Method for Producing 1,1-GPM and / or 1,6-GPS Enriched Isomalt Compositions

Abstract

The present invention relates to a method for producing an isomalt composition enriched with 1-O-α-D-glucopyranosyl-D-mannitol (hereinafter 1,1-GPM) and / or 6-O-α-D-glucopyranosyl-D-sorbitol (hereinafter 1,6-GPS) from an isomalt-containing solution containing hydrogenated isomaltulose, 1,1-GPM and / or 1,6-GPS-enriched isomalt compositions produced by the method of the present invention, and uses of these 1,1-GPM and / or 1,6-GPS-enriched isomalt compositions.

Description

[Technical field]

[0001] The present invention relates to a method for producing an isomalt composition enriched with 1-O-α-D-glucopyranosyl-D-mannitol (hereinafter referred to as 1,1-GPM) and / or 6-O-α-D-glucopyranosyl-D-sorbitol (hereinafter referred to as 1,6-GPS) from an isomalt-containing solution, i.e. a solution containing hydrogenated isomaltulose, to 1,1-GPM and / or 1,6-GPS-enriched isomalt compositions produced by the method according to the invention from an isomalt-containing solution, and to the use of these 1,1-GPM and / or 1,6-GPS-enriched isomalt compositions. [Background technology]

[0002] Isomalt (hydrogenated isomaltulose or hydrogenated palatinose) is an advantageous sugar substitute due to its non-cariogenicity, low calorific value, and diabetic suitability, containing 1,1-GPM and 1,6-GPS as the main components. 1,1-GPM and / or 1,6-GPS-enriched isomalt compositions from isomalt-containing solutions have superior suitability for many applications than products with an approximately equimolar ratio of 1,1-GPM to 1,6-GPS.

[0003] DE 2520173 A1 relates to a process for the production of 1,6-GPS and 1,1-GPM from isomaltulose and their use as sugar substitutes.

[0004] EP0625578A1 discloses the preparation of isomalt and its use as a sweetener in luxury and food products.

[0005] EP0859006B2 and WO1997 / 008958A1 relate to 1,6-GPS-enriched and 1,1-GPM-enriched mixtures, methods for producing 1,6-GPS and 1,1-GPM in pure form, and their uses.

[0006] Such isomalt compositions are used in many products, for example in the luxury goods and food sector. The very wide range of possible applications of such compositions requires compositions containing different proportions of 1,1-GPM and 1,6-GPS depending on the final product, and in particular compositions enriched in 1,1-GPM or 1,6-GPS.

[0007] However, currently no crystallization method is known that allows the simple, safe and efficient, in particular cost-effective and / or energy-efficient, preparation of such 1,1-GPM and / or 1,6-GPS-enriched isomalt compositions and 1,6-GPS and 1,1-GPM in pure form from an isomalt-containing solution.Therefore, there is a need for a method that allows the isomalt composition to be obtained from an isomalt-containing solution that is enriched in 1,1-GPM and / or 1,6-GPS compared to the content of 1,1-GPM and / or 1,6-GPS in the isomalt-containing solution present as starting solution. Summary of the Invention [Problem to be solved by the invention]

[0008] The technical problem underlying the present invention is therefore to provide a crystallization method for producing an isomalt composition enriched in 1,1-GPM and / or 1,6-GPS from an isomalt-containing solution, which can be carried out simply and safely and reproducibly results in high yields of an isomalt composition enriched in 1,1-GPM and / or 1,6-GPS from an isomalt-containing solution. [Means for solving the problem]

[0009] The present invention relates to a method for producing an isomalt composition enriched in 1,1-GPM and / or 1,6-GPS from an isomalt-containing solution, comprising the steps of: a) providing an isomalt-containing solution comprising 65-90% by weight, in particular 70-85% by weight, of isomalt (each based on the total weight of the isomalt-containing solution); b) subjecting the isomalt-containing solution provided in process step a) to flash evaporation in a reactor to generate crystal nuclei to obtain a first isomalt-containing suspension comprising a first crystalline phase and a first liquid phase; c) subjecting the first isomalt-containing suspension obtained in process step b) to a crystallization process to obtain a second isomalt-containing suspension comprising a second crystalline phase enriched in 1,1-GPM and a second liquid phase enriched in 1,6-GPS, d) separating the second crystalline phase enriched in 1,1-GPM and the second liquid phase enriched in 1,6-GPS of the second isomalt-containing suspension from process step c), and e) obtaining an isomalt composition enriched with 1,1-GPM and / or 1,6-GPS; The technical problem is solved by providing a method, characterized in that

[0010] The invention thus provides a method starting from an isomalt-containing solution as starting solution, prepared in process step a), which solution is provided using, inter alia, process steps b), c), d) and e), to provide two different phases, namely a second crystalline phase containing a higher 1,1-GPM content than the isomalt-containing solution used in process step a) and a second liquid phase containing a higher 1,6-GPS content than the isomalt-containing solution used in process step a).The invention thus allows the separation of the isomalt-containing solution into two phases, with a phase-specific enrichment of the components 1,1-GPM present in the isomalt-containing solution used as starting solution in the second crystalline phase and 1,6-GPS in the second liquid phase, providing, according to the invention, 1,1-GPM and 1,6-GPS-enriched phases and enriched compositions that are specifically enriched in terms of their 1,1-GPM and 1,6-GPS content compared to the respective 1,1-GPM and 1,6-GPS content in the starting solution, and that are particularly suitable for certain applications.

[0011] That is, according to the invention, by carrying out process steps b) and c), two phases are obtained, namely a second crystalline phase and a second liquid phase, the second crystalline phase enriched with 1,1-GPM having an increased 1,1-GPM content and a reduced 1,6-GPS content compared to the 1,1-GPM content in the isomalt-containing solution used in process step a), and the second liquid phase enriched with 1,6-GPS having a reduced 1,1-GPM content and an increased 1,6-GPS content compared to the 1,1-GPM content in the isomalt-containing solution used in process step a).By carrying out process steps d) and e), an isomalt-containing composition enriched in 1,1-GPM and 1,6-GPS, i.e. a composition characterized by a higher content of 1,1-GPM compared to the isomalt-containing solution prepared in process step a), as well as a further composition characterized by a higher content of 1,6-GPS compared to the isomalt-containing solution prepared in process step a) is obtained.

[0012] The present invention therefore contemplates a method for producing an isomalt composition enriched in 1,1-GPM and / or 1,6-GPS from an isomalt-containing solution, comprising in process step a) providing an isomalt-containing solution, i.e. a solution comprising an isomalt-containing mixture, in process step b) inducing crystal nucleation by flash evaporation in a reactor, in particular a nucleator, within which crystal nucleation and crystallization starting on these crystal nuclei occurs to obtain a first isomalt-containing suspension, in process step c) subsequent crystallization in a reactor, in particular the same or another reactor, in particular a crystallizer, to obtain a second isomalt-containing suspension comprising a second crystalline phase enriched in 1,1-GPM and a second liquid phase enriched in 1,6-GPS, in process step d) subsequent separation of the 1,1-GPM-enriched and 1,6-GPS-enriched phases, and in process step e) subsequent obtaining an isomalt composition enriched in 1,1-GPM and / or 1,6-GPS.

[0013] In an advantageous and particularly preferred manner, the method according to the present invention results in a simple, efficient, and especially cost-effective process.The particularly preferred intended continuous process mode can avoid the need to continuously add high purity nuclei at intervals, which is time-consuming and expensive in the production, compared to conventional nucleation reactors, especially slurry reactors.

[0014] In an advantageous and particularly preferred manner, the method according to the invention results in a particularly homogeneous crystal nucleation, because under practical operating conditions, i.e. during the method according to the invention, i.e. during the continuous operation of the reactor, crystal nuclei are continuously generated autonomously, so that local steps of initiating crystallization, in particular seeding, are omitted.In an advantageous manner, the method according to the invention results in autonomous crystal nucleation throughout the isomalt-containing solution used, thus resulting in the avoidance of common technical problems, whereas in common crystal nucleation reactors, in particular slurry reactors, the homogenization of the suspension used, which contains the seed, the crystallized solid and the solvent, is often problematic, because the addition of the crystal nuclei requires rapid and thorough mixing to ensure homogeneous crystal growth by avoiding local concentration gradients, which often leads to the destruction of already formed crystals. The present invention takes as its starting point the fact that the solubilities of 1,1-GPM and 1,6-GPS in solutions, especially in aqueous solutions, are different, i.e. both components have different solubility equilibria, so that both components are correspondingly enriched or depleted to different extents in the crystalline and liquid phases during flash evaporation and subsequent crystallization. The solubility equilibria are temperature dependent, and the enrichment of both components can be targeted by controlling preferably the shear and / or process parameters, especially the pressure and / or temperature and / or the concentration of the components 1,1-GPM and / or 1,1-GPS in the liquid phase.

[0015] Flash evaporation is preferably carried out at a reduced pressure relative to atmospheric pressure, the reduction in absolute pressure resulting in overheating of the liquid. Without being bound by theory, when adjusted to reduced absolute pressure, the pressure drop spreads in the reactor used for crystal nucleation, especially in the nucleation device, due to the defined wave propagation, which occurs more quickly than the temperature adaptation of the liquid medium, which is slowed down by heat and mass transfer at the phase boundary. This leads to a thermodynamic imbalance, and the overheating caused by the pressure drop is reduced by energy transfer, especially to the boiling nuclei and / or existing vapor bubbles.

[0016] The reduction in absolute pressure thus leads to the evaporation of a defined portion of the solvent used, in particular water, thereby extracting energy from the isomalt-containing solution used, i.e. the system is cooled in a defined manner. The temperature-dependence of the solubility equilibrium of 1,1-GPM and 1,6-GPS allows a defined nucleation and a defined start of crystallization on the nuclei generated under given process parameters and conditions, with the resulting nuclei and crystals enriched in 1,1-GPM and the remaining liquid enriched in 1,6-GPS. By targeted reduction in pressure and temperature control, the different solubility products of 1,1-GPM and / or 1,6-GPS are exploited to achieve an enrichment of the corresponding substances in crystalline and liquid form. The flash evaporation carried out in process step b) thus leads to the formation of a first isomalt-containing suspension comprising a first crystalline phase and a first liquid phase, enriched in 1,1-GPM in the first crystalline phase and in 1,6-GPS in the first liquid phase.

[0017] Flash evaporation is preferably carried out until sufficient enrichment of 1,1-GPM and / or 1,6-GPS is observed in the resulting first crystalline phase and in the first liquid phase to allow an efficient crystallization process and homogeneous crystal growth, in particular until crystal nuclei comprising, in particular consisting of, 1,1-GPM and crystals growing on and produced from these crystal nuclei are observed in the first crystalline phase.

[0018] The present invention also solves the technical problem underlying the present invention by providing intermediate products obtained within the scope of the implementation of the method, as well as the resulting 1,1-GPM and 1,6-GPS enriched compositions. The present invention therefore also provides a first and second crystalline phase and a liquid phase, as well as a 1,1-GPM and 1,6-GPS enriched composition.

[0019] According to the invention, the second crystalline phase and the crystals contained in the 1,1-GPM enriched isomalt composition are characterized by an advantageous morphology, in particular an advantageous length to width ratio of the crystals, in particular a small length to width ratio compared to conventionally crystallized products.

[0020] In one embodiment preferred according to the invention, the 1,1-GPM enriched isomalt compositions according to the invention as well as the second crystalline phase obtained in process step c) have a length to width ratio of the crystals contained therein of between 7.0 and 10.5, in particular between 7.5 and 10.0, in particular between 7.5 and 9.0, in particular between 7.5 and 8.5, in particular 8.0 (respectively average values).

[0021] In one embodiment preferred according to the invention, the 1,1-GPM enriched isomalt compositions according to the invention as well as the second crystalline phase obtained in process step c) have a length to width ratio of the crystals contained therein of 6.5 to 10.0, in particular 7.0 to 9.5, in particular 7.5 to 9.0, in particular 7.5 to 8.5, in particular 7.8 (respective medians).

[0022] The 1,1-GPM enriched isomalt compositions obtained according to the present invention can advantageously be easily separated from liquid components due to the specific length-to-width ratio of the crystals contained therein. The length-to-width ratio according to the present invention reduces the generation of crystal breakage and leads to a more uniform particle size distribution. This is advantageous because it is known that crystal breakage can sometimes lead to a more broad and non-uniform particle size distribution than a bimodal particle size distribution would have, and to blockage of the void volume in the crystal cake, which impairs the separability of the crystals with the drainage of the crystal cake, thus reducing the product yield. The reduction in crystal breakage made possible by the present invention also has the advantage that the product obtained does not show dust generation or only shows reduced dust generation after drying. Moreover, the relatively small and therefore more spherical length-to-width ratio according to the present invention leads to improved, especially faster sedimentation behavior in the centrifuge intended for the separation of the crystals, and preferably better sieving with improved separation accuracy for the dried product obtained. The length to width ratio according to the invention also reduces the generation of clogging particles, i.e. the formation of crystals characterized by a large length to width ratio, which likewise reduce production efficiency by blocking separation screens due to their elongated structure.

[0023] In an advantageous manner, the method according to the invention, in particular process step b), results in a particularly simple and efficient crystal nucleation and / or enrichment of 1,1-GPM in the first crystalline phase and of 1,6-GPS in the first liquid phase.

[0024] The present invention provides for the flash evaporation in process step b) to be carried out in a reactor, in particular a nucleator.The present invention provides for the crystallization process in process step c) to be carried out in a reactor, in particular a crystallizer.

[0025] In a particularly preferred embodiment, the present invention provides for carrying out the flash evaporation in process step b) in a reactor, in particular in a nucleation device, and for carrying out the crystallization process in process step c) in a reactor, in particular for carrying out the crystallization process in process step c) in the same reactor, in particular in the same nucleation device, as the flash evaporation in process step b).

[0026] In a particularly preferred embodiment, the present invention provides that the reactor used in process step b) is in particular a nucleation device in which process step c) can optionally be carried out, whereby the nucleation device is simultaneously a crystallization device.

[0027] In a particularly preferred embodiment, the present invention provides for carrying out the flash evaporation in process step b) in a reactor, in particular a nucleator, and for carrying out the crystallization process in process step c) in a reactor, in particular for carrying out the crystallization process in process step c) in a reactor separate from the flash evaporation in process step b), in particular a crystallizer.

[0028] Therefore, the present invention contemplates, in a particularly preferred embodiment, that process step b) and process step c) are carried out in the same reactor, in particular a nucleation device.

[0029] Likewise, the present invention contemplates, in a particularly preferred embodiment, that process step b) and process step c) are carried out in separate reactors, i.e. process step b) is carried out, in particular, in a nucleator and process step c) is carried out, in particular, in a crystallizer.

[0030] The present invention provides in a preferred embodiment that the flash evaporation in process step b) is carried out in a reactor, in particular a nucleation device, which reactor, in particular a nucleation device, comprises at least one stirring device.

[0031] In a preferred embodiment, mechanical agitation is performed during process step b), ie preferably a movement, in particular a stirring, of the isomalt-containing solution provided in process step a) is performed during the flash evaporation.

[0032] In a particularly preferred embodiment, the mechanical agitation in process step b) is carried out by means of at least one stirring device present in the reactor, in particular in the nucleation device.

[0033] In an advantageous and preferred manner, the stirring device, preferably present in the nucleation device, ensures mechanical stirring of the isomalt-containing solution used according to the invention for flash evaporation in process step b), in particular a particularly homogeneous and thorough mixing throughout the entire reactor contents. This preferred homogeneous and thorough mixing caused by the stirring device is achieved by shearing the isomalt-containing solution prepared in process step a) and used in process step b). The control of the shear in process step b), together with the control of the process parameters, in particular the pressure and / or temperature and / or the concentration of the components 1,1-GPM and / or 1,6-GPS, in particular the reduction of the temperature and the increase of the dry matter content, induces advantageous rapid and homogeneous crystal nucleation, in particular at the rotor blade tips, preferably present, of the stirring device, and contributes to the rapid and homogeneous distribution of the thus generated crystal nuclei throughout the entire reactor contents, thus ensuring a uniform growth of the crystal nuclei and a controlled reduction of the supersaturation in the entire isomalt-containing solution.

[0034] Surprisingly, the preferably intended control of the shear and / or process parameters, especially pressure and / or temperature, leads to a homogeneous crystal nucleation which is advantageous according to the invention, and the shear caused by the preferably intended stirring device advantageously avoids uncontrolled crystal nucleation which occurs only in the case of high local supersaturation, which due to lack of thorough mixing, disadvantageously spreads slowly and unevenly from the nucleation site throughout the remainder of the isomalt-containing solution.

[0035] The shear caused by the nucleation device, preferably the stirrer used in process step b), can be adjusted by the selection of the various stirring parameters of the stirrer, selected among other stirring parameters, the rotation speed, especially the blade tip speed, the stirrer geometry, especially the degree of cavitation at the rotor blade tips generated thereby, as well as the individual stirrer blades, especially the number and / or shape and / or angle of the rotor blades. In this way, the crystal nucleation, especially the number of crystal nuclei, can be controlled, the stirrer being especially a rotor-stator system.

[0036] Surprisingly, by controlling the shear and / or process parameters in process step b), it is possible to specifically influence the size and size distribution of the crystals produced in process step c), in particular the 1,1-GPM crystals.According to the invention, therefore, in process step c), it is possible to subject the first isomalt-containing suspension obtained in process step b) comprising a first crystalline phase and a first liquid phase to a crystallization process, thereby obtaining a second isomalt-containing suspension comprising a second crystalline phase and a second liquid phase, in particular a second isomalt-containing suspension comprising a homogeneous second crystalline phase and a second liquid phase, and by controlling the shear and / or process parameters, the number and size distribution of the 1,1-GPM crystals contained in the second crystalline phase of the second isomalt-containing suspension is specifically controlled.

[0037] In a preferred embodiment, the at least one stirring device is a rotor-stator system.

[0038] The present invention particularly preferably provides that the rotor-stator system comprises a rotor and a stator, in particular consists of a rotor and a stator.

[0039] The present invention particularly preferably provides that the rotor of the rotor-stator system is preferably a propeller stirrer, in particular a propeller stirrer with at least two rotor blades.

[0040] The present invention particularly preferably provides that the stator of the rotor-stator system is preferably a central tube.

[0041] The invention particularly preferably provides that the rotor, in particular the propeller stirrer, is present within the stator, in particular the central tube, in such a way that free rotation of the rotor is ensured.

[0042] The present invention particularly preferably provides that the rotor is present within the stator, in particular in such a way that the mechanical stirring preferably provided in process step b) allows the isomalt-containing solution provided in process step a) according to the invention to be permanently fed to the side of the rotor blade and discharged to the opposite side of the rotor blade, ensuring a complete and thorough mixing of the reactor contents.

[0043] The invention particularly preferably provides for the rotor blades of the propeller agitator to have a particular shape, in particular rectangular, trapezoidal, double trapezoidal or rectangular trapezoidal.

[0044] The present invention particularly preferably provides that the rotor of the rotor-stator system is a propeller-type agitator with at least two rotor blades, in particular three, in particular four, in particular five, preferably three rotor blades.

[0045] The present invention particularly preferably provides that the rotor blades of the propeller stirrer, starting from each central fixing point, lie at an angle of 36 to 180°, in particular 45 to 120°, in particular 72 to 90°, preferably 72°, to the adjacent rotor blade (calculated from the center of one rotor blade tip to the center of the next).

[0046] The present invention particularly preferably provides for a propeller stirrer in which the rotor of the rotor-stator system has at least two rotor blades, in particular three, in particular four, in particular five, preferably three rotor blades, each of which, starting from a central fixing point, is at an angle of 36° to 180°, in particular 45° to 120°, in particular 72° to 90°, preferably 72° to the adjacent rotor blade (calculated from the center of the tip of one rotor blade to the center of the next).

[0047] The invention particularly preferably provides that the rotor blades of the propeller stirrer are inclined around their longitudinal axis (starting from the rotor blade lying horizontally) by 0°, in particular 1°, in particular 5°, in particular 10°, in particular 20°, in particular 30°, in particular 40°, in particular 45°.

[0048] The present invention particularly preferably contemplates a propeller stirrer in which the rotor of the rotor-stator system has at least two rotor blades, in particular three, in particular four, in particular five, preferably three rotor blades, which are each at an angle of 36° to 180°, in particular 45° to 120°, in particular 72° to 90°, preferably 72° to the adjacent rotor blade (calculated from the center of the tip of one rotor blade to the center of the next) and are inclined around the longitudinal axis of the rotor blade (starting from the rotor blade lying horizontally) by 0°, in particular 1°, in particular 5°, in particular 10°, in particular 20°, in particular 30°, in particular 40°, in particular 45°.

[0049] The present invention particularly preferably contemplates a propeller stirrer in which the rotor of the rotor-stator system has at least two rotor blades, in particular three, in particular four and in particular five rotor blades, preferably three rotor blades, each of which is at an angle of 36° to 180°, in particular 45° to 120°, in particular 72° to 90°, preferably 72° to the adjacent rotor blade (calculated from the center of the tip of one rotor blade to the center of the next), inclined around the longitudinal axis of the rotor blade (starting from the rotor blade lying horizontally) by 0°, in particular 1°, in particular 5°, in particular 10°, in particular 20°, in particular 30°, in particular 40°, in particular 45° and has a particular shape, in particular rectangular, trapezoidal, double trapezoidal or rectangular trapezoidal.

[0050] The process mode according to the invention, in a preferred embodiment, leads to the nucleation of 1,1-GPM dihydrate in a nucleation device, in particular selectively, i.e. at least partially, in particular completely to the exclusion of 1,6-GPS.

[0051] In a particularly preferred embodiment of the present invention, the process according to the invention makes it possible to provide a first isomalt-containing suspension in process step b) in which the crystal nuclei consisting mainly, especially exclusively, of 1,1-GPM, especially 1,1-GPM dihydrate are present.The process according to the present invention therefore provides, in a preferred embodiment, especially in process step b), a first isomalt-containing suspension which is particularly homogeneously constituted, characterized in a preferred embodiment in that all the crystal nuclei contained therein consist of 1,1-GPM, especially 1,1-GPM dihydrate.Such an isomalt-containing suspension which mainly comprises 1,1-GPM crystal nuclei, especially the first crystal phase which has only 1,1-GPM crystal nuclei, is particularly well suited for the subsequent crystallization in process step c).

[0052] In an advantageous and particularly preferred manner, the process according to the invention results in higher operational safety, because, in particular in flash evaporation by targeted control of shear and / or process parameters, no dispersing medium, in particular alcohol, in particular isopropanol, is used compared to conventional crystal nucleation reactors, in particular slurry reactors, which results in a further reduction in operating costs in addition to improved operational safety due to reduced explosion risk.Moreover, advantageously, there is no need to obtain and feed slurry into an upstream process.

[0053] In an advantageous manner, the method according to the invention, in particular and in a preferred embodiment, allows the shear and / or process parameters, in particular supersaturation, temperature and pressure, to be controlled to produce homogeneous crystal nuclei comprising 1,1-GPM, in particular consisting of 1,1-GPM, and the first liquid phase of the first isomalt-containing suspension contains, in addition to the solvent, dissolved 1,6-GPS, so that in the subsequent crystallization process, particularly pure crystals comprising, in particular consisting of, 1,1-GPM or 1,6-GPS or 1,1-GPM and 1,6-GPS are obtained. This is based, without being bound by theory, on the very good growth properties of the crystal nuclei obtained according to the invention in process step b), while in typical industrial reactors, in particular slurry reactors, the process steps can lead to the production of broken edges, which in the continued crystal growth are preferred locations for crystal growth, i.e. crystallization is preferably carried out at these broken edges. The favorable crystal growth at these broken edges results in the inclusion of the solvent, in particular water or the liquid phase present according to the invention, in particular the isomalt-containing liquid phase, in the crystal structure of the obtained crystals, so that after the crystalline phase is obtained, these crystals contain impurities, in particular undesirable inclusions.

[0054] In an advantageous manner, the process according to the invention results in a particularly uniform crystal size distribution in the 1,1-GPM and / or 1,6-GPS-enriched phases, in particular a crystal size distribution which can be adjusted by controlling the shear and / or process parameters, so that these can be efficiently separated from other phases, in particular the liquid phase.

[0055] Thus, the present invention provides a particularly simple and efficient method for producing 1,1-GPM and / or 1,6-GPS enriched isomalt compositions, in particular pure 1,1-GPM and / or pure 1,6-GPS, from an isomalt-containing solution, taking advantage of the different solubility products of 1,1-GPM and 1,6-GPS, resulting in two separate phases with an increased, i.e. enriched, 1,1-GPM or 1,6-GPS content compared to the 1,1-GPM or 1,6-GPS content of the isomalt-containing solution according to process step a), respectively. In particular, the process format according to the present invention makes it possible to obtain both 1,1-GPM and 1,6-GPS enriched isomalt compositions in a single process. According to the present invention, it is also intended to carry out the process according to the present invention to obtain only 1,1-GPM enriched isomalt compositions. According to the present invention, in a preferred embodiment, it is also intended to carry out the process according to the present invention to obtain only 1,6-GPS enriched isomalt compositions.

[0056] The invention particularly contemplates providing in process step a) an isomalt-containing solution having a content of isomalt of 65-90% by weight (based on the total weight of the isomalt-containing solution).

[0057] In one embodiment preferred according to the invention, the isomalt-containing solution provided in process step a) comprises 70-85% by weight, in particular 70-80% by weight, preferably 72-80% by weight, preferably 74-80% by weight, preferably 76-80% by weight, preferably 70-78% by weight, preferably 74-76% by weight, preferably 70-74% by weight, preferably 70-75% by weight, preferably 70-76% by weight, preferably 72-76% by weight, preferably 74-76% by weight, preferably 75-80% by weight or preferably 76-80% by weight of isomalt (each based on the total weight of the isomalt-containing solution).

[0058] In one embodiment preferred according to the invention, the isomalt-containing solution provided in process step a) is a saturated solution, particularly preferably a supersaturated solution.

[0059] In one embodiment preferred according to the invention, the isomalt-containing solution provided in process step a) has a 1,1-GPM content of 35-61% by weight, preferably 46-56% by weight, preferably 48-55% by weight, preferably 49-54% by weight, preferably 50-53% by weight (respectively relative to the total weight of dry matter of the isomalt-containing solution).

[0060] In one embodiment preferred according to the invention, the isomalt-containing solution provided in process step a) has a 1,6-GPS content of 39 to 65% by weight, preferably 44 to 54% by weight, preferably 45 to 52% by weight, preferably 46 to 51% by weight, preferably 47 to 50% by weight (respectively based on the total weight of dry matter of the isomalt-containing solution).

[0061] In one embodiment preferred according to the invention, the isomalt-containing solution provided in process step a) has a 1,1-GPM content of 1,1-GPM of 35 to 61 wt.-%, preferably 46 to 56 wt.-%, preferably 48 to 55 wt.-%, preferably 49 to 54 wt.-%, preferably 50 to 53 wt.-% and a 1,6-GPS content of 1,6-GPS of 39 to 65 wt.-%, preferably 44 to 54 wt.-%, preferably 45 to 52 wt.-%, preferably 46 to 51 wt.-%, preferably 47 to 50 wt.-%.

[0062] In one embodiment preferred according to the invention, the isomalt-containing solution provided in process step a) has a 1,1-GPM content of 35-44% by weight and a 1,6-GPS content of 56-65% by weight (each based on the total weight of dry matter of the isomalt-containing solution).

[0063] In one embodiment preferred according to the invention, the isomalt-containing solution provided in process step a) has a 1,1-GPM content of 35-50% by weight, preferably 37-48% by weight, preferably 39-46% by weight, preferably 39-44% by weight, preferably 39-42% by weight (each based on the total weight of dry matter of the isomalt-containing solution).

[0064] In one embodiment preferred according to the invention, the isomalt-containing solution provided in process step a) has a 1,6-GPS content of 50-65% by weight, preferably 52-63% by weight, preferably 54-61% by weight, preferably 56-59% by weight, preferably 58-59% by weight (respectively based on the total weight of dry matter of the isomalt-containing solution).

[0065] In one embodiment preferred according to the invention, the isomalt-containing solution provided in process step a) has a 1,1-GPM content of 1,1-GPM of 35-50% by weight, preferably 37-48% by weight, preferably 39-46% by weight, preferably 41-44% by weight, preferably 41-42% by weight and a 1,6-GPS content of 1,6-GPS of 50-65% by weight, preferably 52-63% by weight, preferably 54-61% by weight, preferably 56-59% by weight, preferably 58-59% by weight (each based on the total weight of dry matter of the isomalt-containing solution).

[0066] In one embodiment preferred according to the invention, the isomalt-containing solution provided in process step a) has a 1,1-GPM content of 35 to 50% by weight and a 1,6-GPS content of 50 to 65% by weight (each based on the total weight of dry matter of the isomalt-containing solution).

[0067] In one embodiment preferred according to the invention, the isomalt-containing solution provided in process step a) has a 1,1-GPM content (based on the total weight of dry matter of the isomalt-containing solution) of 45-57% by weight, preferably 47-56% by weight, preferably 48-55% by weight, preferably 49-54% by weight, preferably 50-53% by weight.

[0068] In one embodiment preferred according to the invention, the isomalt-containing solution provided in process step a) has a 1,6-GPS content (based on the total weight of dry matter of the isomalt-containing solution) of 43 to 55% by weight, preferably 44 to 53% by weight, preferably 45 to 52% by weight, preferably 46 to 51% by weight, preferably 47 to 50% by weight.

[0069] In one embodiment preferred according to the invention, the isomalt-containing solution provided in process step a) has a 1,1-GPM content of 1,1-GPM of 45-57% by weight, preferably 47-56% by weight, preferably 48-55% by weight, preferably 49-54% by weight, preferably 50-53% by weight and a 1,6-GPS content of 1,6-GPS of 43-55% by weight, preferably 44-53% by weight, preferably 45-52% by weight, preferably 46-51% by weight, preferably 47-50% by weight.

[0070] In one embodiment preferred according to the invention, the isomalt-containing solution provided in process step a) has a 1,1-GPM content of 45 to 57% by weight and a 1,6-GPS content of 43 to 55% by weight (each based on the total weight of dry matter of the isomalt-containing solution).

[0071] In one embodiment preferred according to the invention, the isomalt-containing solution provided in process step a) has a temperature of 50-90° C., preferably 60-90° C., preferably 61-85° C., preferably 64-85° C., preferably 50-80° C., preferably 60-80° C., preferably 60-75° C., preferably 64-75° C., preferably 64-75° C., or preferably 64-70° C. In one preferred embodiment, the isomalt-containing solution is adjusted to one of the abovementioned temperatures in process step a).

[0072] In one embodiment preferred according to the invention, the isomalt-containing solution provided in process step a) comprises 1,1-GPM, 1,6-GPS and at least one substance selected from the group consisting of 1,1-GPS, further deoxydisaccharide alcohols, polysaccharides, oligosaccharides, trisaccharides, monosaccharides, disaccharides, sorbitol, mannitol and isomaltetose.

[0073] In one embodiment preferred according to the invention, the isomalt-containing solution provided in process step a) comprises 1,1-GPM, 1,6-GPS and at least one substance selected from the group consisting of 1,1-GPS, further deoxydisaccharide alcohols, oligosaccharides, trisaccharides, monosaccharides, disaccharides, sorbitol, mannitol and isomaltetose.

[0074] In one embodiment preferred according to the invention, the isomalt-containing solution provided in process step a) and further processed in process steps b) and c) does not contain any further substances besides water, 1,1-GPM, 1,6-GPS and at least one substance selected from the group consisting of 1,1-GPS, further deoxydisaccharide alcohols, oligosaccharides, trisaccharides, monosaccharides, disaccharides, sorbitol, mannitol and isomerezitose.

[0075] In one embodiment preferred according to the invention, the isomalt-containing solution provided in process step a) and further processed in process steps b) and c) does not contain gum arabic.

[0076] In one embodiment preferred according to the invention, the isomalt-containing solution provided in process step a) and further processed in process steps b) and c) contains no further substances besides water and 1,1-GPM and 1,6-GPS.

[0077] In one embodiment preferred according to the invention, the isomalt-containing solution provided in process step a) is a solution of isomalt in a solvent, in particular water, ethanol, propanol, isopropanol, butanol, isobutanol or a mixture thereof. In a particularly preferred embodiment, the isomalt-containing solution provided in process step a) is an aqueous solution with a low proportion of ethanol, propanol, isopropanol, butanol and / or isobutanol, in particular 0.1 to 5% by volume of alcohol based on the total aqueous solution. In a further particularly preferred embodiment, the solvent of the isomalt-containing solution provided in process step a) is water, in particular fully demineralized water. Preferably, the isomalt-containing solution provided in process step a) is free of organic solvents.

[0078] In one embodiment preferred according to the invention, the isomalt-containing solution provided in process step a) is an aqueous solution, in particular an aqueous solution having a pH value in the range 3.0-8.0, preferably 3.5-7.5, preferably 4.0-7.0, preferably 4.3-6.5, preferably 4.6-6.0, preferably 4.8-5.5 or preferably 4.9-5.5, preferably 4.9, preferably 6.0, preferably 8.0, preferably 4.5, preferably 4.0, preferably 3.5, preferably 3.0.

[0079] In one embodiment preferred according to the invention, the isomalt-containing solution is prepared directly from isomalt and water, optionally from isomalt, water and further components as mentioned above.

[0080] In one embodiment preferred according to the invention, the isomalt-containing solution provided in process step a) is obtained in a process step a1) which is carried out prior to process step a) from an isomalt-containing starting solution or suspension by evaporation or reverse osmosis. In one embodiment preferred according to the invention, in process step a1), the isomalt-containing solution provided in process step a) according to the invention is obtained from a starting solution or suspension of isomalt in water by increasing the temperature of the solution or suspension, in particular at reduced pressure relative to atmospheric pressure.

[0081] In one embodiment preferred according to the invention, in process step a1), the isomalt-containing solution provided according to the invention in process step a) is prepared from a starting solution or suspension of isomalt in water, in particular by reverse osmosis at elevated pressure relative to atmospheric pressure.

[0082] In one embodiment preferred according to the invention, in process step a1), the isomalt-containing solution provided according to the invention in process step a) is prepared by adding crystalline isomalt to water, in particular demineralized water.In one embodiment preferred according to the invention, in process step a1), the isomalt-containing solution provided according to the invention in process step a) is prepared by adding crystalline isomalt to a starting solution or suspension containing less concentrated isomalt.

[0083] In one embodiment preferred according to the invention, in step a1), the isomalt-containing solution provided in step a) is prepared from a starting solution or suspension comprising isomalt by concentrating the starting solution, preferably by evaporation, in particular at reduced pressure relative to atmospheric pressure, by reverse osmosis, in particular at elevated pressure relative to atmospheric pressure, and / or by adding crystalline isomalt, or by diluting the starting solution or suspension, preferably by adding water, thus obtaining the isomalt-containing solution provided in step a).

[0084] In one embodiment preferred according to the invention, the isomalt-containing starting solution or suspension used in process step a1) is obtained by selective hydrogenation, in particular by selective hydrogenation of 1,6-GPS.

[0085] In one embodiment preferred according to the invention, the isomalt-containing starting solution used in process step a1) is obtained by selective hydrogenation, in particular by selective hydrogenation using a hydrogenation catalyst, in particular comprising, in particular consisting of, ruthenium or ruthenium oxide and a catalyst support.

[0086] In one embodiment preferred according to the invention, the isomalt-containing starting solution used in process step a1) is obtained by selective hydrogenation, in particular using a hydrogenation catalyst which comprises, in particular consists of, nickel, Raney nickel or supported nickel.

[0087] In one embodiment preferred according to the invention, the isomalt-containing starting solution obtained in process step a1) has a temperature of 50-95°C, in particular 55-90°C, in particular 60-85°C, in particular 65-80°C, preferably 65-70°C.

[0088] In a particularly preferred embodiment, the isomalt-containing starting solution obtained in process step a1) has a temperature that is at least 10° C., preferably at least 8° C., preferably at least 5° C., or preferably at least 3° C. higher than the isomalt-containing solution provided in process step a). Preferably, the isomalt-containing solution obtained in process step a1) is cooled, preferably to the temperature used in process step a).

[0089] In one embodiment preferred according to the invention, process step a1) is carried out in an evaporator.

[0090] The process according to the invention comprises nucleation by flash evaporation in process step b) after process step a) and before process step c).

[0091] In one embodiment preferred according to the invention, the temperature of the isomalt-containing solution is adjusted after process step a) and before process step b). Preferably according to the invention, before the flash evaporation, i.e. after process step a) and before process step b), the temperature of the isomalt-containing solution fed is adjusted to 50-90°C, preferably 55-80°C, particularly preferably 60-75°C.

[0092] Preferably, the isomalt-containing solution provided in method step a) has a temperature of 50-90°C, preferably 55-80°C, particularly preferably 60-75°C.

[0093] In one embodiment preferred according to the invention, the flash evaporation according to process step b) is carried out continuously.

[0094] In one embodiment preferred according to the invention, the flash evaporation according to process step b) is carried out discontinuously.

[0095] In one embodiment preferred according to the invention, during the flash evaporation according to process step b) after process step a) and before process step c), the absolute pressure is reduced (in each case relative to the initial surrounding absolute atmospheric pressure) by at least 5%, preferably at least 10%, preferably at least 50%, preferably at least 70% or preferably at least 90%.

[0096] Process steps a1), a), c), d) and e) are preferably carried out at elevated pressure relative to process step b).

[0097] Process steps a), c), d) and e) are preferably carried out at elevated pressure relative to process step b).

[0098] Process steps a1), a), d) and e) are preferably carried out at elevated pressure relative to process step b).

[0099] Process steps a), d) and e) are preferably carried out at elevated pressure relative to process step b).

[0100] The process steps a1), a), c), d) and e) are preferably carried out at atmospheric pressure.

[0101] The process steps a), c), d) and e) are preferably carried out at atmospheric pressure.

[0102] The process steps a1), a), d) and e) are preferably carried out at atmospheric pressure.

[0103] The process steps a), d) and e) are preferably carried out at atmospheric pressure.

[0104] In a particularly preferred embodiment, if process step c) is carried out in the form of cooling crystallization or isothermal crystallization, process step c) is carried out under atmospheric pressure. If process step c) is carried out as evaporative crystallization, process step c) is preferably carried out at reduced pressure relative to atmospheric pressure, in particular in vacuum.

[0105] In one embodiment which is particularly preferred according to the invention, during the flash evaporation according to process step b) after process step a) and before process step c), the absolute pressure is preferably reduced to 10 to 500 mbar, preferably 20 to 400 mbar, preferably 30 to 300 mbar, preferably 50 to 200 mbar, preferably 90 to 110 mbar, in particular 90 to 100 mbar.

[0106] In a further preferred embodiment of the present invention, during the flash evaporation according to process step b) after process step a) and before process step c), the absolute pressure is reduced to at most 500 mbar, preferably at most 400 mbar, preferably at most 300 mbar, preferably at most 200 mbar, preferably at most 150 mbar, preferably at most 100 mbar, preferably at most 80 mbar, preferably at most 50 mbar, preferably at most 20 mbar, preferably at most 10 mbar.

[0107] In a further embodiment preferred according to the invention, the flash evaporation according to process step b) after process step a) and before process step c) is carried out at a temperature in the range from 30 to 70°C, preferably from 35 to 65°C, preferably from 30 to 60°C, preferably from 40 to 60°C, preferably from 45 to 55°C, preferably from 50 to 55°C.

[0108] In a further embodiment which is preferred according to the invention, the flash evaporation according to process step b) after process step a) and before process step c) is carried out at a temperature in the range from 30 to 70°C, preferably from 35 to 65°C, preferably from 40 to 60°C, preferably from 30 to 60°C, preferably from 45 to 55°C, preferably from 50 to 55°C and at a reduced absolute pressure, preferably from 10 to 500 mbar, preferably from 20 to 400 mbar, preferably from 30 to 300 mbar, preferably from 50 to 200 mbar, preferably from 90 to 110 mbar, in particular from 90 to 100 mbar and at 50 to 55°C.

[0109] In one embodiment preferred according to the invention, during the flash evaporation according to process step b) after process step a) and before process step c), the isomalt-containing solution provided according to process step a) is subjected to reduced absolute pressure until 10 to 50%, in particular 15 to 40%, in particular 20 to 30% of the amount of dissolved 1,1-GPM contained in the isomalt-containing solution provided according to process step a) is transferred to the first crystalline phase, thus achieving enrichment of 1,1-GPM in the first crystalline phase and enrichment of 1,6-GPS in the first liquid phase.

[0110] Method step b) may be carried out over a period of preferably 2 minutes to 12 hours, preferably 3 minutes to 10 hours, preferably 4 minutes to 9 hours, preferably 1 to 12 hours, preferably 2 to 8 hours, preferably 3 to 7 hours, preferably 4 to 6 hours, preferably 1 to 5 hours, preferably 2 to 5 hours, preferably 3 to 5 hours, preferably 4 to 5 hours, preferably 5 hours.

[0111] In one embodiment preferred according to the invention, process step b) is carried out in such a way that 20-30% of the dissolved 1,1-GPM present in process step a) (based on the total weight of 1,1-GPM dry matter (TS: Trokensubstanz) in the solution provided in process step a)) is transformed into the first crystalline phase during process step b).

[0112] In one embodiment preferred according to the invention, the flash evaporation according to process step b) after process step a) and before process step c) is carried out in such a way that the dry matter content of the isomalt-containing solution provided in process step a) is increased during process step b) by 1 to 10% by weight, preferably by 1 to 8% by weight, preferably by 1 to 6% by weight (based on the total weight of the dry matter (TS) of the isomalt-containing solution provided and of the first isomalt-containing suspension obtained).

[0113] In one embodiment preferred according to the invention, in the first crystalline phase of the first isomalt-containing suspension obtained after flash evaporation according to process step b) there is a 1,1-GPM content of 57 to 100% by weight, preferably 60 to 100% by weight, preferably 62 to 99% by weight, preferably 65 to 99% by weight, preferably 67 to 95% by weight of 1,1-GPM and a 1,6-GPS content of 0 to 43% by weight, preferably 0 to 40% by weight, preferably 1 to 38% by weight, preferably 1 to 35% by weight, preferably 5 to 33% by weight of 1,6-GPS (each relative to the total weight of the dry matter of the first crystalline phase of the suspension obtained after process step b).

[0114] In one embodiment preferred according to the invention, in the first liquid phase of the first isomalt-containing suspension obtained after flash evaporation according to process step b) there is a 1,1-GPM content of 25 to 35% by weight, preferably 28 to 34% by weight, preferably 29 to 33% by weight, preferably 30 to 32% by weight, preferably 31% by weight of 1,1-GPM and a 1,6-GPS content of 65 to 75% by weight, preferably 66 to 72% by weight, preferably 67 to 71% by weight, preferably 68 to 70% by weight, preferably 68% by weight of 1,6-GPS (respectively relative to the total weight of dry matter remaining in the first liquid phase after process step b).

[0115] In one embodiment preferred according to the invention, in the first liquid phase of the first isomalt-containing suspension obtained after flash evaporation according to process step b) there is a dry matter content of 56 to 80% by weight, preferably 69 to 74% by weight, preferably 70 to 73% by weight, preferably 71 to 72% by weight (based on the total weight of the first suspension present after process step b).

[0116] In one embodiment preferred according to the invention, no seeding is carried out during process step b), in particular with isomalt, 1,1-GPM and / or 1,6-GPS.

[0117] In one embodiment preferred according to the invention, the crystallization process according to method step c) is carried out in a crystallizer.

[0118] The first isomalt-containing suspension is preferably exposed in process step c) to conditions that do not allow complete dissolution of isomalt in the first liquid phase used, so that a further crystallization of isomalt, preferably 1,1-GPM, takes place, in particular the first crystalline phase is further enriched with 1,1-GPM and the first liquid phase is further enriched with 1,6-GPS, to obtain a second suspension comprising a second crystalline phase, preferably enriched with 1,1-GPM, and a second liquid phase, preferably enriched with 1,6-GPS. In a preferred embodiment, 1,6-GPS and 1,1-GPM are present in this case partially dissolved and partially undissolved.

[0119] In one embodiment preferred according to the invention, the crystallization according to process step c) can be carried out continuously.

[0120] In one embodiment preferred according to the invention, the crystallization according to process step c) can be carried out discontinuously.

[0121] In one embodiment preferred according to the invention, the crystallization in process step c) is an isothermal crystallization, a cooling crystallization and / or an evaporative crystallization, in particular a multi-stage evaporative crystallization.

[0122] In one embodiment preferred according to the invention, the first isomalt-containing suspension obtained from process step b) is subjected to crystallization, preferably isothermal crystallization, in process step c).Preferably according to the invention, when using isothermal crystallization, the temperature of the first isomalt-containing suspension is adjusted to 50-60°C, preferably 52-60°C, preferably 54-60°C, preferably 51-59°C, preferably 52-59°C, preferably 53-59°C, preferably 54-59°C, preferably 52-58°C, preferably 53-57°C, preferably 53-58°C, preferably 54-58°C, preferably 54-57°C, preferably 54-57°C, or preferably 54°C-56°C.

[0123] In one embodiment preferred according to the invention, the temperature of the isothermal crystallization in method step c) is 50-60° C., preferably 51-60° C., preferably 52-60° C., preferably 53-59° C., preferably 50-59° C., preferably 51-59° C., preferably 52-58° C., preferably 53-58° C., preferably 54-60° C., preferably 54-58° C., preferably 54-56° C., preferably 53-57° C., preferably 53-56° C., or preferably 54-56° C. In one embodiment particularly preferred according to the invention, the isothermal crystallization carried out in step c) is carried out at a temperature adjusted in step c), and the crystallization energy released is continuously dissipated.

[0124] In one embodiment preferred according to the invention, the isothermal crystallization of the isomalt-containing suspension in process step c) is carried out over a period of 10 to 100 h, preferably 20 to 100 h, preferably 20 to 80 h, preferably 20 to 60 h, preferably 20 to 52 h, preferably 20 to 40 h, preferably 30 to 80 h, preferably 30 to 70 h, preferably 30 to 60 h, preferably 30 to 50 h or preferably 30 to 40 h.

[0125] In an advantageous manner, carrying out the process step c) by isothermal crystallization results in a uniform crystal size distribution, because, without being bound by theory, the continuous reduction in supersaturation with the progression of the crystallization process minimizes the risk of fines formation at a later point in the process. This mode of operation also leads to an extension of the service life of the reactor used for crystallization, because reduced sediment formation and / or reduced fouling can be observed compared to other crystallizations, in particular cooling crystallizations using cooling lamps. Without being bound by theory, the reduced sediment formation and / or fouling is due only to the small temperature difference between the cooling element used and the isomalt-containing suspension (magma) used.

[0126] In one embodiment preferred according to the invention, the first isomalt-containing suspension obtained from process step b) is subjected to crystallization, preferably cooling crystallization, in process step c).Preferably according to the invention, when cooling crystallization is used, the temperature of the cooling crystallization in process step c) is gradually lowered, preferably by at most 2 K / hour (h), preferably by at most 1 K / h, preferably by at most 0.8 K / h, preferably by at most 0.6 K / h, preferably by at most 0.4 K / h, preferably by at most 0.2 K / h, particularly preferably by at most 0.1 K / h, which additionally increases the yield of crystals enriched with 1,1-GPM.Preferably, the cooling rate of 0.8-1.5 K / h preferably starts at a temperature of 65°C and ends at 37°C.

[0127] In one embodiment preferred according to the invention, the cooling crystallization of the isomalt-containing suspension in process step c) is carried out over a period of 10 to 100 hours, preferably 20 to 100 hours, preferably 20 to 80 hours, preferably 20 to 60 hours, preferably 20 to 52 hours, preferably 20 to 40 hours, preferably 30 to 80 hours, preferably 30 to 70 hours, preferably 30 to 60 hours, preferably 30 to 50 hours or preferably 30 to 40 hours.

[0128] In one embodiment preferred according to the invention, crystallization, in particular evaporative crystallization, in particular multi-stage evaporative crystallization, is brought about in process step c) by increasing the concentration of the first isomalt-containing suspension obtained from process step b), in particular the concentration of isomalt in the liquid phase of the first isomalt-containing suspension is increased, in particular by means of a multiple-effect evaporator.

[0129] In one embodiment preferred according to the invention the multiple effect evaporator has at least 2 reactors, preferably at least 3 reactors, preferably at least 4 reactors, preferably at least 5 reactors, preferably at least 6 reactors, preferably at least 7 reactors, preferably up to 3 reactors, preferably up to 4 reactors, preferably up to 5 reactors, preferably up to 6 reactors, preferably up to 7 reactors.

[0130] In one embodiment preferred according to the invention, at least one solvent, preferably one solvent, preferably several solvents, particularly preferably water and at least one alcohol, are completely or partially removed by a multiple effect evaporator. The concentration of isomalt in the liquid phase of the second isomalt-containing suspension in process step c) is preferably adjusted according to the invention such that the amount of solvent is not sufficient to dissolve the entire amount of isomalt at a given temperature.

[0131] In one embodiment preferred according to the invention the pressure in the multiple effect evaporator in process step c) is between 0.01 and 2 bar, preferably between 0.01 and 1 bar, preferably between 0.01 and 0.5 bar, preferably between 0.1 and 1 bar, preferably between 0.1 and 0.5 bar.

[0132] In one embodiment preferred according to the invention, the evaporative crystallization in each reactor of the multiple-effect evaporator, in each, ie per reactor, process step c), is an isothermal crystallization.

[0133] In one embodiment preferred according to the invention, the pressure in a subsequent reactor in the multiple effect evaporator in process step c) is reduced by at least 5%, preferably by at least 10%, preferably by at least 12%, preferably by at least 15% or preferably by at least 20% compared to the preceding reactor.

[0134] In one embodiment preferred according to the invention, the temperature in a subsequent reactor in the multiple effect evaporator in process step c) is reduced by at least 5%, preferably by at least 10%, preferably by at least 12%, preferably by at least 15% or preferably by at least 20% compared to the preceding reactor.

[0135] The quantitative ratio of 1,1-GPM and 1,6-GPS in the second crystalline phase enriched in 1,1-GPM and in the second liquid phase enriched in 1,6-GPS can be adjusted by the temperature and / or pressure, in particular the temperature profile and / or pressure profile, in the individual reactors of the multiple-effect evaporator.

[0136] In one embodiment preferred according to the invention, the evaporative crystallization of the isomalt-containing suspension in process step c) is carried out, in particular by means of a multiple-effect evaporator, for a period of between 1 minute and 14 hours.

[0137] In one embodiment preferred according to the invention, no seeding is carried out during the crystallization in process step c), in particular with isomalt, 1,1-GPM and / or 1,6-GPS.

[0138] In one embodiment preferred according to the invention, no seeding with seeds, in particular with isomalt, 1,1-GPM and / or 1,6-GPS, is carried out during the process, in particular during the isothermal crystallization preferred according to the invention in process step c).

[0139] In one embodiment preferred according to the invention, no seeding is carried out during process steps b) and c), in particular with isomalt, 1,1-GPM and / or 1,6-GPS.

[0140] In a further embodiment preferred according to the invention, in process step c) crystalline isomalt, 1,1-GPM or 1,6-GPS are added as seeds in pure or almost pure form. After introducing the seeds into the isomalt-containing solution, the more soluble 1,6-GPS crystals dissolve, whereas the less soluble 1,1-GPM crystals remain as crystallization nuclei.

[0141] In one embodiment preferred according to the invention, the second crystalline phase enriched with 1,1-GPM in process step c) comprises a mixture of 1,1-GPM and 1,6-GPS having (respectively relative to the total weight of the dry matter (TS) of the second crystalline phase) 57 to 99% by weight of 1,1-GPM and 43 to 1% by weight of 1,6-GPS, preferably 60 to 80% by weight of 1,1-GPM and 20 to 40% by weight of 1,6-GPS, preferably 60 to 75% by weight of 1,1-GPM and 25 to 40% by weight of 1,6-GPS, preferably 65 to 75% by weight of 1,1-GPM and 25 to 35% by weight of 1,6-GPS.

[0142] In one embodiment preferred according to the invention, the second liquid phase enriched with 1,6-GPS in process step c) comprises a mixture of 1,1-GPM and 1,6-GPS having 43 to 1% by weight of 1,1-GPM and 57 to 99% by weight of 1,6-GPS, preferably 20 to 25% by weight of 1,1-GPM and 80 to 75% by weight of 1,6-GPS (respectively relative to the total weight of dry matter (TS) of the second liquid phase).

[0143] In one embodiment preferred according to the invention, the second crystalline phase separated in process step d) comprises at least 60% by weight, preferably at least 67% by weight, preferably at least 75% by weight, preferably at least 80% by weight, preferably at least 85% by weight, preferably at least 90% by weight, or preferably at least 95% by weight of 1,1-GPM (each based on the total weight (TS) of the second crystalline phase).

[0144] In a particularly preferred embodiment, the second crystalline phase separated in process step d) comprises at least 99% by weight, in particular 100% by weight, of 1,1-GPM (based on the total weight (TS) of the second crystalline phase).

[0145] In one embodiment preferred according to the invention, the second crystalline phase separated in process step d) comprises at most 40 wt.-%, preferably at most 32 wt.-%, preferably at most 25 wt.-%, preferably at most 20 wt.-%, preferably at most 15 wt.-%, preferably at most 10 wt.-%, or preferably at most 5 wt.-% of 1,6-GPS (each relative to the total weight (TS) of the second crystalline phase).

[0146] In a particularly preferred embodiment, the second crystalline phase separated in process step d) comprises at most 1 wt.-%, in particular 0 wt.-%, of 1,6-GPS (based on the total weight (TS) of the second crystalline phase).

[0147] In one embodiment which is particularly preferred according to the invention, the crystalline phase which is separated in process step d) is free or almost free of 1,6-GPS.

[0148] In one embodiment preferred according to the invention, the second crystalline phase separated in process step d) comprises (each relative to the total weight of the second crystalline phase) 60 to 75% by weight of 1,1-GPM, in particular 60 to 72% by weight of 1,1-GPM, preferably 65 to 71% by weight, preferably 66 to 70% by weight, 67 to 69% by weight, preferably 68% by weight of 1,1-GPM and (each relative to the total weight (TS) of the second crystalline phase) 25 to 40% by weight, in particular 28 to 40% by weight of 1,6-GPS, preferably 29 to 35% by weight, preferably 30 to 34% by weight, 31 to 33% by weight, preferably 32% by weight of 1,6-GPS.

[0149] In one embodiment preferred according to the invention, the second crystalline phase separated in process step d) comprises 60 to 75% by weight of 1,1-GPM, in particular 65 to 71% by weight of 1,1-GPM (respectively relative to the total weight of the second crystalline phase) and 25 to 40% by weight, in particular 29 to 35% by weight of 1,6-GPS (respectively relative to the total weight (TS) of the second crystalline phase).

[0150] In one embodiment preferred according to the invention, the second crystalline phase separated in process step d) has a length to width ratio of the crystals contained therein of 7.0 to 10.5, in particular 7.5 to 10.0, in particular 7.5 to 9.0, in particular 7.5 to 8.5, in particular 8.0 (respectively average values).

[0151] In one embodiment preferred according to the invention, the second crystalline phase separated in process step d) has a length to width ratio of the crystals contained therein of 6.5 to 10.0, in particular 7.0 to 9.5, in particular 7.5 to 9.0, in particular 7.5 to 8.5, in particular 7.8 (respective median values).

[0152] In one embodiment preferred according to the invention, the second liquid phase separated in process step d) comprises 15-32 wt.-%, preferably 17-30 wt.-%, preferably 19-28 wt.-%, 20-26 wt.-%, preferably 21-24 wt.-% of 1,1-GPM (each based on the total weight of the dry matter (TS) of the second liquid phase).

[0153] In one embodiment preferred according to the invention, the second liquid phase separated in process step d) comprises at least 72 wt.-%, preferably at least 75 wt.-%, preferably at least 80 wt.-%, preferably at least 85 wt.-%, or preferably at least 90 wt.-% of 1,6-GPS (each based on the total weight of the dry matter (TS) of the second liquid phase).

[0154] In one embodiment preferred according to the invention, the second liquid phase separated in process step d) comprises 68 to 85% by weight, preferably 70 to 83% by weight, preferably 72 to 81% by weight, 74 to 80% by weight, preferably 76 to 79% by weight of 1,6-GPS (each based on the total weight of the dry matter (TS) of the second liquid phase).

[0155] In one embodiment preferred according to the invention, the second liquid phase separated in process step d) comprises (respectively relative to the total weight of the dry matter (TS) of the second liquid phase) 15 to 32% by weight of 1,1-GPM, preferably 17 to 30% by weight, preferably 19 to 28% by weight, preferably 20 to 26% by weight, preferably 21 to 24% by weight of 1,1-GPM and (respectively relative to the total weight of the dry matter (TS) of the second liquid phase) 68 to 85% by weight of 1,6-GPS, preferably 70 to 83% by weight, preferably 72 to 81% by weight, preferably 74 to 80% by weight, preferably 76 to 79% by weight of 1,6-GPS.

[0156] In one embodiment preferred according to the invention, the second liquid phase separated in process step d) comprises 15 to 32 wt.-% of 1,1-GPM (based on the total weight of the dry matter (TS) of the second liquid phase) and 68 to 85 wt.-% of 1,6-GPS (based on the total weight of the dry matter (TS) of the second liquid phase).

[0157] In one embodiment preferred according to the invention, the separated second crystalline phase enriched with 1,1-GPM contains at most 20% by weight of water, preferably at most 18% by weight of water, preferably at most 15% by weight of water, preferably at most 13% by weight of water, preferably between 5 and 20% by weight of water, preferably between 8 and 18% by weight of water, preferably between 10 and 15% by weight of water or preferably between 11 and 13% by weight of water (each based on the total weight of the second crystalline phase enriched with 1,1-GPM).

[0158] In one embodiment preferred according to the invention, the second crystalline phase enriched in 1,1-GPM is separated in process step d) from the second liquid phase enriched in 1,6-GPS by decantation, filtration, sedimentation or centrifugation, particularly preferably by centrifugation. The separation contemplated according to the invention, in particular the centrifugation, results in a separation of the second liquid phase and the second crystalline phase, the second crystalline phase being enriched in 1,1-GPM, whereas the second liquid phase is enriched in 1,6-GPS.

[0159] The separated second crystalline phase enriched in 1,1-GPM can be further processed in further purification and concentration steps to a 1,1-GPM enriched composition, in particular crystalline 1,1-GPM having a purity of at least 95% by weight, preferably at least 96% by weight, preferably at least 97% by weight, preferably at least 98% by weight, or preferably at least 99% by weight (weight of 1,1-GPM relative to the total weight (TS) of the composition, respectively).

[0160] In one embodiment preferred according to the invention, the second crystalline phase enriched with 1,1-GPM is dried after process step d) and obtained in process step e) as a solid 1,1-GPM enriched isomalt composition.

[0161] In one embodiment preferred according to the invention, the second liquid phase enriched with 1,6-GPS is concentrated after process step d) at least once, preferably at least twice or preferably at least three times to obtain in process step e) a liquid 1,6-GPS-enriched isomalt composition.

[0162] In one embodiment preferred according to the invention, the second liquid phase enriched with 1,6-GPS is concentrated after process step d) to a dry matter content of at least 60% by weight, preferably at least 65% by weight, preferably at least 70% by weight, preferably at least 75% by weight, preferably at least 80% by weight, preferably at least 85% by weight, preferably at least 90% by weight or preferably at least 95% by weight (each relative to the total weight of the composition) to be obtained in process step e) as a liquid 1,6-GPS-enriched isomalt composition.

[0163] In a further embodiment preferred according to the invention, the second liquid phase enriched with 1,6-GPS is further processed in further purification and concentration steps to give a 1,6-GPS-enriched isomalt composition, in particular crystalline 1,6-GPS having a dry matter content of at least 95 wt.-%, preferably at least 96 wt.-%, preferably at least 97 wt.-%, preferably at least 98 wt.-% or preferably at least 99 wt.-% (each based on the total weight of dry matter (TS) of the isomalt composition).

[0164] In one embodiment preferred according to the invention, the 1,6-GPS-enriched isomalt composition is obtained from the 1,6-GPS-enriched second liquid phase by concentrating the 1,6-GPS-enriched second liquid phase followed by cooling crystallization, preferably the cooling crystallization is carried out in a temperature range of 40-60° C., preferably 50-60° C., preferably 40-50° C., or preferably 45-55° C., and at a cooling rate of preferably 0.1-0.3 K / h, preferably 0.2-0.3 K / h, or preferably 0.1-0.2 K / h. The concentration and cooling crystallization are optionally repeated under the same conditions until the desired amount of crystals is obtained.

[0165] In one embodiment preferred according to the invention, the second liquid phase enriched with 1,6-GPS after process step d) is dried and obtained in process step e) as a solid 1,6-GPS-enriched isomalt composition.

[0166] In one embodiment preferred according to the invention, the second liquid phase enriched with 1,6-GPS is dried after process step d) and obtained in process step e) as a solid 1,6-GPS-enriched isomalt composition, in particular as a crystalline product.

[0167] In one embodiment preferred according to the invention, the dried 1,6-GPS-enriched composition contains preferably 0.05 to 6 wt.% water, preferably 2.0 to 3.0 wt.% water, preferably 0.05 to 2.5 wt.% water, preferably 0.05 to 1 wt.% water, preferably 0.1 to 0.5 wt.% water, preferably up to 6.0 wt.% water, preferably up to 4.0 wt.% water, preferably up to 2.5 wt.%, preferably up to 2.0 wt.% water, preferably up to 1.0 wt.% water, or preferably up to 0.5 wt.% water (each based on the total weight of the 1,6-GPS-enriched crystalline composition).

[0168] In a further aspect, the present invention provides a 1,1-GPM and / or 1,6-GPS enriched isomalt composition producible, in particular produced, by the process according to the present invention.

[0169] In one embodiment preferred according to the invention, the 1,1-GPM enriched isomalt composition comprises 60-72% by weight, preferably 65-71% by weight, preferably 66-70% by weight, preferably 67-69% by weight, preferably 67 or 68% by weight of 1,1-GPM (each based on the total weight of the dry matter (TS) of the 1,1-GPM enriched composition).

[0170] In a further preferred embodiment of the invention, the 1,6-GPS-enriched isomalt composition of the invention comprises (each based on the total weight of dry matter (TS) of the 1,6-GPS-enriched composition) 15-32% by weight of 1,1-GPM, preferably 17-30% by weight, preferably 19-28% by weight, preferably 20-26% by weight, preferably 21-14% by weight of 1,1-GPM, and 68-85% by weight, in particular 70-83% by weight, in particular 72-81% by weight, in particular 74-80% by weight, in particular 76-79% by weight of 1,6-GPS.

[0171] In a preferred embodiment, the present invention relates in particular to an isomalt composition enriched with 1,1-GPM containing 60 to 75% by weight of 1,1-GPM and 25 to 40% by weight of 1,6-GPS (each relative to the total weight of dry matter (TS) of the composition), which can be produced by the process according to the invention.

[0172] The present invention relates in a preferred embodiment to a 1,1-GPM-enriched isomalt composition comprising 60-75% by weight of 1,1-GPM and 25-40% by weight of 1,6-GPS (relative to the total dry matter weight of 1,1-GPM and 1,6-GPS, respectively), in particular producible by the process according to the invention, and in particular having a 1,1-GPM content of at least 60% by weight (relative to the total dry matter weight of the composition (TS)).

[0173] In a preferred embodiment, the present invention relates in particular to a 1,6-GPS-enriched isomalt composition comprising 15 to 32% by weight of 1,1-GPM and 68 to 85% by weight of 1,6-GPS (each relative to the total weight of dry matter (TS) of the composition), which can be produced by the process according to the invention.

[0174] The present invention relates in a preferred embodiment to a 1,6-GPS-enriched isomalt composition comprising 15-32% by weight of 1,1-GPM and 68-85% by weight of 1,6-GPS (relative to the total dry matter amount of 1,1-GPM and 1,6-GPS, respectively), especially capable of being produced by the process according to the invention, and in particular having a 1,6-GPS content of at least 68% by weight (relative to the total weight of dry matter (TS) of the composition).

[0175] In one embodiment preferred according to the invention, the isomalt composition enriched with 1,1-GPM obtained in process step e) comprises at least 61% by weight, preferably at least 75% by weight, preferably at least 80% by weight, preferably at least 85% by weight, preferably at least 90% by weight, preferably at least 94% by weight, preferably at least 95% by weight, preferably at least 96% by weight, preferably at least 99% by weight, preferably 75-95% by weight, preferably 75-90% by weight, preferably 75-85% by weight or preferably 80-99% by weight of 1,1-GPM (each based on the total weight of the dry matter (TS) of the 1,1-GPM-enriched isomalt composition).

[0176] In one embodiment preferred according to the invention, the isomalt composition enriched with 1,6-GPS obtained in process step e) comprises at least 72% by weight, preferably at least 75% by weight, preferably at least 80% by weight, preferably at least 85% by weight, preferably at least 90% by weight, preferably at least 95% by weight, preferably at least 99% by weight, preferably 72-95% by weight, preferably 72-90% by weight, preferably 72-85% by weight or preferably 80-99% by weight of 1,6-GPS (each based on the total weight of the dry matter (TS) of the 1,6-GPS-enriched isomalt composition).

[0177] In one embodiment preferred according to the invention, the 1,1-GPM and / or 1,6-GPS enriched isomalt composition is present in crystalline form.

[0178] In one embodiment preferred according to the invention, the 1,1-GPM enriched isomalt composition according to the invention, which is preferably one or more of the preferred 1,1-GPM enriched isomalt compositions according to the invention characterized above, has a length to width ratio of the crystals contained therein of 7.0 to 10.5, in particular 7.5 to 10.0, in particular 7.5 to 9.0, in particular 7.5 to 8.5, in particular 8.0 (respectively average values).

[0179] In one embodiment preferred according to the invention, the 1,1-GPM enriched isomalt composition according to the invention, which is preferably one or more of the preferred 1,1-GPM enriched isomalt compositions according to the invention characterized above, has a length to width ratio of the crystals contained therein of 6.5 to 10.0, in particular 7.0 to 9.5, in particular 7.5 to 9.0, in particular 7.5 to 8.5, in particular 7.8 (respectively median values).

[0180] In a further preferred embodiment, the 1,1-GPM and / or 1,6-GPS enriched isomalt composition is present in semi-crystalline or amorphous form.

[0181] In one embodiment preferred according to the invention, the 1,1-GPM and / or 1,6-GPS enriched isomalt composition according to the invention comprises, besides the components 1,1-GPM and 1,6-GPS, at least one further component selected from the group consisting of mannitol, sorbitol, saccharose, 1,1-GPS (1-O-α-D-glucopyranosyl-D-sorbitol), glycosyl glycitols, deoxydisaccharide alcohols, GPI (glucopyranosyl iditol), isomaltose, isomaltulose and isomerezitose.

[0182] In one embodiment preferred according to the invention, the 1,1-GPM and / or 1,6-GPS enriched isomalt composition according to the invention comprises (relative to the total weight (TS) of the 1,1-GPM and / or 1,6-GPS enriched isomalt composition, respectively) 0.01-0.3 wt.-%, preferably 0.01-0.2 wt.-%, preferably 0.01-0.1 wt.-%, preferably 0.01-0.06 wt.-%, 0.02-0.3 wt.-%, preferably 0.02-0.2 wt.-%, preferably 0.02-0.1 wt.-% or preferably 0.02-0.06 wt.-% mannitol, preferably at most 0.3 wt.-%, preferably at most 0.2 wt.-%, preferably at most 0.1 wt.-% or preferably at most 0.06 wt.-% mannitol.

[0183] In one embodiment preferred according to the invention, the 1,1-GPM and / or 1,6-GPS enriched isomalt composition according to the invention does not contain mannitol.

[0184] In one embodiment preferred according to the invention, the 1,1-GPM and / or 1,6-GPS enriched isomalt composition according to the invention comprises (relative to the total weight (TS) of the 1,1-GPM and / or 1,6-GPS enriched isomalt composition, respectively) 0.01 to 0.4 wt.-%, preferably 0.01 to 0.2 wt.-%, preferably 0.01 to 0.1 wt.-%, preferably 0.01 to 0.04 wt.-%, preferably 0.02 to 0.4 wt.-%, preferably 0.02 to 0.02 wt.-%, preferably 0.02 to 0.1 wt.-%, or preferably 0.02 to 0.04 wt.-%, preferably at most 0.4 wt.-%, preferably at most 0.2 wt.-%, preferably at most 0.1 wt.-%, or preferably at most 0.04 wt.-% sorbitol.

[0185] In one embodiment preferred according to the invention, the 1,1-GPM and / or 1,6-GPS enriched isomalt composition according to the invention does not contain sorbitol.

[0186] In one embodiment preferred according to the invention, the 1,1-GPM and / or 1,6-GPS enriched isomalt composition according to the invention comprises (relative to the total weight (TS) of the 1,1-GPM and / or 1,6-GPS enriched isomalt composition, respectively) 0.01 to 2 wt.-%, preferably 0.01 to 1 wt.-%, preferably 0.01 to 0.6 wt.-%, preferably 0.01 to 0.4 wt.-% or preferably 0.01 to 0.1 wt.-% sucrose, preferably at most 2 wt.-%, preferably at most 1 wt.-%, preferably at most 0.6 wt.-%, preferably at most 0.4 wt.-% or preferably at most 0.1 wt.-% sucrose.

[0187] In one embodiment preferred according to the invention, the 1,1-GPM and / or 1,6-GPS enriched isomalt composition according to the invention does not contain sucrose.

[0188] In a preferred embodiment, the 1,1-GPM and / or 1,6-GPS enriched isomalt composition according to the invention is (relative to the total weight (TS) of the 1,1-GPM and / or 1,6-GPS enriched isomalt composition, respectively) 0.1 to 10% by weight, preferably 0.1 to 8% by weight, preferably 0.1 to 6% by weight, preferably 0.1 to 4% by weight, preferably 0.1 to 2% by weight, preferably 0.1 to 1% by weight, preferably 0.1 to 0.6% by weight, preferably 0.1 to 0.4% by weight, preferably 0.1 to 0.2% by weight, preferably 0.2 to 10% by weight, preferably 0.2 % or less, preferably 0.2-6% by weight, preferably 0.2-4% by weight, preferably 0.2-2% by weight, preferably 0.2-1% by weight, preferably 0.2-0.6% by weight, or preferably 0.2-0.4% by weight of 1,1-GPS, preferably at most 10% by weight, preferably at most 8% by weight, preferably at most 6% by weight, preferably at most 4% by weight, preferably at most 2% by weight, preferably at most 1% by weight, preferably at most 0.6% by weight, preferably at most 0.4% by weight, or preferably at most 0.2% by weight of 1,1-GPS.

[0189] In one embodiment which is particularly preferred according to the invention, the 1,1-GPM and / or 1,6-GPS enriched isomalt composition according to the invention does not contain 1,1-GPS.

[0190] In one embodiment preferred according to the invention, the 1,1-GPM and / or 1,6-GPS enriched isomalt composition according to the invention comprises (relative to the total weight (TS) of the 1,1-GPM and / or 1,6-GPS enriched isomalt composition, respectively) 0.01 to 2 wt.-%, preferably 0.01 to 1 wt.-%, preferably 0.01 to 0.6 wt.-%, preferably 0.01 to 0.4 wt.-%, preferably 0.01 to 0.1 wt.-%, preferably 0.03 to 2 wt.-%, preferably 0.03 to 1 wt.-%, preferably 0.03 to 0.6 wt.-%, preferably 0.03 to 0.4 wt.-%, preferably 0.03 to 0.1 wt.-%, or preferably 0.03 to 0.1 wt.-%, of glycosyl glycitol, preferably at most 2 wt.-%, preferably at most 0.6 wt.-%, preferably at most 0.4 wt.-%, or preferably at most 0.1 wt.-% of glycosyl glycitol.

[0191] In one embodiment preferred according to the invention, the 1,1-GPM and / or 1,6-GPS enriched isomalt composition according to the invention does not contain glycosyl glycitols.

[0192] In a preferred embodiment, the 1,1-GPM and / or 1,6-GPS enriched isomalt composition according to the invention comprises (relative to the total weight (TS) of the 1,1-GPM and / or 1,6-GPS enriched isomalt composition, respectively) 0.01 to 2 wt.-%, preferably 0.01 to 1 wt.-%, preferably 0.01 to 0.6 wt.-%, preferably 0.01 to 0.2 wt.-%, preferably 0.01 to 0.1 wt.-%, preferably 0.03 to 2 wt.-%, preferably 0.03 to 1 wt.-%, preferably 0.03 to 0.6 wt.-%, preferably 0.03 to 0.2 wt.-%, or preferably 0.03 to 0.1 wt.-%, preferably at most 2 wt.-%, preferably at most 1 wt.-%, preferably at most 0.6 wt.-%, preferably at most 0.2 wt.-%, or preferably at most 0.1 wt.-% deoxydisaccharide alcohol.

[0193] In a particularly preferred embodiment according to the invention, the 1,1-GPM and / or 1,6-GPS enriched isomalt composition according to the invention does not contain deoxydisaccharide alcohols. In a particularly preferred embodiment according to the invention, the 1,1-GPM and / or 1,6-GPS enriched isomalt composition according to the invention comprises (relative to the total weight (TS) of the 1,1-GPM and / or 1,6-GPS enriched isomalt composition, respectively) 0.01 to 2% by weight, preferably 0.01 to 1% by weight, preferably 0.01 to 0.6% by weight, preferably 0.01 to 0.4% by weight or preferably 0.01 to 0.1% by weight of GPI, preferably at most 2% by weight, preferably at most 1% by weight, preferably at most 0.6% by weight, preferably at most 0.4% by weight or preferably at most 0.1% by weight of GPI.

[0194] In one embodiment preferred according to the invention, the 1,1-GPM and / or 1,6-GPS enriched isomalt composition according to the invention does not contain GPI.

[0195] In one embodiment preferred according to the invention, the 1,1-GPM and / or 1,6-GPS enriched isomalt composition according to the invention comprises (relative to the total weight (TS) of the 1,1-GPM and / or 1,6-GPS enriched isomalt composition, respectively) 0.01 to 2 wt.-%, preferably 0.01 to 1 wt.-%, preferably 0.01 to 0.6 wt.-%, preferably 0.01 to 0.4 wt.-% or preferably 0.01 to 0.1 wt.-% isomaltose, preferably at most 2 wt.-%, preferably at most 1 wt.-%, preferably at most 0.6 wt.-%, preferably at most 0.4 wt.-% or preferably at most 0.1 wt.-% GPI.

[0196] In one embodiment preferred according to the invention, the 1,1-GPM and / or 1,6-GPS enriched isomalt composition according to the invention does not contain isomaltose.

[0197] In one embodiment preferred according to the invention, the 1,1-GPM and / or 1,6-GPS enriched isomalt composition according to the invention comprises (relative to the total weight (TS) of the 1,1-GPM and / or 1,6-GPS enriched isomalt composition, respectively) 0.01 to 2 wt.-%, preferably 0.01 to 1 wt.-%, preferably 0.01 to 0.6 wt.-%, preferably 0.01 to 0.4 wt.-% or preferably 0.01 to 0.1 wt.-% isomerezitose, preferably at most 2 wt.-%, preferably at most 1 wt.-%, preferably at most 0.6 wt.-%, preferably at most 0.4 wt.-% or preferably at most 0.1 wt.-% GPI.

[0198] In one embodiment preferred according to the invention, the 1,1-GPM and / or 1,6-GPS enriched isomalt composition according to the invention does not contain isomerezitose.

[0199] In one embodiment preferred according to the invention, the 1,1-GPM and / or 1,6-GPS enriched isomalt composition according to the invention has a particle size distribution in which at least 90% of the particles have a particle size, especially a diameter, of 100-1000 μm, preferably 100-800 μm, preferably 100-200 μm, preferably 100-500 μm, preferably 200-800 μm, preferably 300-600 μm, preferably 20-80 μm, preferably 40-80 μm or preferably 50-100 μm.

[0200] In one embodiment preferred according to the invention, the 1,1-GPM and / or 1,6-GPS enriched isomalt composition according to the invention has a particle size distribution in which at least 90% of the particles have a particle size, in particular a diameter, of at most 1000 μm, preferably at most 800 μm, preferably at most 600 μm, preferably at most 500 μm, preferably at most 400 μm, preferably at most 200 μm, preferably at most 100 μm, preferably at most 80 μm, preferably at most 40 μm, preferably at most 20 μm.

[0201] In a further aspect, the present invention also provides the use of a 1,1-GPM and / or 1,6-GPS enriched isomalt composition produced by a method according to the invention in a product for human and / or animal consumption. Preferably, the product for human or animal consumption is a food or luxury item or a medicine.

[0202] In one embodiment preferred according to the invention, the food or luxury item is a confectionery, a confectionery filling, soft caramel, hard caramel, fondant, yoghurt, a pastry, chewing gum, ice cream, milk, a dairy product, a beverage, a fruit juice, a fruit juice concentrate, a fruit preparation, a jam, a jelly or a smoothie.

[0203] In the context of the present invention, the term "isomalt" or "hydrogenated isomaltulose" preferably means a mixture consisting of or containing 1,1-GPM and 1,6-GPS, in particular a mixture consisting of or containing 35-61% by weight of 1,1-GPM and 65-39% by weight of 1,6-GPS, in particular an equimolar or nearly equimolar mixture consisting of or containing 1,1-GPM and 1,6-GPS. Isomalt can therefore also be interpreted as a mixture consisting of or containing 1,1-GPM and 1,6-GPS which does not have an equimolar ratio of 1,1-GPM to 1,6-GPS, but in which there is a higher 1,1-GPM content than the 1,6-GPS content or a higher 1,6-GPS content than the 1,1-GPM content.

[0204] In a particularly preferred embodiment, isomalt contains no further components besides both the components 1,1-GPM and 1,6-GPS.

[0205] In a particularly preferred embodiment, isomalt contains both the components 1,1-GPM and 1,6-GPS in addition to one or more further components, such as mannitol, sorbitol, saccharose, 1,1-GPS (1-O-α-D-glucopyranosyl-D-sorbitol), glycosyl glycitols, deoxydisaccharide alcohols, GPI (glucopyranosyl iditol), isomaltose, isomaltulose, isomerezitose, hydrogenated or non-hydrogenated oligosaccharides, especially hydrogenated or non-hydrogenated trisaccharides, or / and other substances.

[0206] In the context of the present invention, a 1,1-GPM and / or 1,6-GPS enriched isomalt composition obtainable according to the invention preferably means a 1,1-GPM and / or 1,6-GPS enriched isomalt, i.e. a composition in which there is a higher 1,1-GPM content than the 1,6-GPS content in the case of a 1,1-GPM enriched isomalt composition, and in which there is a higher 1,6-GPS content than the 1,1-GPM content in the case of a 1,6-GPS enriched isomalt composition.

[0207] In the context of the present invention, a 1,1-GPM-enriched phase obtainable according to the invention or a 1,1-GPM-enriched isomalt composition obtainable according to the present invention means in particular a phase or mixture in which (relative to the total weight of dry matter of the amounts of 1,6-GPS and 1,1-GPM present in the phase or composition, respectively) there is at least 57% by weight of 1,1-GPM, preferably at least 60, particularly at least 70, particularly at least 80, particularly at least 90, particularly at least 95, particularly at least 98, particularly at least 99% by weight of 1,1-GPM and at most 43% by weight of 1,6-GPS, particularly at most 40, particularly at most 30, particularly at most 20, particularly at most 10, particularly at most 5, particularly at most 2, particularly at most 1% by weight of 1,6-GPS.

[0208] In the context of the present invention, a 1,6-GPS-enriched phase obtainable according to the invention or a 1,6-GPS-enriched isomalt composition obtainable according to the present invention means a phase or mixture in which at least 57% by weight of 1,6-GPS, preferably at least 60, particularly at least 70, particularly at least 80, particularly at least 90, particularly at least 95, particularly at least 98, particularly at least 99% by weight of 1,6-GPS and at most 43% by weight of 1,1-GPM, particularly at most 40, particularly at most 30, particularly at most 20, particularly at most 10, particularly at most 5, particularly at most 2, particularly at most 1% by weight of 1,1-GPM is present (relative to the total weight of the dry matter of 1,1-GPM and 1,6-GPS present in the phase or composition, respectively).

[0209] In a preferred embodiment, the 1,1-GPM and / or 1,6-GPS enriched isomalt composition may also be a 1,1-GPM-enriched and / or 1,6-GPS-enriched phase. The 1,1-GPM-enriched phase and the 1,1-GPM-enriched isomalt composition obtained according to the invention, in particular according to process step e), have a higher 1,1-GPM content than the isomalt-containing solution used for its preparation according to the invention, in particular according to process step a). The 1,6-GPS-enriched phase and the 1,6-GPS-enriched composition obtained according to the invention, in particular according to process step e), have a higher 1,6-GPS content than the isomalt solution used for its preparation according to the invention, in particular according to process step a).

[0210] In a preferred manner, the increased 1,1-GPM content relative to the isomalt-containing solution in the 1,1-GPM-enriched phase or composition is increased by at least 5, at least 10, at least 15, at least 20, at least 30, at least 40, at least 50, at least 60, at least 70, at least 80, at least 90, at least 100, at least 150, in particular at least 200% by weight (respectively relative to the 1,1-GPM content in the isomalt solution provided by method step a)).

[0211] In a preferred manner, the increased 1,6-GPS content relative to the isomalt-containing solution in the 1,6-GPS-enriched phase or composition is increased by at least 5, at least 10, at least 15, at least 20, at least 30, at least 40, at least 50, at least 60, at least 70, at least 80, at least 90, at least 100, at least 150, in particular at least 200% by weight (respectively relative to the 1,6-GPS content in the isomalt solution provided by method step a)).

[0212] In the context of the present invention, the term "nucleation" refers to crystal nucleation, the first partial process initiating a first-order phase transition, during which a new phase that is thermodynamically stable under given conditions is formed by nuclei from an existing metastable, preferably supersaturated, phase.

[0213] In the context of the present invention, the term "supersaturated solution" or "supersaturated phase" refers to a metastable state of a solution containing a greater amount of solute than corresponds to the solubility of the substance of interest at a particular temperature. Such a supersaturated solution is preferably produced by slow cooling of a saturated solution, by evaporation of a portion of the solvent, or by a combination of cooling of the saturated solution and evaporation of a portion of the solvent, after which the excess solute precipitates, in particular crystallizes.

[0214] In the context of the present invention, the term "flash evaporation" refers to moderate evaporation, i.e. the production of steam when the pressure in a liquid-filled reactor is reduced. Flash evaporation increases the supersaturation of the isomalt-containing solution, which, in combination with the shear forces acting on the solution, triggers nucleation. In a flash evaporator, steam is produced when the pressure in the liquid-filled reactor is reduced, especially since during flash evaporation the liquid enters the reactor in a superheated state. The energy transfer thus induced causes the solution, especially the supersaturated solution, to cool and at the same time increases the dry matter content, which leads to nucleation. Flash evaporation is caused when the pressure is reduced in a reactor filled with saturated or supersaturated liquid and an associated vapor phase.

[0215] According to the present invention, the flash evaporation can be carried out continuously or intermittently. In the continuous flash evaporation, which is preferably carried out according to the present invention, the isomalt-containing solution is continuously fed into the reactor and the crystal syrup suspension according to the present invention obtained by flash evaporation is discharged at the same time.

[0216] In the context of the present invention, the term "isothermal crystallization" refers to the crystallization of a solution or suspension held at a constant crystallization temperature until crystallization is complete or until a specific amount of a component, in particular a crystalline phase enriched in 1,1-GPM or a crystalline phase enriched in 1,6-GPS, crystallizes out of the solution or suspension.

[0217] In the context of the present invention, a 1,1-GPM-enriched or 1,6-GPS-enriched phase means a 1,1-GPM-enriched or 1,6-GPS-enriched isomalt composition, respectively, having similar physical and chemical properties, such as a liquid or crystalline phase. Such a phase therefore comprises at least one 1,1-GPM-enriched or 1,6-GPS-enriched isomalt composition, respectively, optionally together with one or more solvents.

[0218] In the context of the present invention, a "Multiple-Effect-Evaporator" means an evaporator in which a solution or suspension is crystallized in several stages at low temperatures. In a Multiple-Effect-Evaporator, the solution is boiled in several interconnected stages, each successive reactor having a lower pressure than the previous reactor. Due to the decreasing pressure in the series of interconnected reactors, the boiling point of the solvent in the series of interconnected reactors is gradually reduced.

[0219] In the context of the present invention, the term "cooling crystallization" refers to the crystallization of a substance from a solution or suspension by lowering the temperature until crystallization is complete or until a specific amount of a component, in particular a crystalline phase enriched in 1,1-GPM or a crystalline phase enriched in 1,6-GPS, crystallizes out of the solution or suspension.

[0220] In the context of the present invention, the term "multi-stage evaporative crystallization" refers to enrichment of a crystalline phase by crystallization in several reactors, each having a different pressure level and / or temperature.

[0221] In the context of the present invention, "phase" means a continuous or discontinuous spatial portion of a suspension in which essentially the same homogeneous material properties are present. Thus, the liquid phase is the portion of a suspension that is characterized by its liquid state. The crystalline phase is the portion of a suspension that is characterized by its crystalline and therefore solid state.

[0222] In the context of the present invention, "crystalline phase" or "liquid phase" means a phase which is formed in the course of the process according to process steps b) and c).

[0223] In the context of the present invention, "reduced or reduced" absolute pressure means an absolute pressure that is reduced compared to the absolute ambient pressure, in particular compared to atmospheric pressure of 1 bar.

[0224] In the context of the present invention, unless otherwise specified and / or acknowledged, the percentage percentages of individual components specified with respect to the composition of the component total 100% by weight, i.e. the total composition.

[0225] In the context of the present invention, the term "and / or" means that all members of the group connected by the term "and / or" are represented mutually in any combination, both mutually additive and alternative. By way of example, the expression "A, B and / or C" should mean the disclosure of: i) (A or B or C), or ii) (A and B), or iii) (A and C), or iv) (B and C), or v) (A and B and C).

[0226] In the context of the present invention, "shear" means mechanical agitation, ie preferably movement, especially stirring.

[0227] In the context of the present invention, "stirring device" means inter alia a rotor-stator system.

[0228] In the context of the present invention, "rotor-stator system" means inter alia a homogenizer.

[0229] In the context of the present invention, "rotor" refers to the rotating part of the homogenizer, especially if a stator is present.

[0230] In the context of the present invention, "stator" means the stationary part of the homogenizer, especially if a rotor is present.

[0231] In the context of the present invention, the rotor is the stator, i.e. a propeller-type agitator which resides within a central tube and can rotate within the central tube.

[0232] In the context of the present invention, a "rotor blade having a rectangular shape" means a rotor blade having a constant blade chord.

[0233] In the context of the present invention, a "rotor blade having a trapezoidal shape" means a rotor blade having a chord that decreases in the longitudinal direction.

[0234] In the context of the present invention, a "rotor blade with a double trapezoid" means a rotor blade with a chord that increases and then decreases in the longitudinal direction.

[0235] In the context of the present invention, a "rotor blade having a rectangular trapezoidal shape" means a rotor blade having a chord that is constant and then decreases in the longitudinal direction.

[0236] In the context of the present invention, "crystal" means a solid having building blocks, especially molecules, regularly arranged in a crystalline structure.

[0237] In the context of the present invention, "reactor" particularly preferably means a vessel, in particular an maturation vessel, in which process step b) and / or process step c) is carried out.

[0238] In the context of the present invention, "evaporation" means the transition of a liquid or liquid mixture into the gaseous state.

[0239] In the context of the present invention, "reverse osmosis" refers to the reverse principle of osmosis, which refers to the process of concentration equilibration of two liquids through a semipermeable membrane. Reverse osmosis is particularly preferably carried out at elevated pressure relative to atmospheric pressure. Thereby, the solute, especially isomalt, remains in the starting solution or suspension, and the solvent, especially water, is expelled through a solvent-permeable membrane, especially a water-permeable membrane.

[0240] In the context of the present invention, "seeding" means the addition of seed crystals to the solution or suspension to be seeded.

[0241] In the context of the present invention, "tip speed" also means the rotor blade tip speed measured at the tip, i.e., the outer edge, of the rotor blade.

[0242] In the context of the present invention, the length-to-width ratio of a crystal is determined according to the methodology described in Example 2.

[0243] Further advantageous configurations of the invention emerge from the dependent claims.

[0244] The present invention will now be described in more detail with reference to examples and comparative examples and accompanying drawings. [Brief description of the drawings]

[0245] [Figure 1]1 shows the solubility diagram according to Schiweck (H. Schiweck, alimenta 19, Palatinit® - Production, technical properties and analysis of food products containing Palatinit (Palatinit® - Herstellung, technologische Eigenschaften und Analytik palatinithaltiger Lebensmittel), 5-16, 1980) for 1,1-GPM (GPM, 3), 1,6-GPS (GPS, 2) and isomalt (Isomalt, 1) in water, where the solubility limits of the abovementioned components are plotted as a function of temperature. [Diagram 2] AD show micrographs (4x magnification) of the crystallized product from Example 2.1. [Diagram 3] 5A-D show micrographs (10x magnification) of the crystallized product from Example 2.1. [Figure 4] 5A-D show micrographs (10x and 20x magnification) of the crystallized product from Example 2.2. [Diagram 5] AF show micrographs (4x and 10x magnification) of the crystallized product from Example 2.3. [Figure 6] AF show micrographs (4x and 10x magnification) of the crystallized product from Example 2.4. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0246] [Example 1]: Separation of Isomalt (hydrogenated isomaltulose) into 1,1-GPM and 1,6-GPS enriched isomalt compositions by flash evaporation in process step b) and subsequent isothermal crystallization in process step c). The two main components of isomalt, namely 1,1-GPM and 1,6-GPS, have different solubility products in aqueous solutions (Figure 1). In the suspension, each component forms its own solubility equilibrium. In the solid part (crystalline phase) of the suspension, an enrichment of the more crystallizable or less soluble component 1,1-GPM is obtained, since the less crystallizable or more soluble component 1,6-GPS preferably dissolves or remains dissolved. The equilibrium formed depends on the temperature for the same concentration of the suspension of isomalt in water. At the same temperature, as the proportion of dry matter (TS) of the suspension increases, the proportion of 1,6-GPS in the solution increases. The solubility diagrams (drawings) of 1,1-GPM, 1,6-GPS and isomalt show a constant increase in the solubility of the individual components with increasing temperature. The present invention makes use of this observation. The isomalt-containing solution obtained by the usual process steps is thermally concentrated in process step a1) to a dry matter content of 70 to 85% by weight. The isomalt-containing solution thus obtained and prepared in process step a) having a 1,1-GPM content of 35-44% by weight, i.e. 40.7% by weight, and a 1,6-GPS content of 56-65% by weight, i.e. 58.4% by weight (respectively relative to the total weight of the dry matter of the isomalt-containing solution), 0.01-2% by weight of GPI, 0.01-2% by weight of glycosyl glycitols, 0.01-0.4% by weight of sorbitol, 0.001-2% by weight of deoxydisaccharide alcohols, 0.1-10% by weight of 1,1-GPS and / or 0.01-0.3% by weight of mannitol (isomalt content 70-85% by weight relative to the total weight of the solution) is subsequently brought to a temperature of 60-75° C. and then subjected to flash evaporation according to process step b) of the process according to the invention for crystal nucleation in a so-called nucleation apparatus. The temperature of the isomalt-containing solution is adjusted to 60-75°C and then flash evaporation is carried out at an absolute pressure of 50-200 mbar, in particular 90-100 mbar, and a temperature of 50-55°C.The reduction in absolute pressure leads to an increase in the vapor pressure, which induces the dissipation of energy, leading to the transfer of 1,1-GPM, which is less soluble in water compared to 1,6-GPS (solubility according to Schiweck, see Figure 1), into a first crystalline phase according to its thermodynamic solubility product (initially about 5% of the 1,1-GPM present in the starting solution). Due to the stirrer geometry used in the reactor and the shear forces thus continuously generated, further 1,1-GPM-enriched crystal nuclei are subsequently produced.

[0247] After a residence time of up to 5 h, about 25% by weight of the 1,1-GPM initially present in the starting solution has been transferred to the first crystalline phase, and the first liquid phase obtained after carrying out the nucleation process according to process step b) contains 31% by weight of 1,1-GPM and 68% by weight of 1,6-GPS (based on the total weight of dry matter present in the solution). The first isomalt-containing suspension obtained from process step b) containing the 1,1-GPM-enriched crystal nuclei obtained according to process step b) is continuously subjected to a crystallization process according to process step c) carried out in a temperature-controlled crystallizer. In this case, under isothermal conditions in the temperature range of 50-60 ° C, in particular at 56 ° C, the crystal nuclei enriched with 1,1-GPM continue to grow further into crystals until the residual supersaturation is significantly reduced. The maintenance of isothermal conditions is ensured by the continuous dissipation of the released crystallization energy. By slowly and stepwise lowering the temperature of the maturation tank (crystallizer) to 55° C. (at most 0.5 K / h, in particular at most 0.1 K / h), the yield of crystals enriched with 1,1-GPM is additionally increased, without adversely affecting the purity of these crystals. The second suspension thus obtained can be worked up by suitable separation techniques (e.g. centrifugation) according to process step d), the second crystalline phase thus obtained contains 69.9% by weight of 1,1-GPM and 29.8% by weight of 1,6-GPS (based on the total weight of the dry matter of the second crystalline phase) and the separated second liquid phase contains 20.2% by weight of 1,1-GPM and 78.6% by weight of 1,6-GPS (based on the total weight of the dry matter of the second liquid phase).

[0248] [Example 2] The following examples compare the method according to the invention (Example 2.1) with known crystallization methods (Examples 2.2 to 2.4).

[0249] The experiments were carried out in a 2 liter cooling crystallizer equipped with a stirrer and a double jacket for thermostatic heating. The separation of the crystal magma was carried out in a heated pressure nutsche or in an industrial centrifuge. A microscope was used to image document the crystals in the crystal suspension. Image analysis was carried out using Olympus Stream Motion software.

[0250] The enriched phase obtained in the experiment was analyzed as follows: - Analysis of the water content of the filter cake (second crystalline phase) using the Karl Fischer method - Analysis of the water content of the filtrate (second liquid phase) using refractometry - Analysis of 1,1-GPM and 1,6-GPS contents by HPLC - Length to width ratio analysis: Microscopic crystal images of the second isomalt-containing suspension (magma) dispersed in glycerol were recorded at 4x and 10x magnifications using an Olympus camera (Olympus UC 90) and associated software and a Zeiss microscope (Carl Zeiss Axiolab re). At least 20 individual crystals per crystal image selected using a random generator were measured for crystal length and crystal width using the image analysis software Olympus Stream Motion (maximum characteristic crystal length and maximum characteristic crystal width at an angle of 90° thereto), and the ratio of the measured length to the measured width was calculated, from which the mean or median value was determined. Preferably, a diagonal line drawn across the microscopic crystal photograph (crystal image) was used as a random generator, and the length to width ratio was determined using all crystals on this diagonal line that allowed for a clear demarcation and determination of the crystal length and width. At least 20 crystals must be recognizable on the line. Otherwise, another microscopic photograph was taken and used.

[0251] Table 1 below shows the TS (dry matter) of the isomalt solution used in this example and the content of 1,1-GPM and 1,6-GPS relative to the total mass of the isomalt solution.

[0252] [Table 1]

[0253] [Example 2.1 (according to the present invention)]: The second suspension (magma) obtained according to the teaching according to Example 1 is partially removed from the crystallizer before centrifugation according to method step d), diluted in glycerol and a crystal image is taken. Separation of the solid and liquid phases in the centrifuge according to method step d) is further carried out for 30 minutes at a speed of 1800 revolutions per minute:

[0254] 2A-2D show crystal images (magnification x4) of the resulting magma dispersed in glycerol, and FIGS. 3A-3D show crystal images (magnification x10) of the resulting magma dispersed in glycerol.

[0255] The length to width ratios of the obtained crystals in the magma and in the second crystalline phase obtained in process step d) were 8.0 (average value) and 7.8 (median value).

[0256] From Table 2 below it is possible to see the composition of the phases obtained after separation (the filter cake is the solid crystalline phase and the filtrate is the liquid phase).

[0257] [Table 2]

[0258] The crystals obtained in the solid phase are particularly pure and show a high degree of uniformity in shape and size. The crystal suspension after the crystallization is complete does not show the formation of fine particles in the crystal image. The length to width ratio of the crystals contained in the second crystalline phase obtained in process step d) is relatively small. The separation of the obtained second crystalline phase by centrifugation is carried out very satisfactorily without problems. This is shown in particular in the enrichment of 1,1-GPM in the crystalline phase after centrifugation. The 1,6-GPS-enriched filtrate, i.e. the second liquid phase enriched with 1,6-GPS, leaves the filter cake very well. According to the invention, in the obtained second crystalline phase, an enrichment of 1,1-GPM and a reduction in 1,6-GPS are found, whereas in the obtained second liquid phase enriched with 1,6-GPS, an enrichment of 1,6-GPS and a reduction in 1,1-GPM are likewise found, respectively, compared to the starting composition.

[0259] [Example 2.2 (not according to the invention)]: WO1997 / 008958A1 discloses a method for producing a mixture enriched in 1,6-GPS and enriched in 1,1-GPM. Example 2 of this document discloses adding Isomalt® to 5 kg of (fully demineralized) water and stirring the resulting suspension at 35° C. for 1 to 20 hours depending on the particle size to produce a 1,1-GPM and 1,6-GPS enriched 1,1-GPM / 1,6-GPS mixture. The suspension is subsequently separated into liquid and solid phases at 35° C. in a heated pressure nutsche.

[0260] Testing Procedure: 1. Switch on the thermostat to heat the 2 liter crystallizer and adjust the flow temperature to 35.3°C. Temperature control is performed via the internal temperature sensor of the thermostat. Add 2.999.79 g of fully demineralized water to a 2 liter crystallizer. 3. Switch on the agitator and adjust the rotation speed to 60 revolutions per minute. 4. Preheat the water to 35℃ Add 5.999.96g of Isomalt ST-M to a 2 liter crystallizer. 6. 19.5 hours after isomalt addition: Preheat the double-jacketed pressure nutsche via the thermostat to 35°C. 7. 20 hours after isomalt addition: The resulting crystal suspension (magma) is removed from the crystallizer. 8. Prepare a portion of the magma for analysis by diluting it (1:1) with fully demineralized water. 9. Disperse some of the magma in glycerol to take images of the crystals in suspension 10. 200 ml of the magma is transferred to a preheated pressure nutsche and the crystals and mother liquor are separated. A polyethylene filter fleece of type Vyon D from Porvair Sciences with a mesh size of 15-25 μm is used as the filter. 11. Dilute the collected filtrate (1:1) with fully demineralized water for analysis. 12. Remove the crystals from the pressure nutsche for analysis

[0261] Test results: According to Example 2 of WO1997 / 008958A1, a suspension of isomalt in water is used as the starting material for the targeted enrichment and subsequent separation of the enriched solid and liquid phases, rather than an isomalt-containing solution.Therefore, within the scope of this method, there is no crystallization of the isomalt components from the solution during incubation at 35°C for about 20 hours, but only partial dissolution and dissolution of undissolved isomalt components from the solid phase of the suspension into the liquid phase and vice versa.

[0262] 4A and 4B show images (10x magnification) of the resulting magma dispersed in glycerol, and FIGS. 4C and 4D show images (20x magnification) of the resulting magma dispersed in glycerol.

[0263] Despite the high resolution magnification chosen, no individual crystals are visible, only partially dissolved flake-like particles, which are due to the partially amorphous solidified structure of the isomalt particles, which correspond to agglomerates of small microcrystals of 1,1-GPM and 1,6-GPS used in the starting suspension. These structures do not show the crystalline morphology expected in classical crystallization, since they originate from the drying process and not from the crystallization process. The enrichment principle interpreted in this comparative example is based on the elution of the more soluble 1,6-GPS component from a 1,1-GPM and 1,6-GPS-containing solid, and therefore does not correspond to the enrichment according to the invention by crystallization from a 1,1-GPM and 1,6-GPS-containing solution.

[0264] From table 3 below it is possible to see the 1,1-GPM and 1,6-GPS contents of the phases obtained after separation.

[0265] [Table 3]

[0266] [Example 2.3 (not according to the invention)]: EP0859006B2 discloses a method for producing a mixture enriched in 1,6-GPS and enriched in 1,1-GPM. Example 1 of this document discloses the use of a seeding process and two different cooling rates during crystallization to produce a 1,1-GPM / 1,6-GPS mixture enriched in 1,1-GPM and 1,6-GPS.

[0267] Testing Procedure: 1. Switch on the thermostat to heat the 2 liter crystallizer and adjust the flow temperature to 85°C. 2. Add 649.91 g of fully demineralized water to a 2 liter crystallizer. 3. Switch on the agitator and adjust the rotation speed to 100 rpm. 4. Heat the water to 85℃ 5. Add 2453.2g of Isomalt ST-F to a 2 liter crystallizer. 6. Start the cooling program a. Maintain 85°C for 2 hours - Temperature control via external PT100 in the crystallizer - Agitator speed of 100 revolutions per minute b. Cooling from 85°C to 65°C over 2 hours - Temperature control via internal PT100 in thermostat - Agitator speed of 60 revolutions per minute c.23. Cooling from 65°C to 37°C over 3 hours - Temperature control via internal PT100 in thermostat - Stirrer speed 60 revolutions per minute After reaching 7.62°C: Add 0.5 g of Isomalt ST-PF in 4.95 g of isopropanol via syringe to the solution. 8. After reaching 37℃: Remove the magma from the crystallizer. 9. Prepare a portion of the magma for analysis by diluting it (1:1) with fully demineralized water. 10. Disperse some of the magma in glycerol to take images of the crystals in suspension 11.604 g of magma is transferred to a centrifuge to separate the crystals from the mother liquor. A polyethylene filter fleece of type Vyon D from Porvair Sciences with a mesh size of 15-25 μm is used as a screen. The rotation speed is 1800 revolutions per minute. Centrifugation time is 30 minutes. No water washing. 12. Dilute the collected effluent (1:1) with fully demineralized water for analysis. 13. Remove the crystals from the centrifuge

[0268] Separation in the centrifuge could not be carried out satisfactorily. The amount of liquid discharged was small. The filter cake contained a high residual moisture content which could be clearly recognized visually.

[0269] 5A, 5B, and 5C show images of magma crystals dispersed in glycerol (magnification x4), and FIG. 5D, 5E, and 5F show images of magma crystals dispersed in glycerol (magnification x10).

[0270] The length-to-width ratio of the crystals in the magma is 11.2 (mean) and 11.1 (median).

[0271] From table 4 below it is possible to see the 1,1-GPM and 1,6-GPS contents of the phases obtained after separation.

[0272] [Table 4]

[0273] In the crystal images it is clearly visible that after crystallization is complete, significant fines formation occurs in the crystal suspension. The length to width ratio of the crystals is relatively large. Separation of the crystalline phases using centrifugation is not satisfactorily possible. The enrichment of 1,1-GPM in the crystalline phase obtained after centrifugation is minimal, and the content of 1,1-GPM and 1,6-GPS in the filter cake approximately corresponds to the composition of the starting solution. The 1,6-GPS-enriched filtrate only very poorly escapes from the filter cake.

[0274] [Example 2.4 (not according to the invention)]: US 6,414,138 B1 also discloses a method for producing a mixture enriched in 1,6-GPS and enriched in 1,1-GPM, Example 1 of this document discloses the production of a 1,1-GPM / 1,6-GPS mixture enriched in 1,1-GPM and 1,6-GPS using two different cooling rates during crystallization similar to that described in Example 2.3, but without seeding.

[0275] Testing Procedure: 1. Switch on the thermostat to heat the 2 liter crystallizer and adjust the flow temperature to 85°C. Add 2.627.44 g of fully demineralized water to a 2 liter crystallizer. 3. Switch on the agitator and adjust the rotation speed to 100 rpm. 4. Heat the water to 85℃ 5. Add 2372.5g of Isomalt ST-F to a 2 liter crystallizer. 6. Start the cooling program a. Maintain 85°C for 2 hours - Temperature control via external PT100 in the crystallizer - Agitator speed of 100 revolutions per minute b. Cooling from 85°C to 65°C over 2 hours - Temperature control via internal PT100 in thermostat - Agitator speed of 60 revolutions per minute c.23. Cooling from 65°C to 37°C over 3 hours - Temperature control via internal PT100 in thermostat - Stirrer speed 60 revolutions per minute 7. After reaching 37℃: Remove the magma from the crystallizer. 8. Prepare a portion of the magma for analysis by diluting it (1:1) with fully demineralized water. 9. Disperse some of the magma in glycerol to take images of the crystals in suspension

[0276] 6A, 6B, and 6C show images of magma crystals dispersed in glycerol (magnification x4), and FIG. 6D, 6E, and 6F show images of magma crystals dispersed in glycerol (magnification x10).

[0277] The length-to-width ratios of the crystals within the magma were 11.3 (mean) and 10.5 (median).

[0278] It is also clearly visible in these crystal images that significant fine particle formation occurs in the crystal suspension after crystallization is complete. The length to width ratio of the crystals is relatively large, comparable to the ratio from Example 2.3.

Claims

1. 1. A method for producing a 1,1-GPM and / or 1,6-GPS enriched isomalt composition from an isomalt-containing solution, comprising the steps of: a) providing an isomalt-containing solution comprising 65-90% by weight isomalt (based on the total weight of the isomalt-containing solution); b) subjecting the isomalt-containing solution provided in process step a) to flash evaporation in a reactor to generate crystal nuclei to obtain a first isomalt-containing suspension comprising a first crystalline phase and a first liquid phase; c) subjecting the first isomalt-containing suspension obtained in process step b) to a crystallization process to obtain a second isomalt-containing suspension comprising a second crystalline phase enriched in 1,1-GPM and a second liquid phase enriched in 1,6-GPS, d) separating the second crystalline phase enriched in 1,1-GPM and the second liquid phase enriched in 1,6-GPS of the second isomalt-containing suspension from process step c), and e) Obtaining a 1,1-GPM and / or 1,6-GPS enriched isomalt composition A method comprising:

2. 2. The method according to claim 1, wherein mechanical agitation is performed during method step b).

3. 2. The method according to claim 1, wherein the isomalt-containing solution provided in method step a) comprises 35 to 61% by weight of 1,1-GPM (based on the total weight of the dry matter (TS) of the provided isomalt-containing solution).

4. 2. The method according to claim 1, wherein the isomalt-containing solution provided in method step a) is adjusted to a temperature of 50 to 90°C.

5. 2. The method according to claim 1, wherein the isomalt-containing solution provided in method step a) is selected from the group consisting of 1,1-GPM, 1,6-GPS and 1,1-GPS, further deoxydisaccharide alcohols, and comprises at least one substance selected from the group consisting of 1,1-GPS, further deoxydisaccharide alcohols, polysaccharides, oligosaccharides, trisaccharides, disaccharides, monosaccharides, sorbitol, mannitol, and isomerezitose.

6. 2. The method according to claim 1, wherein the isomalt-containing solution provided in process step a) is obtained in process step a1) from an isomalt-containing starting solution or suspension by evaporation or reverse osmosis.

7. 2. The process according to claim 1, wherein the isomalt-containing solution used in process step a1) is obtained by selective hydrogenation, in particular by selective hydrogenation of 1,6-GPS.

8. 2. The process according to claim 1, wherein the reactor used for flash evaporation in process step b) is a nucleation device.

9. 2. The process according to claim 1, wherein the flash evaporation carried out in process step b) is carried out at an absolute pressure of 10 to 500 mbar, in particular 50 to 200 mbar, and at a temperature of 30 to 70° C., in particular 30 to 60° C.

10. 2. The method according to claim 1, wherein the flash evaporation carried out in method step b) is carried out for a period of from 2 minutes to 12 hours.

11. 2. The method according to claim 1, wherein the flash evaporation carried out in method step b) is carried out continuously.

12. 2. The method according to claim 1, wherein process step b) is carried out in such a way that during process step b) 20-30% (relative to the total weight of the dry matter (TS) of 1,1-GPM present in process step a) and dissolved is transferred into the first crystalline phase of the first crystalline isomalt-containing suspension.

13. 2. The method according to claim 1, wherein process step b) is carried out in such a way that during process step b) the dry matter content of the isomalt-containing solution provided in process step a) is increased by 1 to 6 wt. % (based on the total weight of dry matter (TS) of the provided isomalt-containing solution and of the obtained first isomalt-containing suspension, respectively).

14. 2. The method according to claim 1, wherein the crystallization process according to method step c) is carried out in a crystallizer.

15. 2. The method according to claim 1, wherein the crystallization process according to method step c) is carried out continuously.

16. 2. The method according to claim 1, wherein the crystallization process according to method step c) is an isothermal crystallization, in particular at a temperature of 50-60°C.

17. 2. The method according to claim 1, wherein the crystallization process according to method step c) is a cooling crystallization.

18. 2. The method according to claim 1, wherein the crystallization process according to method step c) is evaporative crystallization, in particular multi-stage evaporative crystallization.

19. 2. The method according to claim 1, wherein no seeding with seed crystals is carried out during the method, in particular during the isothermal crystallization in method step c).

20. 2. The method according to claim 1, wherein after process step d) the second crystalline phase enriched with 1,1-GPM is dried to obtain in process step e) a solid 1,1-GPM enriched isomalt composition.

21. 2. The method according to claim 1, wherein after process step d) the second liquid phase enriched with 1,6-GPS is concentrated at least once, in particular to a dry matter content of at least 60% by weight (based on the total weight of the second liquid phase), to obtain in process step e) a liquid 1,6-GPS-enriched isomalt composition.

22. 2. The method according to claim 1, wherein after process step d) the second liquid phase enriched with 1,6-GPS is dried to obtain in process step e) a solid 1,6-GPS-enriched isomalt composition.

23. 2. The method according to claim 1, wherein the second crystalline phase separated in method step d) comprises at least 60% by weight of 1,1-GPM (based on the total weight of the dry matter (TS) of the crystalline phase).

24. 2. The method of claim 1, wherein the second liquid phase separated in method step d) comprises at least 72% by weight of 1,6-GPS (based on the total weight of the dry matter (TS) of the second liquid phase).

25. 1,1-GPM enriched isomalt composition, particularly producible by the method according to claim 1, wherein the length to width ratio of the crystals contained in the 1,1-GPM enriched isomalt composition is between 7.0 and 10.5, particularly between 7.5 and 10.0, particularly between 7.5 and 9.0, particularly between 7.5 and 8.5, particularly 8.0 (average values ​​respectively).

26. 1. A 1,6-GPS enriched isomalt composition comprising 15-32% by weight of 1,1-GPM and 68-85% by weight of 1,6-GPS (relative to the total dry matter amount of 1,1-GPM and 1,6-GPS, respectively), in particular producible by the method according to claim 1, in particular having a 1,6-GPS content of at least 68% by weight (relative to the total weight of the dry matter (TS) of the composition).

27. 27. Use of a 1,1-GPM or 1,6-GPS enriched isomalt composition produced using the method of any one of claims 1 to 24 or a composition according to claim 25 or 26 in a product for human and / or animal consumption.

Images