mass of the isomalt preparation, KF method). The present invention also relates in particular to a dried isomalt preparation, in particular producible according to one of the processes according to the invention, which is characterized by a particle size distribution with a d50 value of 0.40 to 1.60 mm, in particular 0.45 to 0.90 mm, in particular 0.45 to 1.55 mm, in particular 0.71 to 0.87 mm.

[0078] The present invention also relates in particular to a dried isomalt preparation, in particular producible according to one of the processes according to the invention, which is characterized by a dissolution rate of 80 to 105 seconds, in particular 80 to 102 seconds, in particular 81 to 102 seconds, in particular 94 to 101 seconds (measured at 60 °C and in 20 wt.% aqueous solution).

[0079] The present invention also relates in particular to a dried isomalt preparation, in particular producible according to one of the processes according to the invention, which is characterized by a bulk density of 0.80 to 0.90, in particular 0.84 to 0.89, in particular 0.84 to 0.89, in particular 0.85 to 0.86 g / ccm.

[0080] The present invention also relates in particular to a dried isomalt preparation, in particular producible according to one of the processes according to the invention, which is characterized by a flowability of 6.0 to 10.0, in particular from 6.5 to 9.5, in particular 6.7 to 9.3, in particular 6.8 to 8.0 seconds / 100 g (10 mm nozzle).

[0081] The present invention also relates in particular to a dried isomalt preparation, in particular producible according to one of the processes according to the invention, which is characterized by an angle of repose of 20.0 to 50.0, in particular of 30.0 to 40.0, in particular 36.0 to 39.0°.

[0082] The present invention also relates in particular to a dried isomalt preparation, in particular producible according to one of the processes according to the invention, which is characterized by a texture profile analysis (TPA) value of 5.0 to 30.0, in particular of 10.0 to 20.0, in particular 10.0 to 15.2, in particular 14.4 to 14.7 N / s.

[0083] In a particularly preferred embodiment of the present invention, the dried isomaltulose- and trehalulose-containing preparation obtained in process step d) has a water content of 2.5 to 7.0, preferably 3.0 to 6.5, in particular 4.5 to 6.5 wt% (in each case based on the total mass of the isomaltulose- and trehalulose-containing preparation, KF method). In a particularly preferred embodiment of the present invention, the dried isomaltulose- and trehalulose-containing preparation obtained in process step d), in particular producible by one of the processes according to the invention, has a particle size distribution with a d50 value of 0.50 to 4.50, in particular 1.00 to 3.55, in particular 1.00 to 1.50 mm.

[0084] The present invention also relates in particular to a dried isomaltulose- and trehalulose-containing preparation, in particular producible according to one of the processes according to the invention, which is characterized by a dissolution rate of 80 to 105, in particular 80 to 102 seconds (measured at 60 °C and in 20 wt.% aqueous solution).

[0085] The present invention also relates in particular to a dried isomaltulose- and trehalulose-containing preparation, in particular producible according to one of the processes according to the invention, which is characterized by a bulk density of 0.70 to 0.90, in particular 0.72 to 0.79 g / ccm

[0086] The present invention also relates in particular to a dried isomaltulose- and trehalulose-containing preparation, in particular producible according to one of the processes according to the invention, which is characterized by a flowability of 2.0 to 9.0, in particular of 2.0 to 5.5 seconds / 100g (13 mm nozzle).

[0087] The present invention also relates in particular to a dried isomaltulose- and trehalulose-containing preparation, in particular producible according to one of the processes according to the invention, which is characterized by a flowability of 2.0 to 18.0, in particular of 10.0 to 17.0 seconds / 100g (8 mm nozzle).

[0088] The present invention also relates in particular to a dried isomaltulose- and trehalulose-containing preparation, in particular producible according to one of the processes according to the invention, which is characterized by a flowability of 2.0 to 10.0, in particular of 5.0 to 9.0 seconds / 100g (10 mm nozzle).

[0089] The present invention also relates in particular to a dried isomaltulose- and trehalulose-containing preparation, in particular producible by one of the processes according to the invention, which is characterized by a flowability of 0.5 to 9.0, in particular 1.0 to 5.0 seconds / 100g (15 mm nozzle). The present invention also relates in particular to a dried isomaltulose- and trehalulose-containing preparation, in particular producible by one of the processes according to the invention, which is characterized by a flowability of 0.1 to 5.0, in particular 0.1 to 2.0, in particular 0.1 to 0.5 seconds / 100g (25 mm nozzle).

[0090] The present invention also relates in particular to a dried isomaltulose- and trehalulose-containing preparation, in particular producible according to one of the processes according to the invention, which is characterized by an angle of repose of 20.0 to 50.0°, in particular of 30.0 to 40.0°, in particular 35.0 to 37.0° (for particle size distribution of the isomaltulose- and trehalulose-containing preparation: dso approximately 1.14 mm).

[0091] In a particularly preferred embodiment of the present invention, the dried carbohydrate preparation obtained in process step d) is semi-crystalline, i.e., it has crystalline and amorphous phases.

[0092] The present invention also relates in particular to a dried carbohydrate preparation, wherein the dried carbohydrate preparation is a dried isomalt preparation or a dried isomaltulose- and trehalulose-containing preparation, in particular producible according to a process according to the present invention, and wherein the dried carbohydrate preparation is partially crystalline.

[0093] The present invention also relates in particular to a dried carbohydrate preparation, wherein the dried carbohydrate preparation is a dried isomalt preparation, in particular producible according to a process according to the present invention, and wherein the dried carbohydrate preparation is partially crystalline.

[0094] The present invention also relates in particular to a dried carbohydrate preparation, wherein the dried carbohydrate preparation is a dried isomaltulose- and trehalulose-containing preparation, in particular producible according to a process according to the present invention, and wherein the dried carbohydrate preparation is partially crystalline.

[0095] The present invention also relates in particular to a product, in particular a powdered sugar preparation, comprising a dried carbohydrate preparation according to the invention, wherein the dried carbohydrate preparation is a dried isomalt preparation or a dried isomaltulose- and trehalulose-containing preparation, in particular producible according to a process according to the present invention, and wherein the dried carbohydrate preparation is partially crystalline.

[0096] In a particularly preferred embodiment, the product contains 0.5 to 10, in particular 1 to 8, in particular 2 to 6 wt.% dried carbohydrate preparation, preferably adding up to 100 wt.% with powdered sugar and, optionally, at most 1 wt.% flow aid.

[0097] The present invention also relates to a vacuum mixing dryer, suitable and equipped for carrying out a method according to the invention, said vacuum mixing dryer being characterized by the essential and optionally preferred device features disclosed above in connection with the method according to the invention.

[0098] The present invention also relates to a vacuum mixing dryer, suitable and configured for carrying out a method according to the invention, in particular comprising a housing with at least one injection opening, at least one discharge opening, at least one injection region assigned to the at least one injection opening, a discharge region assigned to the discharge opening, a drying region connecting the injection region and the discharge region, in which at least one dryer shaft, in particular one, that is to say in particular exactly a single dryer shaft, is arranged, which has at least one disk element with at least one bar, and at least one return conveyor screw arranged outside the housing and functionally connecting the drying region or discharge region to the at least one injection region and / or dryer head.

[0099] In a particularly preferred embodiment of the present invention, the vacuum mixing dryer according to the invention has a housing in which there is a dryer shaft with at least one disc element, in particular 1 to 55, in particular 33 to 55, in particular three to five, in particular three disc elements, each of which has or has at least one bar, in particular two bars.

[0100] In a particularly preferred embodiment of the present invention, the vacuum mixer-dryer according to the invention comprises a housing on whose inner wall at least one counter-hook, in particular a plurality of counter-hooks, are arranged and fixed. In a particularly preferred embodiment of the present invention, the vacuum mixer-dryer according to the invention comprises a housing, wherein spatially separated heating and cooling zones are present in the housing of the vacuum mixer-dryer, in particular with two separately controllable heating circuits. In a preferred embodiment, the housing of the vacuum mixer-dryer comprises a double-jacket heating and cooling system.

[0101] In a particularly preferred embodiment of the present invention, the vacuum mixing dryer according to the invention has a housing, wherein the drying area is separated from the discharge area of ​​the dryer housing by a preferably adjustable, in particular cross-section-regulating, in particular height-adjustable, discharge weir.

[0102] In a preferred embodiment, the adjustable discharge weir may comprise a non-adjustable partition wall and an adjustable partition wall.

[0103] According to the invention, a liquid carbohydrate starting preparation is provided in a process step a1) and a dry product template is provided in a process step a2).

[0104] In a preferred embodiment of the present invention, the amount of dry product initial charge is 20 to 50 wt.% (based on the total weight of dry product initial charge and injected carbohydrate starting preparation).

[0105] In a preferred embodiment of the present invention, the amount of injected carbohydrate starting preparation is 50 to 80 wt.% (based on the total weight of dry product template and injected carbohydrate starting preparation).

[0106] According to the invention, in a process step e) a dried carbohydrate preparation is discharged and in a process step f) a dried carbohydrate preparation is recycled as a dry product feedstock.

[0107] In a preferred embodiment of the present invention, 40 to 70 wt.% of dried carbohydrate preparation is discharged (based on total weight TS of dried carbohydrate preparation).

[0108] In a preferred embodiment of the present invention, 30 to 60 wt.% of dried carbohydrate preparation is recycled as dry product feedstock (based on the total dry matter weight of dried carbohydrate preparation). In a preferred embodiment, the mass ratio of dry product feedstock to injected carbohydrate feedstock is 0.50 to 0.70 (dry product feedstock in wt.% / injected carbohydrate feedstock in wt.%).

[0109] In a preferred embodiment, the mass ratio of injected carbohydrate starting preparation to discharged dried carbohydrate preparation is 1.00 to 1.5 (injected carbohydrate starting preparation in wt.% / discharged dried carbohydrate preparation in wt.%).

[0110] In a preferred embodiment, the mass ratio of discharged dried carbohydrate preparation to dried carbohydrate preparation returned as dry product initial charge is 1.00 to 1.5, in particular 1.2 to 1.4 (discharged dried carbohydrate preparation in wt.% / dried carbohydrate preparation returned as dry product initial charge in wt.%).

[0111] In the context of the present invention, the term "flash evaporation" or "flashed" refers to flash evaporation, i.e., the formation of steam upon entry into the reduced-pressure injection zone of the dryer. Flash evaporation creates an increase in supersaturation of the isomalt-containing solution, which, in combination with the shear forces acting on the solution, leads to nucleation at the dry product reservoir located in the injection zone. In a flash evaporator, steam is formed when the pressure in the dryer drops, particularly because the liquid enters the dryer superheated during flash evaporation. The energy transfer induced in this way leads to a cooling of the solution, especially of the supersaturated solution, with a simultaneous increase in the dry matter content, which results in nucleation.

[0112] In the context of the present invention, the term “carbohydrate” (here also referred to as saccharide) is understood to mean a polyhydroxyaldehyde or polyhydroxyketone as well as compounds obtained by reduction or oxidation thereof, in particular sugar alcohols and sugar acids.

[0113] In the context of the present invention, the term "monomer" refers to a monomeric carbohydrate, in particular a monosaccharide, especially glucose, fructose, sorbitol, and mannitol. In the context of the present invention, the term "dimer" refers to a dimeric carbohydrate, in particular a disaccharide, especially isomaltulose, trehalulose, sucrose, 1,1-GPM, 1,6-GPS, and 1,1-GPS.

[0114] In the context of the present invention, a saccharide may be present as a saccharide sugar, in particular fructose, glucose, sucrose, isomaltulose, trehalulose, isomaltose or isomelezitose, or as a saccharide alcohol, in particular 1,1-GPM, 1,6-GPS, 1,1-GPS, sorbitol or mannitol.

[0115] In the context of the present invention, the terms “carbohydrate preparation” and “carbohydrate starting preparation” are understood to mean a mixture of at least two carbohydrates.

[0116] In the context of the present invention, a "poorly soluble carbohydrate" is understood to mean a carbohydrate that has a solubility of at most 65 g / 100 g, in particular at most 60 g / 100 g, in particular at most 50 g / 100 g (per g of dry matter in 100 g of solution) in pure water, in particular distilled water, at a temperature of 50°C. Poorly soluble carbohydrates include, in particular, isomaltulose, mannitol, and GPM.

[0117] In the context of the present invention, a "highly soluble carbohydrate" is understood to mean a carbohydrate that has a solubility of at least 66 g / 100 g (per g of dry matter in 100 g of solution) in pure water, especially distilled water, at a temperature of 50 °C. A high-soluble carbohydrate is, in particular, sucrose, 1,6-GPS, 1,1-GPS, glucose, fructose, trehalulose, and sorbitol.

[0118] In the context of the present invention, “isomalt” (here also referred to as isomalt preparation) is understood to mean a mixture comprising 6-OaD-glucopyranosyl-D-sorbitol (1,6-GPS) and 1-OaD-glucopyranosyl-D-mannitol (1,1-GPM) and optionally 1-OaD-glucopyranosyl-D-sorbitol (1,1-GPS), in particular comprising at least 80.0, at least 85.0, in particular at least 90.0, in particular at least 94.0, in particular at least 95.0 wt.% of 1,1-GPM and 1,6-GPS (in each case based on the total dry mass of the isomalt).

[0119] In the context of the present invention, the term “isomalt” or “hydrogenated isomaltulose” is preferably understood to mean a mixture consisting of or comprising 1,1-GPM and 1,6-GPS, in particular a mixture consisting of or comprising 22 to 61 wt.%

[0120] 1.1-GPM and 78 to 39 wt.% 1,6-GPS, in particular an equimolar or nearly equimolar mixture consisting of or comprising 1,1-GPM and 1,6-GPS (each based on the dry substance of the isomalt).

[0121] Isomalt can therefore also be understood as mixtures consisting of or comprising 1,1-GPM and 1,6-GPS which do not have an equimolar ratio of 1,1-GPM to 1,6-GPS, but in which there is a higher 1,1-GPM than 1,6-GPS content or a higher 1,6-GPS than 1,1-GPM content.

[0122] In a particularly preferred embodiment, the isomalt comprises, in addition to the two components

[0123] 1.1-GPM and 1.6-GPS do not have any additional components.

[0124] In a particularly preferred embodiment, the isomalt comprises, in addition to the two components

[0125] 1,1-GPM and 1,6-GPS additionally contain one or more further components, for example mannitol, sorbitol, sucrose, 1,1-GPS (1-OaD-glucopyranosyl-D-sorbitol), glycosylglycitols, deoxy-disaccharide alcohols, GPI (glucopyranosyl-idit), isomaltose, isomaltulose, isomelezitose, hydrogenated or non-hydrogenated oligosaccharides, in particular hydrogenated or non-hydrogenated trisaccharides, and / or other substances.

[0126] In the context of the present invention, the terms isomaltulose and palatinose are used synonymously.

[0127] In the context of the present invention, an “isomaltulose- and trehalulose-containing mixture” (here also referred to as isomaltulose- and trehalulose-containing preparation) is understood to mean a mixture comprising isomaltulose and trehalulose, in particular obtained from an enzymatic conversion of sucrose by means of a sucrose isomerase to a sucrose isomer mixture containing isomaltulose and trehalulose, and, optionally, one or more further substances selected from the group consisting of sucrose, fructose, glucose, turanose, leucrose, isomaltose, raffinose, isomelezitose, 6-gluc isomaltulose and 1-gluc isomaltulose.

[0128] In the context of the present invention, "a carbohydrate starting preparation dissolved in water" is understood to mean a preparation consisting of at least two carbohydrates that is completely dissolved in water. In particular, a dissolved carbohydrate preparation, especially carbohydrate starting preparations, can also be a highly concentrated solution, also referred to as a syrup. The syrup can be in the supersaturated, metastable range with respect to individual carbohydrates dissolved therein.

[0129] In the context of the present invention, a "dry product precursor" is understood to mean a carbohydrate preparation that is present in solid, in particular at least partially crystalline or fully crystalline form. The "dry product precursor" is preferably present in dried, in particular agglomerated or powdered, form, in particular in a region of a vacuum mixer-dryer into which an aqueous carbohydrate solution to be dried is injected, and wherein the aqueous carbohydrate solution to be dried is at least partially sprayed onto the dry product precursor.

[0130] In the context of the present invention, the term "semi-crystalline" means that part of the carbohydrate preparation in question is in the form of crystals and another part is in amorphous form. A semi-crystalline product therefore has both amorphous and crystalline phases.

[0131] In the context of the present invention, a "dryer head" is understood to mean a terminal region of the vacuum mixing dryer, in the region of which the drive for the dryer shaft is preferably arranged and which, viewed in the conveying flow direction of the dryer shaft, is located above, i.e. upstream of, the injection region.

[0132] In the context of the present invention, an “injection area” is understood to mean the area of ​​the vacuum mixing dryer in which the carbohydrate starting preparation is injected and optionally also dried.

[0133] In the context of the present invention, “injection” is understood to mean in particular the introduction of a liquid medium, in particular liquid carbohydrate starting preparation, under increased pressure, with subsequent water evaporation by reducing the pressure, wherein no further product stream, in particular no heating gas or heating gas mixture, is introduced into the dryer in addition to the liquid medium. “Injection” is therefore not spray drying, and in particular not convection drying, according to which water evaporation is carried out by high temperatures of a heating gas. In the context of the present invention, a “drying region” is understood to mean the region of the vacuum mixing dryer in which drying but not injection of the carbohydrate starting preparation takes place. The drying region is located downstream of the injection region as seen in the conveying flow direction of the dryer shaft.

[0134] In the context of the present invention, a "discharge area" is understood to mean the area of ​​the vacuum mixer-dryer in which the carbohydrate starting preparation is discharged and optionally also dried. The discharge area is located downstream of the drying area, as seen in the conveying flow direction of the dryer shaft.

[0135] In the context of the present invention, an arrangement “proximal” to a given reference point is understood to mean a spatial arrangement close to or approximated to the reference point, while an arrangement “distal” to a given reference point is understood to mean a spatial arrangement far from the reference point.

[0136] In the context of the present invention, a "discharge weir" is understood to mean a mechanical device that causes a reduction in the throughput of the material flow, in particular a damming effect, in a container through which a material flow flows, in particular the housing of a vacuum mixer-dryer. A discharge weir can be designed as a partition arranged transversely to the longitudinal direction of the material flow, in particular the longitudinal direction of the housing, and preferably comprises a fixed and an adjustable partition.

[0137] In the context of the present invention, a “reduced, reduced or lowered” absolute pressure is understood to mean an absolute pressure that is reduced compared to the absolute ambient pressure, in particular the atmospheric pressure or standard pressure of 1 bar.

[0138] In the context of the present invention, an “elevated” absolute pressure is understood to mean an absolute pressure that is higher than the absolute ambient pressure, in particular the atmospheric pressure or standard pressure of 1 bar.

[0139] In the context of the present invention, “wt%” means “weight%”, “DSC” means differential scanning calorimetry, “TS” means dry substance, “KF” means Karl Fischer method, “GC” means gas chromatography, “HPLC” means high performance liquid chromatography or high pressure liquid chromatography, “TPA” means texture profile analysis and “NIR” means near infrared.

[0140] In the context of the present invention, the particle size distribution (in particular d50, CV (coefficient of variation)) is determined by sieve analysis according to method description ICUMSA GS 2 / 9-37.

[0141] In the context of the present invention, "X-ray diffraction" is a measurement method in which the recurring atomic distances in a substance under investigation generate signals at corresponding angles in the diffractogram. In amorphous substances, very different distances between the molecular chains exist. This leads to a very broad distribution in the diagram in the form of a very broad bell-shaped curve (halo). The regular arrangements in crystalline regions, on the other hand, produce much narrower distributions in the form of peaks. In diffractograms of real polymers, both halos and peaks are superimposed. By peak deconvolution, the intensities of the peaks and the halo can be determined, and from this, the X-ray crystallinity can be calculated.While crystalline solids show characteristic diffraction intensity maxima (visible as peaks in the X-ray diffractograms - intensity versus angle 29), amorphous substances show only diffuse scattering ("halo"), which is visible in the X-ray diffractogram as a flat, broad peak.

[0142] In the context of the present invention, flowability is tested using the ERWEKA GT granule tester. The outlet nozzle with an opening width of 10 mm is used. Approximately 100 g is weighed into a measuring beaker and transferred into the 480 mL funnel of the granule tester. The measuring beaker is then placed under the outlet nozzle, and the measurement is started. The measured time required for the sample to flow is standardized to a sample mass of 100 g and displayed. A triplicate determination is performed (according to the European Pharmacopoeia, 2.9.16 Flow Behavior).

[0143] In the context of the present invention, the "angle of repose" is investigated using the ERWEKA GT granulate tester. The outlet nozzle with an opening width of 10 mm is used. Approximately 150 mL is weighed into a measuring beaker and transferred into the 480 mL funnel of the granulate tester. The solid is allowed to flow from a funnel onto a collecting tray with a collecting plate attached. A cone forms on the plate, and excess product flows into the collecting tray. After the sample has completely flowed out, the resulting cone is measured using a laser beam, and the angle of repose is calculated. A triplicate determination is performed (European Pharmacopoeia, 2.9.16 Flow Behavior).

[0144] In the context of the present invention, the dry matter content of isomalt solutions is determined via the refractive index. For this purpose, the solution is applied to the prism of a digital refractometer with a sucrose scale, and the dry matter content is read on the refractometer as °Bx. Isomalt solutions with dry matter contents < 50 g / 100 g are measured directly. For isomalt solutions with dry matter contents > 50 g / 100 g, the sample is diluted 1 + 1 with deionized water, and the dry matter content is determined based on the measured refractive index at 20 °C. The measured value is corrected according to the specified formula. For samples diluted 1 + 1, the correction is performed first and then multiplied by 2. The correction formula for isomalt solutions is:

[0145] WTS = WTS ref, Sac. * 0.9866 + 0.0613.

[0146] WTS : corrected dry matter content for isomalt

[0147] WTS, ref. Sac. : read dry matter content in °Bx,

[0148] 0.9866 and 0.0613: Correction function for correcting the refractometrically determined dry matter content of the sucrose scale to isomalt

[0149] The result is given in g / 100g.

[0150] In the context of the present invention, the dry matter content of isomaltulose solutions is determined via the refractive index. For this purpose, the solution is applied to the prism of a digital refractometer with a sucrose scale, and the dry matter content is read on the refractometer as °Bx. The refractometric dry matter determination is carried out in a sample solution diluted in a weight ratio of 1+1 as [°Bx] at 20 °C. The measured value is multiplied by 2 and expressed as g / 100 g. For isomaltulose solutions, no correction is required; the read value can be used directly.

[0151] In the context of the present invention, the water content of solid isomalt and solid palatinose is measured by Karl Fischer titration. 0.2 g of palatinose and 0.3 g of isomalt are dissolved at 50 °C in a mixture of 30 mL of Hydranal solvent and 20 mL of formamide and simultaneously titrated with Hydranal titrant 5. The water content can be calculated from the weighed sample amount, the consumption of titrant 5, and the titer; modern Karl Fischer titrators perform these calculations automatically and provide the water content in g / 100 g sample as the result.

[0152] In the context of the present invention, the dissolution time is investigated in a thermostatted 1 L stainless steel container from IKA, which is equipped with an anchor stirrer, a temperature sensor, an ultrasonic sensor from Sensotech, and a scattered light sensor (homemade). 800 g of water are placed in the stainless steel container and heated to 60 °C while stirring. When the temperature in the container has stabilized at 60 °C, the sensors start recording the measured values. A few minutes later, 200 g of sample are added. After the sample has completely dissolved, the measured values ​​are recorded for a further few minutes. The measurement curves are then divided into three sections: baseline - dissolution process - baseline.The difference between the time of sample addition and the break point, when the measurement curve returns to a stable baseline after the dissolution process, is considered the dissolution time, i.e. the time until the last particle has dissolved.

[0153] In the context of the present invention, the bulk density is investigated in a funnel apparatus from Janz Präzisionstechnik. The receiving container of the funnel apparatus is filled with approximately 600 mL of sample. By moving a slide, the bottom opening of the receiving container is released, and the sample flows into the collecting container located below, which has a capacity of exactly 500 mL. Excess sample portions are removed by scraping them off with a ruler. The collecting container containing the sample is then weighed. The bulk density is calculated from the mass difference between the filled and empty collecting containers divided by the volume of the collecting container (500 mL). A duplicate determination is performed.

[0154] In the context of the present invention, the texture analysis (TPA) tests were conducted using the TA-XTplus Texture Analyzer from Stable Micro System with a 50 kg measuring cell. The P / 49 compression plate with a diameter of 4.9 cm was used as the tool. Between 100 and 120 mL of isomalt were poured into a 250 mL plastic measuring cup with an inner diameter of 6.8 cm. The measuring cup containing the isomalt was placed in the center of the measuring table with the aluminum plate, and the measurement was started. The following parameters were used:

[0155] The measurements were performed tenfold, with the measuring cup being filled with a fresh sample for each individual measurement. The slope of the curves was evaluated in the interval from 30 seconds to 35 seconds, as the measurement curves were linear for all samples within this range. The mean of the ten individual measurements is given as the result.

[0156] In the context of the present invention, the composition of carbohydrate-containing preparations is determined by gas chromatography (GC), unless explicitly stated otherwise.

[0157] In the context of the present invention, the water content is determined titrimetrically as total water content (free water) using the Karl Fischer method.

[0158] If quantitative information, in particular percentage information, of components of a product or composition is given in connection with the present invention, these add up to 100% of the composition and / or product together with the other explicitly stated or expertly apparent further components of the composition or product, unless explicitly stated otherwise or apparent to a person skilled in the art.

[0159] If in connection with the present invention a “presence”, a “containing”, a “having” or a “content” of a component is expressly mentioned or implied, this means that the respective component is present, in particular is present in a measurable amount.

[0160] If in connection with the present invention a "presence", a "containing" or a "having" of a component in an amount of 0 [unit], in particular mg / kg, pg / kg or wt.%, is expressly mentioned or implied, this means that the respective components are not present in a measurable amount, in particular are not present.

[0161] If the first and second decimal places or the second decimal place are not specified in connection with the present invention, they are to be set as 0.

[0162] In the context of the present invention, the term "and / or" means that all members of a group linked by the term "and / or" are disclosed both alternatively to one another and cumulatively among one another in any combination. For the expression "A, B, and / or C," this means that the following disclosure content is to be understood: a) A or B or C or b) (A and B), or c) (A and C), or d) (B and C), or e) (A and B and C).

[0163] In the context of the present invention, the terms "comprising" and "having" are understood to mean that, in addition to the elements explicitly covered by these terms, further, not explicitly mentioned elements can be added. In the context of the present invention, these terms are also understood to mean that only the explicitly mentioned elements are covered and no further elements are present. In this particular embodiment, the meaning of the terms "comprising" and "having" is synonymous with the term "consisting of". Furthermore, the terms "comprising" and "having" also encompass compositions which, in addition to the explicitly mentioned elements, also contain further elements not mentioned, which, however, are of a functional and qualitatively subordinate nature. In this embodiment, the terms "comprising" and "having" are synonymous with the term "consisting essentially of".

[0164] Further advantageous embodiments of the invention emerge from the subclaims.

[0165] The invention is explained in more detail using exemplary embodiments and associated figures.

[0166] The figures show: Figure 1 schematically the structure of a vacuum

[0167] mixing dryer,

[0168] Figure 2A is a schematic longitudinal section side view of a vacuum mixing dryer according to the invention,

[0169] Figure 2B is a cross-section through a vacuum mixing dryer according to the invention along the plane AB, showing the position and geometry of the adjustable discharge weir,

[0170] Figure 3 schematically shows the structure and arrangement of the disc element, bars and counter hooks,

[0171] Figure 4 X-ray powder diagram of dried

[0172] Isomalt preparation A

[0173] Figure 5 X-ray powder diagram of dried

[0174] Isomalt preparation B

[0175] Figure 6 X-ray powder diagram of dried

[0176] Isomalt preparation C

[0177] Figure 7 X-ray powder diagram of dried

[0178] Isomalt preparation D

[0179] Figure 8 X-ray powder diagram of a dried according to the invention

[0180] Preparation containing isomaltulose and trehalulose

[0181] Figure 9 SEM image (lOOx) of dried according to the invention

[0182] Isomalt preparation D and

[0183] Figure 10 SEM image (50x) of dried according to the invention

[0184] Isomalt preparation D.

[0185] List of reference symbols:

[0186] 1 vacuum mixing dryer

[0187] 2 storage containers

[0188] 5 Drive for dryer shaft

[0189] 7 Drive for return screw

[0190] 10 cylindrical housing (dryer cylinder)

[0191] 15 Housing inner wall

[0192] 16 Front wall

[0193] 18 dryer head

[0194] 20 injection opening

[0195] 22 Inlet valve

[0196] 24 feed line

[0197] 25 Injection area

[0198] 30 discharge opening

[0199] 34 adjustable partition wall of the discharge weir (discharge gate)

[0200] 35 Discharge area

[0201] 36 adjustable discharge weir

[0202] 37 Discharge lock

[0203] 38 non-adjustable partition wall of the discharge weir

[0204] 39 Discharge flap

[0205] 40 drying area

[0206] 50 dryer shaft

[0207] 51 Dryer shaft pin (shaft nail)

[0208] 70 disc element

[0209] 78 bars

[0210] 80 return screw conveyor

[0211] 81 Return screw failure

[0212] 82 Return screw feed

[0213] 90 counter hooks

[0214] 110 Heating zone examples:

[0215] Example 1:

[0216] Structure and function of the vacuum mixing dryer according to the invention

[0217] A vacuum mixing dryer according to the invention and used according to the invention is shown schematically in Figure 1; in the following, a vacuum mixing dryer is also referred to as a “dryer”.

[0218] Figure 1 shows a dryer (1). Carbohydrate solution to be dried is fed to the dryer (1) from a storage tank (2) via the feed valves (22) and feed lines (24), in particular via the injection openings (20) from the pressurized storage tank (2) into the vacuum-pressured dryer interior, in particular into the injection area (25). Figure 1 illustrates the conveying flow direction of the carbohydrate preparations to be dried by arrows along the longitudinal axis of the dryer shaft (50) (Figure 2) arranged in the horizontally arranged housing (10) of the dryer (1), which is mounted in the housing via dryer shaft journals (51).The material to be dried passes through the injection zone (25), defined by the arrangement of the injection openings (20) there, the downstream drying zone (40), and is partially discharged in the downstream discharge zone (35), which is partially separated from the drying zone (40) by an adjustable discharge weir (36). A portion of the dried material held back by the discharge weir (36) in the drying zone (40) does not, if necessary, reach the discharge zone (35), but is transported via an inlet return screw (82) to the return screw (80) by the return screw (80) provided with a drive (7), and then via a return screw (81) back into the dryer head (18) located upstream of the injection zone. The dryer head (18) is the terminal area of ​​the dryer (1) and is located in front of the injection area (25) in the direction of flow, i.e. upstream.The return screw conveyor (80) is located outside the dryer interior. Also shown is a heating zone (110) located on the outer wall of the dryer housing (10).

[0219] The internal structure of the dryer (1) includes the dryer shaft (50) running centrally in the longitudinal direction of the horizontal dryer cylinder (10), as well as various internal components, each with a specific function (Figures 2A, 2B, and 3). Counterhooks (90) are located on the inner wall of the dryer (1), and disc elements (70) and bars (78) fixed and located at their ends are located on the dryer shaft (50). The bars (78) ensure the mixing function, the cleaning of stationary dryer elements and in particular the dryer inner wall (15), and also the product transport. The counterhooks (90) on the dryer inner wall (15) enable the cleaning of the disc elements (70), bars (78), and dryer shaft (50). In addition, the freely selectable setting of the shaft speed, within the framework of design limitations, results in additional freedom for controlling the drying process and thus the product quality.The product travels along the dryer shaft (50) under mechanical agitation, i.e. movement, caused by its rotation, to the discharge area (35) on the end wall (16). At the same time, if desired, a defined portion of the dried product is returned upstream of the discharge area (35) through an inlet (82) for the return screw (80) into and through the return screw (80) to the dryer head (18), and from there, on the dryer head side upstream of the injection area (25), is fed into the dryer interior via a return screw (81). This returned portion of the dried product can serve as a dry product reservoir, providing a surface for drying additional carbohydrate solution. Here, too, flexibility in process control is gained by variability in the speed at which the return screw (80) is operated, allowing, for example, defined control of residence times.This recycling of the product stream is also important for the success of the drying process.

[0220] Located at the end wall (16) of the horizontal dryer cylinder (10), opposite the dryer head (18) at the other end of the dryer (1), is the discharge area (35), which is partially separated from the drying area (40) by an adjustable discharge weir (36). As explained, a partial flow of the dryer contents is retained by the height-adjustable discharge weir (36) (also referred to here as the weir), which reduces the cross-section of the dryer interior. If necessary, this flow is transported via the feed line (82) to the return screw (80), into and through the return screw (80), and then via a return pipe (81) back into the dryer head (18) as a dry product feed. The dried material which is guided over the weir (36) and not retained is discharged in portions through the discharge opening (30) from the discharge area (35) via discharge flaps (39) and the discharge lock (37) and is discharged into the downstream weighing container.Due to its backflow effect, the weir (36) also ensures that a portion of at least partially dried product is always present in the drying (40) and injection (25) areas. In the dryer (1), the concentrated isomalt solution is dried to a defined residual water content under targeted process control. A semi-crystalline product is produced. The dried isomalt product is discharged batchwise via the discharge area (35), for example, into a downstream weighing container.

[0221] Figure 2A shows a schematic longitudinal section side view of a vacuum mixing dryer (1) according to the invention. It is shown that the dryer (1), in particular its housing (10) is arranged horizontally, has a drive (5) for the dryer shaft (50), wherein the dryer shaft (50) is arranged centrally and centrally over the entire length of the housing (10) in the dryer (1). Also shown are the disc elements (70) arranged on the dryer shaft (50) and fixed thereto. The disc elements (70) each have two bars (78) arranged at the end, as seen from the dryer shaft, on the distal edge of the disc elements (70), only one of which bars is visible in the schematic side view shown here.

[0222] Also shown are counter hooks (90) arranged on the dryer inner wall (15), which are functionally and spatially assigned to the disc elements (70), which are arranged at a distance from each other essentially over the entire length of the longitudinal axis, in particular over the entire length arranged in the dryer housing (10), of the dryer shaft (50) and which extend essentially radially from the housing inner wall (15), to which they are fixed, to the dryer shaft (50). Figure 2B shows a cross-section along the plane AB according to Figure 2A. The discharge weir (36) comprises a partition wall (38) which blocks part of the cross-section (section AB) of the dryer interior and thus separates the product discharge area (35) from the drying area (40), and at the same time releases a defined part of the cross-section (AB) so that dried material can pass into the product discharge area (35) via the partition wall.Figure 2B illustrates that the discharge weir (36) reduces the cross-section of the interior of the dryer (1) and thus allows a backflow for material to be dried in the dryer interior.

[0223] Figure 3 shows a detail Z according to Figure 2A. Example 2:

[0224] Comparison isomalt drying process in batch operation

[0225] Isomalt solution (approximately 50 wt% dry matter (DS)) is evaporated to approximately 80 wt% DS in an evaporation station. This syrup is injected into a dryer without a return screw for crystallization. The dryer consists of three sections: injection, drying, and discharge.

[0226] The entire dryer is temperature-controlled (double jacket, 50 °C) and hydraulically driven. Counter hooks are located on the dryer's inner wall, and disc elements with attached bars are located on the dryer shaft. Three dosing pumps are available for injection. The pumps are mounted on nozzles and inject the syrup into the dryer's interior. The dryer operates at approximately 50 °C and 50 mbar. The injected isomalt grows into undefined balls or spheres and eventually forms a mortar-like slurry that encrustes the dryer's interior, solidifying there and making further conveyance and drying impossible.

[0227] Example 3:

[0228] Inventive isomalt drying process in batch operation

[0229] Isomalt solution (approximately 50 wt% dry matter (DS)) is evaporated to approximately 80 wt% DS in an evaporation station. This syrup is injected into a dryer without a return screw for crystallization. The dryer consists of three sections: injection, drying, and discharge.

[0230] The entire dryer is temperature-controlled (double jacket, 50 °C) and hydraulically driven. Counterhooks are located on the inner wall of the dryer, and disc elements with attached bars are located on the dryer shaft. Three dosing pumps are available for injection. The pumps are mounted on nozzles and inject the syrup onto the already crystallized inoculant (isomalt), which is present as a dry product in the dryer. The dryer operates at approximately 50 °C and 50 mbar. The injected isomalt grows into spherical structures and is ground on the bars or counterhooks. The water is evaporated in a vacuum.

[0231] When injecting the isomalt solution into the dryer, a viscous slurry can form over time, which can cause problems in the dryer. This slurry may encruste on the dryer's internal surfaces and solidify into a very hard layer. This hard layer is gripped by the bars on the dryer shaft, resulting in very high torque absorption of the drive.

[0232] If a limit is exceeded, the drive stops due to overload. These problems occur at the feed point for all three dosing pumps.

[0233] If the drive fails due to overload, it can no longer be put into operation immediately.

[0234] Cleaning the entire dryer is therefore frequently necessary. At the same time, the dryer's throughput can be increased. Continuous drying operation is not always possible.

[0235] Example 4:

[0236] Inventive isomalt drying process in continuous operation

[0237] In multi-stage evaporation stations, the isomalt solutions are concentrated to a desired dry matter content and transferred to a storage tank (2). From this tank, a desired amount of feed solution is injected into the vacuum mixer-dryer (1).

[0238] In preparation for the drying process, the isomalt solution is thickened to a defined dry matter content in a multi-stage evaporation station, preferably under vacuum at specific temperatures. This solution is temporarily stored in the storage tank (2) in order to be fed "quasi-continuously" to the dryer (1) via one or more timed inlet valves (22) at various feed points (20) along the dryer (1) (Figure 1) at defined time intervals and in adjustable quantities. Alternatively, it can be provided that the solution temporarily stored in the storage tank (2) is fed, i.e. injected, in a non-timed manner, i.e. continuously, via non-timed inlet valves. The feeding takes place in the form of injection and not spraying or jetting.While a portion of the supplied solution is flashed directly in the reduced-pressure injection area (25) of the dryer (1), i.e., suddenly evaporated under reduced pressure and dried to fine particles, another significant portion encounters the dry product receiver in liquid form and dries on this surface in a snowball-like manner onto the already existing dry product. The receiver vessel (2) is preferably pressurized, while the dryer (1) itself is under reduced pressure (also referred to here as vacuum). The receiver vessel (2) is equipped with trace heating to ensure a constant temperature in the reactant flow to the dryer (1). As a result, when the inlet valves (22) open, the injected solution experiences both a push from the preferably applied overpressure in the feed line (24) (pushing in) and a suction into the vacuum.The injection of the solution to be dried preferably takes place at several defined locations in the head area (18) of the dryer (1).

[0239] Both during start-up and during continuous operation of the dryer (1), the fresh isomalt solution to be dried is always injected into a dryer (1) already partially filled with dried product (dry product feed). If necessary, a partial flow of the dry product is returned via the external return screw (80) from the dryer outlet to the dryer head (18) in the opposite direction to the actual product flow in the dryer interior.

[0240] The dryer (1) is therefore partially filled with dried product (dry product pre-filled) before commissioning, for example, after cleaning. After the dryer (1) and its peripherals have warmed up to operating temperature, the vacuum is applied and the moving parts are started. Injection and continuous dryer operation can then begin immediately.

[0241] Even during continuous operation of the dryer (1), the fresh isomalt solution to be dried is always injected into a dryer (1) already partially filled with dry product (dry product feed). The isomalt solution is dried on the surface of the crystalline material already in the dryer (1), so that the particles already present gradually grow into a snowball.

[0242] The vacuum in the dryer (1) and the return screw conveyor, which is preferably very constant, is achieved by a powerful vacuum pump and is subject to only very slight pressure fluctuations. By varying the absolute drying pressure, the product quality is controlled in terms of residual moisture. At the same time, product properties can also be influenced during the process by controlling the drying pressure, for example, very rapid or slightly slower water release of the product as it transforms into the amorphous, crystalline phase.

[0243] The dryer (1) and the return screw conveyor (80) operate under vacuum, thus enabling very gentle product drying due to moderate temperatures during the process. In addition to numerous other advantages offered by the process according to the invention, it enables very high product quality, particularly with regard to quality parameters such as color or the undesired thermally induced cleavage of oligosaccharides when used in carbohydrate drying.

[0244] Example 5:

[0245] Drying of isomalt

[0246] Drying according to the invention was carried out in a vacuum mixing dryer according to the invention according to Example 3 and according to the process described in Example 4 for four different isomalt embodiments, here called Isomalt A, Isomalt B, Isomalt C and Isomalt D. Table 1 : Characterization of the dissolved carbohydrate (isomalt) starting preparations

[0247] The isomalt starting preparations described in Table 1 were dried according to the procedure of Examples 3 and 4 using the specific process parameters shown in Table 2 below.

[0248] Table 2: Process control / parameter set in the drying process

[0249] * Isomalt A and B: 0.5mm - 3.55mm, Isomalt C: 0.063mm - 0.9mm Isomalt D: <5.6mm

[0250] Table 3: Characterization of the dried isomalt preparation obtained according to the invention

[0251] SEM analyses and porosimetry measurements were performed. Neither the SEM images nor the porosimetry measurements (Hg measurements) revealed any evidence of internal pores. Only interstitial volumes could be measured.

[0252] The resulting dried isomalt preparations therefore exhibit no porous particles. The SEM images also revealed the presence of advantageous, largely spherical particles composed of individual crystallites in all four samples. In the case of Isomalt D, the large particles exhibit a blackberry-like substructure (Figures 9 and 10).

[0253] Texture profile analyses (TPA) were performed and the following values ​​were obtained: Isomalt A 15.2 N / s, Isomalt B 14.7 N / s, Isomalt C 14.4 N / s and Isomalt D 10.0 N / s.

[0254] DSC measurements were performed on the four dried isomalt preparations obtained. It was found that the product is essentially crystalline, but also contains a small amorphous portion, which is detectable by DSC measurement.

[0255] The four dried isomalt preparations obtained according to the invention were also examined by powder diffraction. The results are shown in Figures 4 to 7. Powder diffraction (PXRD) was performed using a Bruker D8 Advance in Bragg-Brentano geometry with Cu Ka radiation (= 1.54 Å; U = 40 kV, I = 40 mA) and long fine focus (LFF), with an irradiated sample length of L = 16 mm. Four powdered isomalt samples were prepared and examined in PMMA sample holders with sample holders of D = 25 mm (diameter) and T = 1 mm (well) in rotation mode. The following conditions were selected for the measurement: θ = 5-90°, step size θ = 0.01°, time count θ = 0.6 s, which resulted in a total measurement time of approximately 1.5 hours. To interpret the obtained diffractograms, CSD "BAVCAC" and CSD "BAGZEO" data sets were used from the Cambridge Crystallographic Data Centre database (CSD, version 5.3848) was used for the two diastereomers of isomalt, 1,6-GPS (6-OaD-glucopyranosyl-D-sorbitol) and 1,1-GPM dihydrate (1-OaD-glucopyranosyl-D-mannitol). The amorphous fraction in the isomalt sample was qualitatively evaluated by comparing the amorphous halo to the overall reflection peaks of the GPS / GPM phase using EVA VI software (Bruker).

[0256] All four isomalt samples examined exhibit peaks for the known crystalline phases 1,1-GPM dihydrate and 1,6-GPS. In the isomalt D sample, the sugar alcohols 1,1-GPM and 1,6-GPS are present solely in the form of crystalline 1,6-GPS and crystalline 1,1-GPM dihydrate (Figure 7). The other three isomalt samples A, B, and C also exhibit peaks from another crystalline phase that could be attributed to GPM anhydrate (Figures 4 to 6). Furthermore, these three samples exhibit a halo, typical of semi-amorphous (semi-crystalline) products.

[0257] It is evident that the dried product contains very low color values ​​and a very low amount of reducing substances ("reducing agents"), which is a clear indication of a very gentle drying process. The products are very stable in storage, readily soluble, non-sticky, free-flowing, and easy to dose.

[0258] According to the invention, a variable degree of drying can be set. If the drying is preferably carried out stoichiometrically, color formation can be prevented or reduced, which enables advantageous application in the production of hard caramels. If the drying is overdried, i.e., dried to a greater than stoichiometric level (removal of water of crystallization), the resulting carbohydrate preparations can be used particularly advantageously for chocolate production. If products are produced with residual moisture, the process according to the invention is particularly gentle and low-energy.

[0259] By carefully controlling the process parameters, the dissolution rate, bulk density, angle of repose, and / or flowability of the resulting crystalline and dried carbohydrate preparations can be precisely adjusted. Example 6:

[0260] Drying process of isomaltulose and trehalulose-containing starting preparation dissolved in water

[0261] A drying according to the invention was carried out in a vacuum mixing dryer (1) according to the invention according to Example 3 with an aqueous solution of a starting preparation containing isomaltulose and trehalulose.

[0262] Table 4: Characterization of the carbohydrate (isomaltulose and trehalulose)-containing starting preparations dissolved in water and dry product template (dried crystalline isomaltulose), solution of an isomaltulose and trehalulose-containing starting preparation referred to as ITL, the dry product template is a powdery, crystalline isomaltulose

[0263] The solutions of isomaltulose- and trehalulose-containing starting preparations described in Table 4 were dried according to the following procedure using an operating pressure in a range of 300 to 500 mbar.

[0264] The amount of dry product feedstock was 38 wt.% (based on the total weight of dry product feedstock and injected carbohydrate starting preparation), and the amount of injected carbohydrate starting preparation was 62 wt.% (based on the total weight of dry product feedstock and injected carbohydrate starting preparation).

[0265] 52 wt.% of dried carbohydrate preparation, in particular according to process step e), was discharged (based on the total weight of dry matter of dried carbohydrate preparation) and 38 wt.% of dried carbohydrate preparation was recycled as dry product feedstock (based on the total weight of dry matter of dried carbohydrate preparation).

[0266] A solution of a starting preparation containing isomaltulose and trehalulose (for characterization, see Table 4) under vacuum (350-400 mbar) is continuously injected at a rate of approximately 500 g / h into a dry product reservoir, namely powdered isomaltulose (approx. 3.5 kg). At the same time, a roughly corresponding amount of dry product is continuously discharged. It is returned from the dryer discharge area (35) to the dryer head (18) by the "quasi-continuous" addition of approximately 100 g / 10 min of powdered isomaltulose, or, later in the test, 100 g / 10 min of dry product. During the entire test run, the jacket temperature of the vacuum mixing dryer (1) is approximately 58 °C. At the appropriate vacuum, this leads to a product temperature in the dryer chamber of approximately 53-58 °C.With these parameter settings, the dry product feed and the portion-wise dry product return, the process can be operated continuously and stably, and over the course of the test period, a dry, granular product enriched increasingly with isomaltulose and trehalulose is obtained (characterization see Table 5).

[0267] Table 5: Characterization of the dried isomaltulose and

[0268] Trehalulose-containing carbohydrate preparation. The process was run continuously (with interruptions at night) for three days. The product described here corresponds to the dryer output on day 3 at the end of the experiment. A fresh solution to be dried was used daily.

[0269] DSC measurements were performed on the dried product, but no glass transition was observed upon initial heating. With decreasing purity, the melting peak becomes broader and shifts to lower temperatures due to a lower melting temperature caused by an increase in secondary components.

[0270] The melting peak of pure isomaltulose (dry product) is 127 °C. With increasing enrichment, the melting peak of the dried mixture becomes broader and shifts to a lower temperature (approximately 117 °C at 75% enrichment). This is due to the lower melting temperature caused by the increase in secondary components.

[0271] The resulting dried carbohydrate preparation containing isomaltulose and trehalulose was also analyzed by powder diffraction, analogous to Example 5. The results are shown in Figure 8. It is evident that the resulting product is crystalline and contains amorphous components, thus representing a semi-crystalline product.

[0272] Example 7:

[0273] Application of a dried isomalt preparation in powdered sugar

[0274] In the present example, a powdered sugar preparation containing an isomalt preparation produced according to the invention was compared with a conventional powdered sugar preparation with regard to its storage stability.

[0275] The conventional powdered sugar preparation contains 94.9 wt.% powdered sugar (finely ground sucrose) and 5.0 wt.% corn starch and 0.1 wt.% SiO2 as flow improvers. This sample serves as a comparison example.

[0276] The powdered sugar preparation according to the invention comprises 94.9 wt.% powdered sugar, 0.1 wt.% SiO2, and 5.0 wt.% isomalt preparation, prepared according to Example 5, Isomalt Preparation A. It differs from the comparative example only in the replacement of the cornstarch with isomalt. The two powdered sugar preparations were prepared by homogeneously mixing the aforementioned ingredients.

[0277] The preparations were then placed in glass jars and covered with aluminum foil, each of which had nine holes drilled into it. They were stored in a climate-controlled cabinet at 25 °C and 60% relative humidity for 14 days.

[0278] 14 days after homogeneous mixing of the respective sample components, a visual inspection was carried out regarding clumping and flowability.

[0279] Table 6: Flowability test

[0280] As can be seen from Table 6 above, the powdered sugar sample containing the isomalt preparation according to the invention has a significantly improved storage life, since after a storage time of 14 days no lump formation could be observed and the

[0281] The product was free-flowing. In contrast, clumping was observed after 14 days of storage for the comparative sample. The addition of isomalt instead of the conventionally used corn starch therefore leads to a significant improvement in storage stability.

Claims

CLAIMS 1. A process for producing a dried carbohydrate preparation from a carbohydrate starting preparation dissolved in water, comprising the steps: a1) providing a carbohydrate starting preparation dissolved in water comprising at least one poorly soluble carbohydrate with a solubility of at most 50 g / 100 g and at least one readily soluble carbohydrate with a solubility of at least 66 g / 100 g (in each case g of dry substance in 100 g of solution, each measured at 50 °C in pure water), wherein the carbohydrate is a monomer or dimer, and a2) providing a dry product reservoir present in at least one injection area (25) of a vacuum mixing dryer (1) having a dryer shaft (50), b) injecting the solution of the carbohydrate starting preparation at a temperature of 80 to 110 °C onto the dry product reservoir present in at least one injection area (25),c) drying and homogenizing the carbohydrate starting preparation sprayed onto the dry product reservoir at a temperature of 40 to 85 °C and a pressure of 30 to 600 mbar under mechanical agitation caused by the dryer shaft (50) and transferring it from the injection area (25) via a subsequent drying area (40) into a subsequent discharge area (35) of the vacuum mixer-dryer, d) obtaining the dried carbohydrate preparation, and e) discharging at least a portion of the dried carbohydrate preparation from the discharge area (35) and, optionally, from the drying area (40), in particular from the discharge area (35), of the vacuum mixer-dryer (1).

2. The method according to claim 1, wherein following method step d), in a method step f), a first portion of the dried carbohydrate preparation obtained in method step d) is returned as a dry product feedstock under a pressure of 30 to 600 mbar to the at least one injection region (25) and / or drying region (40) of the vacuum mixing dryer (1) and a second portion of the dried carbohydrate preparation obtained in method step d) is discharged from the vacuum mixing dryer (1) in method step e).

3. The method according to claim 1 or 2, wherein the vacuum mixing dryer (1) comprises a housing (10) with at least one injection opening (20), at least one discharge opening (30), at least one injection region (25) assigned to the at least one injection opening (20), a discharge region (35) assigned to the discharge opening (30), and a drying region (40) connecting the at least one injection region (25) and the discharge region (35), in which drying region a dryer shaft (50) having at least one disk element (70) is arranged, and wherein the at least one disk element (70) has at least one bar (78), preferably two bars (78).

4. Method according to one of the preceding claims, wherein the vacuum mixing dryer (1), in particular outside the housing (10), has at least one return screw (80) functionally connecting the drying area (40) and / or discharge area (35) with the at least one injection area (25) and / or dryer head (18).

5. Method according to one of the preceding claims, wherein the dryer shaft (50) has disc elements (70) over its entire length in the vacuum mixing dryer (1), and wherein, optionally, counter hooks (90) associated with the disc elements (70) are arranged on the inner wall (15) of the housing (10).

6. Method according to one of the preceding claims, wherein in method step b) the carbohydrate starting preparation is injected from a storage container at a pressure of more than 1 bar, in particular 1.5 to 3.0 bar, in particular 1.5 to 2.5 bar, in particular 2.0 to 3.0 bar, into the injection region (25) having a pressure of 30 to 600 mbar, in particular in a timed or non-timed manner.

7. A process according to any one of the preceding claims, wherein the carbohydrate starting preparation dissolved in water provided in process step a1) has a water content from 5.0 to 95.0, in particular 15.0 to 87.0 wt.% (in each case based on the total mass of the carbohydrate starting preparation dissolved in water).

8. A process according to any one of the preceding claims, wherein the poorly soluble carbohydrate is 1,1-GPM (1-O-alpha-D-glucopyranosyl-D-mannitol) and the highly soluble carbohydrate is 1,6-GPS (6-O-alpha-D-glucopyranosyl-D-sorbitol).

9. The method according to any one of the preceding claims, wherein the carbohydrate starting preparation dissolved in water provided in process step a1) is an isomalt starting preparation, in particular an isomalt starting preparation having a 1,1-GPM (1O-alpha-D-glucopyranosyl-D-mannitol) content of 35.0 to 60.0 wt.% and a 1,6-GPS (6-O-alpha-D-glucopyranosyl-D-sorbitol) content of 65.0 to 40.0 wt.% (each based on the total dry mass of the isomalt starting preparation) or an isomalt starting preparation having a 1,1-GPM (1-O-alpha-D-glucopyranosyl-D-mannitol) content of 15.0 to 30.0 wt.% and a 1,6-GPS (6-O-alpha-D-glucopyranosyl-D-sorbitol) content of 70.0 to 85.0 wt.% (each based on the total dry mass of the isomalt starting preparation).

10. The method according to claim 9, wherein process step c) and optionally f) for the provided isomalt starting preparation is carried out at a pressure of 30 to 150 mbar, in particular 35 to 130 mbar, in particular 40 to 150 mbar.

11. The method according to any one of claims 1 to 7, wherein the poorly soluble carbohydrate provided in process step a1) is isomaltulose and the readily soluble carbohydrate is trehalulose, fructose and / or glucose, in particular wherein the carbohydrate starting preparation provided in process step a1) is an isomaltulose- and trehalulose-containing starting preparation, in particular wherein the isomaltulose- and trehalulose-containing carbohydrate starting preparation also comprises fructose, glucose, isomaltose or isomelezitose or a mixture of two or more thereof.

12. The process according to claim 11, wherein process step c), and optionally f), for the provided isomaltulose- and trehalulose-containing starting preparation is carried out at a pressure of 300 to 600 mbar, in particular 350 to 500 mbar.

13. Process according to one of the preceding claims, wherein the dry product template provided in process step a2) comprises a carbohydrate preparation having a water content of 0.0 to 10.0, in particular 0.1 to 8.0 wt.%, preferably 0.2 to 7.0 wt.% (in each case based on the total mass of the carbohydrate preparation), in particular is a dried carbohydrate preparation obtained in process step d).

14. The method according to any one of the preceding claims, wherein the dry product template provided in process step a2) has the same composition as the carbohydrate starting preparation provided in process step a2) or a composition different therefrom.

15. Process according to one of the preceding claims, wherein the dried carbohydrate preparation obtained in process step d) has a water content of 0.0 to 10.0, in particular 0.1 to 8.0, preferably 0.2 to 7.0 wt.% (in each case based on the total mass of the carbohydrate preparation.

16. Dried carbohydrate preparation, wherein the dried carbohydrate preparation is a dried isomalt preparation or a dried isomaltulose- and trehalulose-containing preparation, in particular producible according to a process according to one of claims 9 to 12, and wherein the dried carbohydrate preparation is partially crystalline.

17. Product, in particular powdered sugar preparation, containing a dried carbohydrate preparation according to claim 16.

18. Vacuum mixing dryer (1), suitable and arranged for carrying out a method according to one of claims 4 to 15, in particular comprising a housing (10) with at least one injection opening (20), at least one discharge opening (30), at least one of the at least one injection opening (20) associated Injection area (25), a discharge area (35) associated with the discharge opening (30), a drying area (40) connecting the injection area (25) and the discharge area (35), in which at least one dryer shaft (50) is arranged, which has at least one disc element (70) with at least one bar (78), and at least one return conveyor screw (80) arranged outside the housing and functionally connecting the drying area (40) and / or discharge area (35) with the at least one injection area (25) and / or dryer head (18).

19. Vacuum mixing dryer according to claim 18, wherein at least one, preferably each, disc element (70) is assigned at least one counter hook (90).

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