Free-flowing carbohydrates and process for their preparation

Abstract

The present invention relates to a process for preparing a dry carbohydrate preparation from an aqueous crystalline carbohydrate starting preparation and carbohydrate particles and to a carbohydrate preparation prepared using the process.

Description

Technical Field

[0001] This invention relates to a method for preparing a dried carbohydrate preparation from an aqueous crystalline carbohydrate starting material and carbohydrate particles. Background Technology

[0002] Crystalline carbohydrate formulations coated with a syrupy film, or partially amorphous solid carbohydrate formulations, readily absorb moisture during storage, subsequently clumping together. This syrupy film may originate from previous carbohydrate processing steps. This causes the carbohydrate formulation to clump, making it difficult or impossible to flow, transport, measure, and store. However, for marketable carbohydrate formulations, storage-stable and measurable formulations are required. When processing easily clumping, non-free-flowing solid carbohydrate formulations, all process steps—including conveying, weighing, metering, and similar mechanical handling—incur problems. However, low-purity or syrup-coated solid crystalline carbohydrate formulations often possess desirable flavor characteristics, such as improved aroma, and are at least favored by certain consumer groups. However, only in exceptional circumstances will buyers in the local market accept so-called "soft candy carbohydrate formulations" (e.g., "Farin" or "Basterd"), i.e., viscous carbohydrate formulations, as specialty goods. Nevertheless, buyers (whether end consumers or processors) generally insist on carbohydrate formulations with free flowability and storage stability. In particular, "gummy carbohydrate formulations" can cause problems for processors in terms of handling and packaging. Prolonged packaging times and frequent production interruptions are detrimental to economic efficiency. Furthermore, carbohydrate formulations should contain as few additives or excipients as possible, including the use of so-called flow aids.

[0003] In existing technologies, carbohydrate formulations are typically dried to a certain degree so that the syrup film adhering to the crystals no longer directly sticks together. In this case, airtight packaging is required to prevent subsequent moisture absorption during the adsorption process. However, not all carbohydrate formulations can be processed in this way. The main problem with this method is that packaging and storage are complex and inconvenient due to the need to prevent subsequent moisture absorption. Carbohydrate formulations that are difficult to dry can be converted to a dried form using a spray drying process. However, this technology is expensive and unsuitable for carbohydrate formulations that are predominantly crystalline and contain only a small amount of syrup. This method also requires careful packaging and storage to prevent subsequent moisture absorption and sticking. Crystalline carbohydrate formulations that are prone to surface adhesion can use so-called flow aids. These flow aids typically do not contain the same carbohydrates as the desired end product, but are inorganic substances (such as SiO2, serotonin) or starches. The drawback is that additional adjuvants must be added to the carbohydrate formulation, which may create regulatory hurdles or consumer unacceptability, and cannot rule out a slight impact on sensory perception.

[0004] A drawback of some carbohydrate preparations, especially crystalline carbohydrate preparations containing sucrose, is their increased water content (exceeding 0.05 wt.% by total weight of the crystalline carbohydrate preparation, especially those containing sucrose). This is particularly problematic when the crystalline particles are coated with a syrupy film, leading to clumping and loss of free flowability. Furthermore, substances remaining on the crystal surface can exacerbate hygroscopicity. Summary of the Invention

[0005] In view of this, the technical problem to be solved by the present invention is to overcome the above-mentioned defects. Specifically, the technical problem of the present invention is to provide a low-cost, easy-to-implement method that can provide a free-flowing, transportable, measurable, and storable carbohydrate formulation, particularly a carbohydrate starting formulation containing syrup-coated crystalline particles, wherein the resulting carbohydrate formulation uses as few additives or adjuvants as possible or not at all, especially flow aids, and is particularly easy to package.

[0006] Specifically, the technical problem of the present invention is to provide a method for drying a starting preparation of water-soluble crystalline carbohydrates, the starting preparation containing at least two carbohydrates with different water solubility, particularly at least one poorly soluble carbohydrate and at least one readily soluble carbohydrate, which can efficiently provide a dried carbohydrate preparation while minimizing disturbance, and in particular can dry carbohydrate preparations that are difficult or impossible to dry by conventional methods.

[0007] To address the aforementioned technical problems of this invention, the present invention specifically provides a method for preparing a dried carbohydrate preparation from an aqueous crystalline carbohydrate starting material, comprising the following steps:

[0008] (a) Provides an aqueous crystalline carbohydrate starting material with a water content of 0.4 to 22.5 wt.%, particularly 2.5 to 12 wt.%, (based on the total weight of the carbohydrate starting material), wherein, in a drying reactor, the carbohydrate starting material is selected from sucrose-containing compositions, isomaltulose-containing trehalose-containing compositions and isomaltulitol-containing compositions, and provides carbohydrate particles, wherein the proportion of carbohydrate crystals with a diameter less than or equal to 100 μm in the carbohydrate particles is at least 80 wt.%, particularly when the water content of the carbohydrate starting material exceeds any possible water of crystallization, especially on the crystalline particles in liquid film form in the carbohydrate starting material;

[0009] (b) Under a pressure of 10–1100 mbar, carbohydrate particles are metered into an aqueous crystalline carbohydrate starting material within the drying reactor using a metering device, at a dosage of 2–30 wt.% (based on the total weight of the carbohydrate starting material), wherein the temperature of the aqueous carbohydrate starting material in the drying reactor is 20–80°C, particularly 40–60°C; and

[0010] (c) Under the conditions mentioned in step (b), the resulting mixture is homogenized by a mixing device to obtain a dried carbohydrate formulation.

[0011] Preferably, the aqueous crystalline carbohydrate starting material (based on the total weight of the carbohydrate starting material) provided in step (a) with a water content of 0.4–22.5 wt.%, particularly 2.5–12 wt.%, contains crystalline carbohydrate particles with a liquid-coated membrane, and is particularly composed of such liquid-coated crystalline particles. Preferably, in step (c), the obtained dried carbohydrate preparation comprises crystalline carbohydrate particles without a liquid-coated membrane, and is particularly composed of such liquid-coated crystalline particles.

[0012] The aqueous crystalline carbohydrate starting material used in this invention is particularly a formulation in which the carbohydrate crystals, especially the crystalline particles, are coated with a liquid film (also referred to herein as a liquid-encapsulating film). The liquid film (also referred to herein as a syrup film) represents an aqueous solution or suspension on the surface of the crystalline particles in one or more carbohydrate starting materials, which may originate from previous processing steps of the carbohydrate. Therefore, the water represented by the syrup film is not entirely present in the crystalline particles, but rather on the surface of the crystalline particles; in particular, the water in the syrup film is not water of crystallization. If water of crystallization is present in the carbohydrates, the syrup film represents more (i.e., additional) water in the product. Therefore, according to the invention, the water content of the crystalline particles in the aqueous crystalline carbohydrate starting material preferably exceeds any possible water of crystallization content. The aqueous crystalline carbohydrate starting material used in this invention is neither a dry carbohydrate preparation containing water of crystallization nor a dry carbohydrate preparation without water of crystallization.

[0013] Surprisingly, according to the present invention, the proportion of carbohydrate crystals with a diameter of less than or equal to 100 μm in the carbohydrate particles is at least 80 wt.%, which does not result in the expected agglomeration of crystalline particles as in aqueous starting formulations where the carbohydrate particles are coated with a syrup film. On the contrary, it advantageously enhances free flowability.

[0014] To address the aforementioned technical problems of this invention, the present invention specifically provides a method for preparing a dried carbohydrate preparation from an aqueous crystalline carbohydrate starting material, comprising the following steps:

[0015] (a) Provides an aqueous crystalline carbohydrate starting material with a water content of 0.4 to 22.5 wt.%, particularly 2.5 to 12 wt.%, (based on the total weight of the carbohydrate starting material), wherein, in a drying reactor, the carbohydrate starting material is selected from sucrose-containing compositions, isomaltulose-containing trehalose-containing compositions and isomaltulitol-containing compositions, and provides carbohydrate particles, wherein the proportion of carbohydrate crystals with a diameter of less than or equal to 100 μm in the carbohydrate particles is at least 80 wt.%;

[0016] (b) Under a pressure of 10–1100 mbar, carbohydrate particles are metered into an aqueous crystalline carbohydrate starting material within the drying reactor using a metering device, at a dosage of 2–30 wt.% (based on the total weight of the carbohydrate starting material), wherein the temperature of the aqueous carbohydrate starting material in the drying reactor is 20–80°C, particularly 40–60°C; and

[0017] (c) Under the conditions mentioned in step (b), the resulting mixture is homogenized by a mixing device to obtain a dry carbohydrate preparation, particularly with a water content of up to 6.0 wt.%, particularly up to 5.0 wt.%, particularly up to 1.9 wt.%, particularly 0.01 to 0.70 wt.% (all based on the total weight of the dry carbohydrate preparation).

[0018] The basic concept of this invention is an aqueous crystalline carbohydrate starting material with a water content of 0.4 to 22.5 wt.% (based on the total weight of the carbohydrate starting material), which is provided to a drying reactor in step (a) and carried out by a method, particularly using steps (b) and (c), to obtain a dried carbohydrate preparation with a lower water content than the aqueous crystalline carbohydrate starting material.

[0019] The aqueous crystalline carbohydrate starting material used in this invention is selected from the group consisting of sucrose-containing compositions, isomaltulose-containing and trehalose-containing compositions, and isomaltulitol-containing compositions. In step (a), carbohydrate particles are also provided, preferably containing the same carbohydrates as those in the carbohydrate starting material, and the proportion of carbohydrate crystals with a diameter less than or equal to 100 μm in the carbohydrate particles is at least 80 wt.%. In step (b), the carbohydrate particles provided in step (a) are added to the aqueous crystalline carbohydrate starting material in the drying reactor at a pressure of 10–1100 mbar using a metering device, at an amount of 2–30 wt.% (based on the total weight of the carbohydrate starting material), wherein the temperature of the aqueous carbohydrate starting material in the drying reactor is 20–80°C, thereby obtaining a mixture of carbohydrate particles and the aqueous starting material. In step (c), under the conditions mentioned in step (b), the mixture thus obtained is homogenized by a mixing device to obtain a dry carbohydrate preparation, particularly with a water content of at most 6.0 wt.%, at most 5.0 wt.%, or at most 1.9 wt.% (all based on the total weight of the dry carbohydrate preparation).

[0020] According to steps (b) and (c) of the present invention, the crystalline carbohydrate starting material with a certain moisture content can be dried to obtain a dried carbohydrate preparation with a moisture content lower than that of the crystalline carbohydrate starting material used in step (a) with a moisture content of 0.4 to 22.5 wt.% (based on the total weight of the carbohydrate starting material). Therefore, regardless of the specific moisture content of the crystalline carbohydrate starting material used, steps (b) and (c) can always reduce this moisture content, while unexpectedly and significantly improving free flowability. In particular, the dried carbohydrate preparation obtained according to steps (b) and (c) is characterized by its ability to be easily further processed in optional subsequent conditioning steps to form a particularly easily measurable and free-flowing dried conditioning product, an effect that would not be possible without upstream drying via steps (b) and (c) provided according to the present invention.

[0021] In particular, the present invention enables the aqueous crystalline carbohydrate starting material (e.g., a sucrose-containing starting material coated with a syrup film) provided in the drying reactor during step (a) to be completely undried or only dried to an economically advantageous degree of dryness before being provided according to step (a). According to the present invention, preparations directly derived from the carbohydrate crystallization process (e.g., crystal suspensions still containing residual water content, particularly residual mother liquor content) can be dried in the method of the present invention by adding 2–30 wt.% carbohydrate particles (based on the total weight of the carbohydrate starting material) in step (b) without increasing the cost burden.

[0022] Therefore, the present invention provides a method for preparing a dried carbohydrate preparation from an aqueous crystalline carbohydrate starting material and carbohydrate particles, wherein an aqueous crystalline carbohydrate starting material with a water content of 0.4 to 22.5 wt.% (based on the total weight of carbohydrates) is placed in a drying reactor, carbohydrate particles are provided in step (a), and carbohydrate particles are metered into the aqueous crystalline carbohydrate starting material placed in the drying reactor in step (b), and the resulting mixture is homogenized in step (c), and a dried carbohydrate preparation is obtained by means of the carbohydrate particles metered into the aqueous crystalline carbohydrate starting material.

[0023] The method of this invention achieves simple, efficient, and particularly cost-effective process control through a particularly preferred and advantageous approach. Specifically, the dried carbohydrate formulation obtained by the method of this invention is free-flowing, transportable, measurable, and storable, and is especially easier to flow, transport, measurable, and storable compared to dried carbohydrate formulations known in the art. Preferably, the dried carbohydrate formulation obtained by the method of this invention is easier to package than dried carbohydrate formulations known in the art, for example, dried carbohydrate formulations known in the art require airtight sealed packaging. Preferably, the method of this invention advantageously obtains a dried carbohydrate formulation with minimal or no additives or auxiliaries, particularly flow aids.

[0024] The advantage of this invention is that even if water is subsequently absorbed, the resulting carbohydrate preparation will not stick together, thus the resulting carbohydrate preparation can be stored stably.

[0025] The advantage of this invention lies in that it can still produce a storage-stable and measurable dry carbohydrate preparation without the need for additives or adjuvants. Furthermore, the storage stability of the carbohydrate preparation obtained by the method of this invention is not constrained by complex packaging designs to prevent future water absorption and clumping.

[0026] Compared to existing technologies, this invention provides a storage-stable dried carbohydrate formulation from a difficult-to-dry carbohydrate starting material using a low-energy process, making the technical work relatively simpler. Preferably, a mixing and metering device and a drying reactor, particularly a closed drying reactor, are used. Preferably, the low negative pressure in the drying reactor is particularly suitable for the drying process of this invention. Preferably, this invention achieves the drying of the carbohydrate starting material into a mixture of readily soluble and poorly soluble carbohydrates, which is particularly beneficial for sensory factors. Compared to existing technologies, this invention also preferably achieves the acquisition of a more marketable dried carbohydrate formulation according to the invention from a readily crystallizing aqueous carbohydrate starting material using only a few simple process steps. Particularly preferably, the method of this invention comprises only relatively simple process steps: providing, metering, homogenizing, and optionally packaging. Compared to existing technologies, the carbohydrate formulation of this invention exhibits good storage stability, remaining free-flowing even after subsequent absorption of moisture through adsorption. Specifically, the method of this invention can produce a dried carbohydrate formulation that is sensorily comparable to traditional gummy carbohydrate formulations, but without the same difficulty in processing.

[0027] In a preferred embodiment of the present invention, the method of the present invention is performed continuously, semi-continuously, or in batches.

[0028] In a preferred embodiment of the present invention, the drying reactor used in process steps (a) and (b) and preferred process step (c) is a container, particularly a container having at least one mixing device or configured to perform mixing motion (preferably regular mixing motion), particularly a container capable of rotation or pivoting motion, especially when one or more built-in components are present in the container.

[0029] In a preferred embodiment of the present invention, the drying reactor used in process steps (a) and (b) is particularly:

[0030] a) A vertical or substantially upright cylindrical dryer, preferably having one or more vertically mounted stirring shafts; or

[0031] b) A dryer having cylindrical and conical drying shell sections, or a completely conical dryer, preferably with a vertically positioned stirring shaft; or

[0032] c) A horizontal, substantially horizontal, or inclined dryer, preferably with one or more horizontal or horizontal stirring shafts; or

[0033] d) Mobile dryer, i.e., rotary or asymmetrical mobile dryer, with or without built-in components.

[0034] In a preferred embodiment of the invention, the drying reactor used in the invention may be equipped with a fixed or movable built-in component, such as a rotary built-in component, particularly a chopper, to better mix the material to be dried.

[0035] In a preferred embodiment of the present invention, the dryer can be arranged vertically, horizontally, or at any angle to the ground.

[0036] In a preferred embodiment of the present invention, the dryer, particularly the dryer shell, can perform symmetrical or asymmetrical movements.

[0037] In a preferred embodiment of the present invention, the dryer may adopt a symmetrical or asymmetrical configuration or any combination thereof, particularly a double-cylinder or triple-cylinder configuration. Preferably, the dryer may be configured as a circular, elliptical, or conical cylinder.

[0038] In a preferred embodiment of the present invention, the dryer may have one or more stirring shafts.

[0039] In a preferred embodiment of the present invention, the stirring shaft may have a fixed rotation axis or a movable position.

[0040] In a preferred embodiment of the present invention, the dryer can operate under vacuum or micro-overpressure.

[0041] In a preferred embodiment of the present invention, the dryer is provided with a heating and / or cooling system to regulate or control a specific temperature.

[0042] In a preferred embodiment of the present invention, the water content of the aqueous crystalline carbohydrate starting material provided in step (a) is 0.4–22.5 wt.%, particularly 0.5–22.5 wt.%, particularly 0.7–20.0 wt.%, particularly 1.0–18.0 wt.%, particularly 1.5–15.0 wt.%, particularly 2.0–13.0 wt.%, particularly 2.5–12.0 wt.%, particularly 4.0–10.0 wt.%, particularly 6.0–8.0 wt.%, particularly 0.4–4.0 wt.%, particularly 0.4–3.5 wt.%, particularly 0.4–3.0 wt.%, particularly 0.4–2.5 wt.%, particularly 0.6–2.0 wt.%, particularly 0.8–1.5 wt.%, particularly 1.0 wt.% (all based on the total weight of the carbohydrate starting material). Here, the water exists in the form of a liquid film on the solid crystalline carbohydrate particles of the carbohydrate starting material. If the carbohydrates in the carbohydrate starting formulation contain water of crystallization, the water content consists of the liquid film water content and the water of crystallization content.

[0043] Particularly preferably, the aqueous crystalline carbohydrate starting agent provided in step (a) is a crystalline carbohydrate particle coated with a syrup film, particularly a solid or semi-solid crystalline form.

[0044] Particularly preferably, the aqueous crystalline carbohydrate starting agent provided in step (a) is a suspension of crystalline carbohydrate particles in an aqueous medium, particularly a crystal slurry.

[0045] In a preferred embodiment of the present invention, the aqueous carbohydrate starting preparation provided in step (a) comprises: at least one poorly soluble carbohydrate having a solubility in water at 20°C of 5.0–53.0 g / 100 g, particularly 14.5–53.0 g / 100 g, particularly 15.2–53.0 g / 100 g, particularly 29.0–53.0 g / 100 g, particularly 47.1–53.0 g / 100 g, particularly 5.0 g / 100 g, particularly 1 g / 100 g. 4.5 g / 100 g, particularly 15.2 g / 100 g, particularly 29.0 g / 100 g, particularly 47.1 g / 100 g; and at least one readily soluble carbohydrate having a solubility in water at 20°C greater than 53.0 g / 100 g, particularly at least 58.6 g / 100 g, particularly at least 66.7 g / 100 g, particularly at least 68.7 g / 100 g, particularly at least 70.0 g / 100 g, particularly at least 78.9 g / 100 g.

[0046] In a preferred embodiment of the present invention, the aqueous carbohydrate starting formulation comprises at least one poorly soluble carbohydrate selected from the group consisting of: 1,1-GPM (1-O-α-D-glucopyranosyl-D-mannitol), isomaltulose, glucose, and mannitol.

[0047] In a preferred embodiment of the present invention, the aqueous carbohydrate starting formulation comprises at least one soluble carbohydrate selected from the group consisting of sucrose, 1,6-GPS(6-O-α-D-glucopyranosyl-D-sorbitol), fructose, trehalose, and sorbitol.

[0048] In a preferred embodiment of the present invention, the aqueous carbohydrate starting material comprises at least one insoluble carbohydrate selected from 1,1-GPM, isomaltulose, glucose and mannitol, and one soluble carbohydrate selected from sucrose, 1,6-GPS, fructose, trehalose and sorbitol.

[0049] In a preferred embodiment of the present invention, the insoluble carbohydrate is glucose. In another preferred embodiment of the present invention, glucose is a component selected from invert sugar, caramel syrup, and cane syrup containing carbohydrates.

[0050] In a preferred embodiment of the present invention, the aqueous carbohydrate starting formulation comprises: at least one poorly soluble carbohydrate selected from 1,1-GPM, isomaltulose, glucose, and mannitol, having a solubility in water at 20°C of 5.0–53.0 g / 100 g, particularly 14.5–53.0 g / 100 g, particularly 15.2–53.0 g / 100 g, particularly 29.0–53.0 g / 100 g, particularly 47.1–53.0 g / 100 g, particularly 5.0 g / 100 g, particularly 14.5 g / 100 g. 00g, particularly 15.2g / 100g, particularly 29.0g / 100g, particularly 47.1g / 100g; and at least one soluble carbohydrate selected from sucrose, 1,6-GPS, fructose, trehalose and sorbitol, having a solubility in water at 20°C greater than 53.0g / 100g, particularly at least 58.6g / 100g, particularly at least 66.7g / 100g, particularly at least 68.7g / 100g, particularly at least 70.0g / 100g, particularly at least 78.9g / 100g.

[0051] In a preferred embodiment of the present invention, the aqueous crystalline carbohydrate starting agent provided in step (a) is a sucrose starting agent.

[0052] In a preferred embodiment of the present invention, the aqueous carbohydrate starting agent provided in step (a) is a sucrose-containing starting agent containing sucrose (preferably in crystalline form), particularly composed of or containing at least one other substance.

[0053] In a preferred embodiment of the present invention, the aqueous carbohydrate starting agent provided in step (a) is a sucrose starting agent containing sucrose (preferably in crystalline form), glucose and fructose, particularly sucrose-containing starting agents.

[0054] In a preferred embodiment of the present invention, the aqueous crystalline carbohydrate preparation provided in step (a) comprises: sucrose, particularly 91.0–99.5 wt.%, particularly 92.0–98.5 wt.%, particularly 92.5–98.2 wt.%, particularly 92.7–98.1 wt.%, particularly 93.0–98.1 wt.% (all based on the total dry matter weight of the carbohydrate preparation provided in step (a)); glucose, particularly 0.30–1.00 wt.%, particularly 0.40–1.00 wt.%, particularly 0.44–0.77 wt.%, particularly 0.46–0.77 wt.%, particularly 0.48–0.77 wt.% (all based on the total dry matter weight of the carbohydrate preparation provided in step (a)); glucose, particularly 0.30–1.00 wt.%, particularly 0.40–1.00 wt.%, particularly 0.44–0.77 wt.%, particularly 0.46–0.77 wt.%, particularly 0.48–0.77 wt.% (all based on the total dry matter weight of the carbohydrate preparation provided in step (a)). The carbohydrate preparation provided in step (a) is based on the total dry weight of the carbohydrate preparation; fructose, particularly 0.10 to 0.70 wt.%, 0.30 to 0.60 wt.%, particularly 0.41 to 0.55 wt.%, particularly 0.43 to 0.54 wt.%, particularly 0.44 to 0.50 wt.% (all based on the total dry weight of the carbohydrate preparation provided in step (a)); water; and optional minor components, particularly 0.40 to 4.50 wt.%, particularly 0.40 to 4.36 wt.%, particularly 0.42 to 4.24 wt.%, particularly 0.40 to 4.04 wt.% (all based on the total dry weight of the carbohydrate preparation provided in step (a)).

[0055] In a preferred embodiment of the present invention, the aqueous carbohydrate starting preparation provided in step (a) is an aqueous sucrose composition containing crystalline sucrose and at least one other carbohydrate component selected from invert sugar, caramel syrup and cane syrup.

[0056] In a preferred embodiment of the present invention, the aqueous carbohydrate starting agent provided in step (a) is a sucrose starting agent containing sucrose (preferably in crystalline form), glucose and fructose (invert syrup form), and particularly sucrose-containing starting agent composed of the same.

[0057] In a preferred embodiment of the present invention, the aqueous carbohydrate starting agent provided in step (a) is a sucrose starting agent containing crystalline beet sucrose and sucrose in caramel syrup form, particularly a sucrose starting agent composed of the latter.

[0058] In a preferred embodiment of the present invention, the aqueous carbohydrate starting agent provided in step (a) is crystalline beet sugar and sucrose in the form of sucrose syrup, particularly a sucrose-containing starting agent composed thereof.

[0059] In a preferred embodiment of the present invention, the aqueous sucrose-containing starting agent provided in step (a) comprises sucrose (preferably in crystalline form) and invert sugar syrup, or comprises sucrose (preferably in crystalline form) and caramel syrup, or comprises sucrose (preferably in crystalline form) and cane sugar syrup, or comprises sucrose (preferably in crystalline form) and cane sugar syrup and caramel syrup.

[0060] In a preferred embodiment of the present invention, the aqueous sucrose-containing starting agent provided in step (a) comprises beet sucrose, particularly composed of beet sucrose.

[0061] In a preferred embodiment of the present invention, the aqueous sucrose-containing starting preparation provided in step (a) comprises sucrose, and is particularly composed of sucrose.

[0062] In a preferred embodiment of the present invention, the aqueous sucrose-containing starting agent provided in step (a) comprises sucrose (especially beet sucrose) and glucose, or comprises cane sucrose and glucose, particularly composed thereof.

[0063] In a preferred embodiment of the present invention, the aqueous sucrose-containing starting agent provided in step (a) comprises sucrose (especially beet sucrose) and fructose, or comprises cane sucrose and fructose, particularly composed thereof.

[0064] In a preferred embodiment of the present invention, the aqueous sucrose-containing starting agent provided in step (a) comprises sucrose (especially beet sucrose) as well as glucose and fructose, or comprises cane sucrose as well as glucose and fructose, particularly composed thereof.

[0065] In a preferred embodiment of the present invention, the aqueous sucrose-containing starting preparation provided in step (a) particularly comprises, in particular, beet sucrose or cane sucrose, glucose and / or fructose (especially in the form of invert sugar syrup), sucrose in the form of caramel syrup and sucrose in the form of cane syrup, and is particularly composed thereof.

[0066] In a particularly preferred embodiment of the present invention, the aqueous crystalline sucrose starting preparation provided in step (a) comprises, in particular, 70.0–98.0 wt.%, in particular, 80–98.0 wt.%, in particular, 90.0–98.0 wt.%, in particular, 95.0–98.0 wt.%, of sucrose, particularly crystalline sucrose (all based on the total dry weight of the aqueous sucrose starting preparation).

[0067] In a particularly preferred embodiment of the present invention, the hydrated sucrose starting material provided in step (a) comprises: sucrose, particularly 80.0–98.0 wt.%, particularly 90.0–98.0 wt.%, particularly 95.0–98.0 wt.% (all based on the total weight of the hydrated sucrose starting material); invert sugar syrup, particularly 1.40–12.0 wt.%, particularly 1.40–6.0 wt.%, particularly 1.40–3.0 wt.% (all based on the total weight of the hydrated sucrose starting material); and caramel syrup, particularly 0.60–8.0 wt.%, particularly 0.6–4.0 wt.%, particularly 0.6–2.0 wt.% (all based on the total weight of the hydrated sucrose starting material), particularly composed of the above.

[0068] In a particularly preferred embodiment of the present invention, the hydrated sucrose starting material provided in step (a) comprises: sucrose, particularly 80.0–92.2 wt.%, particularly 85.0–92.2 wt.%, particularly 90.0–92.2 wt.% (all based on the total weight of the hydrated sucrose starting material); cane sugar syrup, particularly 1.8–4.6 wt.%, particularly 1.80–3.4 wt.%, particularly 1.8–2.40 wt.% (all based on the total weight of the hydrated sucrose starting material); and caramel syrup, particularly 6.00–15.4 wt.%, particularly 6.0–11.6 wt.%, particularly 6.0–7.6 wt.% (all based on the total weight of the hydrated sucrose starting material), particularly composed of the above.

[0069] In a particular preferred embodiment, the present invention relates to the above method, wherein the aqueous crystalline carbohydrate starting agent provided in step (a) is a water-soluble isomaltitol starting agent or a water-soluble isomaltitol-containing or trehalose-containing starting agent.

[0070] In a particular preferred embodiment, the present invention relates to the above method, wherein the aqueous crystalline carbohydrate starting agent provided in step (a) is a water-soluble isomaltitol starting agent.

[0071] In a preferred embodiment of the present invention, isomaltitol is ST type isomaltitol or GS type isomaltitol.

[0072] In a particularly preferred embodiment of the present invention, the aqueous isomaltitol starting material provided in step (a) contains 1,1-GPM (1-O-α-D-glucopyranosyl-D-mannitol) and 1,6-GPS (6-O-α-D-glucopyranosyl-D-sorbitol) in a content of 90.0–100.0 wt.%, particularly 92.0–99.0 wt.%, particularly 93.0–98.0 wt.%, particularly 95.0–100.0 wt.% (based on the total dry weight of the aqueous isomaltitol starting material).

[0073] In a preferred embodiment of the present invention, the isomaltitol starting material provided in step (a) contains 45.0 to 50.0 wt.% 1,1-GPM (1-O-α-D-glucopyranosyl-D-mannitol) and 50 to 55 wt.% 1,6-GPS (6-O-α-D-glucopyranosyl-D-sorbitol) (both based on the total dry weight of the aqueous isomaltitol starting material).

[0074] In a preferred embodiment of the present invention, the isomaltitol starting material provided in step (a) contains 20.0 to 30.0 wt.% 1,1-GPM (1-O-α-D-glucopyranosyl-D-mannitol) and 70.0 to 80.0 wt.% 1,6-GPS (6-O-α-D-glucopyranosyl-D-sorbitol) (both based on the total dry weight of the aqueous isomaltitol starting material).

[0075] In a preferred embodiment of the present invention, the isomaltitol starting agent provided in step (a) contains 1,1-GPS (1-O-α-D-glucopyranosyl-D-sorbitol), sorbitol, mannitol, or GPI (glucopyranosyl-idutitol) or a mixture of two or more of the above.

[0076] In a particularly preferred embodiment of the present invention, the isomaltitol starting material provided in step (a) contains sorbitol, mannitol or GPI, in an amount of 0.00 to 0.20 wt.%, particularly 0.04 to 0.17 wt.% (all based on the total dry weight of the aqueous isomaltitol starting material, as determined by GC).

[0077] In a particularly preferred embodiment of the present invention, the isomaltitol starting material provided in step (a) contains 1,1-GPS in an amount of 0.20 to 0.70 wt.%, particularly 0.30 to 0.60 wt.% (all based on the total dry weight of the aqueous isomaltitol starting material, as determined by GC).

[0078] In a particularly preferred embodiment of the present invention, the pH value of the isomaltitol starting agent provided in step (a) is 4.0 to 4.7, particularly 4.1 to 4.5.

[0079] In a particular preferred embodiment, the present invention relates to the above method, wherein the carbohydrate starting agent provided in step (a) is a water-soluble starting agent containing isomaltulose and trehalose.

[0080] In a particularly preferred embodiment, the present invention relates to the above-described method, wherein the carbohydrate starting agent provided in step (a) is a water-soluble isomaltulose- and trehalose-containing starting agent, wherein the isomaltulose content is 65.0–90.0 wt.%, particularly 70.0–90.0 wt.%, particularly 75.0–88.0 wt.%, particularly 75.0–85.0 wt.%, and the trehalose content is 5.0–15.0 wt.%, particularly 6.5–13.0 wt.%, particularly 6.0–12.0 wt.%, particularly 7.0–10.0 wt.% (based on the total dry weight of the water-soluble isomaltulose- and trehalose-containing starting agent).

[0081] In a particularly preferred embodiment, the present invention relates to the above-described method, wherein the carbohydrate starting preparation provided in step (a) is a water-soluble isomaltulose-containing and trehalose-containing starting preparation, having an isomaltulose content of 65.0–90.0 wt.%, particularly 70.0–90.0 wt.%, particularly 75.0–88.0 wt.%, particularly 75.0–85.0 wt.%, and a trehalose content of 5.0–15.0 wt.%, particularly 6.5–13.0 wt.%, particularly 6.0–12.0 wt.%, particularly 7.0–10.0 wt.% (based on the total dry weight of the water-containing isomaltulose-containing and trehalose-containing starting preparation), and containing fructose, glucose, and sucrose, and optionally containing isomalutose and isomaltose.

[0082] In a particularly preferred embodiment, the present invention relates to the above-described method, wherein the carbohydrate starting agent provided in step (a) is a water-soluble isomaltulose- and trehalose-containing starting agent, wherein the isomaltulose content is 65.0–90.0 wt.%, particularly 70.0–90.0 wt.%, particularly 75.0–88.0 wt.%, particularly 75.0–85.0 wt.%, and the trehalose content is 5.0–15.0 wt.%, particularly It contains 6.5–13.0 wt.%, particularly 6.0–12.0 wt.%, particularly 7.0–10.0 wt.%, and its fructose content is 2.0–4.0 wt.%, glucose content is 1.0–3.0 wt.%, sucrose content is 0.1–12.0 wt.%, particularly 0.2–3.0 wt.% (based on the total dry weight of the starting preparation containing water, isomaltulose, and trehalose), and optionally contains isomalutose and isomaltose.

[0083] In a preferred embodiment of the present invention, the aqueous crystalline carbohydrate starting agent is semi-crystalline or fully crystalline.

[0084] In a preferred embodiment of the present invention, in step (a1) preceding step (a), an aqueous carbohydrate starting agent is prepared from at least two different carbohydrates.

[0085] In a preferred embodiment of the present invention, in process step (a1), at least two types of carbohydrates are mixed, particularly two types of carbohydrates with different solubilities, particularly at least one carbohydrate with good solubility and at least one carbohydrate with poor solubility.

[0086] In a preferred embodiment of the present invention, in process step (a1), the preparation temperature of the aqueous crystalline carbohydrate starting agent is 50-70°C, particularly 55-65°C, particularly 60°C.

[0087] In a preferred embodiment of the present invention, the at least two carbohydrates used in step (a1) are selected from the group consisting of sucrose (especially beet sucrose or cane sucrose), glucose and / or fructose (especially in the form of invert sugar syrup), sucrose in the form of caramel syrup and sucrose in the form of cane syrup.

[0088] In a preferred embodiment of the present invention, the carbohydrates in the aqueous crystalline carbohydrate starting preparation and the carbohydrate particles provided in step (a) are the same carbohydrates.

[0089] In a preferred embodiment of the present invention, the carbohydrate particles provided in step (a) comprise a sucrose-containing composition, an isomaltulose-containing trehalose-containing composition, and / or an isomaltulitol-containing composition, or are composed thereof.

[0090] In a preferred embodiment of the present invention, the carbohydrate particles are composed of sucrose or isomaltulose and trehalose or isomaltulitol or a mixture thereof.

[0091] In a preferred embodiment of the present invention, the carbohydrate particles are composed of sucrose, particularly in crystalline form, and especially in powder form.

[0092] In a preferred embodiment of the present invention, the carbohydrate particles are composed of isomaltulose and trehalose, particularly in crystalline form, and especially in powder form.

[0093] In a preferred embodiment of the present invention, the carbohydrate particles are composed of isomaltitol, particularly in crystalline form, and especially in powder form.

[0094] In a preferred embodiment of the present invention, the proportion of carbohydrate crystals with a diameter less than or equal to 100 μm, particularly less than or equal to 80 μm, particularly less than or equal to 70 μm, particularly less than or equal to 60 μm, particularly less than or equal to 50 μm, particularly less than or equal to 40 μm, particularly less than or equal to 32 μm, particularly less than or equal to 20 μm, and particularly less than or equal to 10 μm in the carbohydrate particles provided in step (a) is at least 80 wt.% (based on the total weight of the carbohydrate particles).

[0095] In a preferred embodiment of the present invention, the proportion of carbohydrate crystals with a diameter of less than or equal to 100 μm in the carbohydrate particles provided in step (a) is at least 80 wt.%, particularly at least 85 wt.%, particularly at least 90 wt.%, particularly at least 95 wt.%.

[0096] In a preferred embodiment of the present invention, the proportion of carbohydrate crystals with a diameter less than or equal to 100 μm in the carbohydrate particles provided in step (a) is at least 80 wt.%, particularly at least 85 wt.%, particularly at least 90 wt.%, particularly at least 95 wt.%, while the proportion of carbohydrate particles with a diameter of at most 32 μm is at least 70 wt.%.

[0097] In a preferred embodiment of the present invention, the proportion of carbohydrate crystals with a diameter of less than or equal to 50 μm in the carbohydrate particles provided in step (a) is at least 80 wt.%, particularly at least 85 wt.%, particularly at least 90 wt.%, particularly at least 95 wt.%.

[0098] In a preferred embodiment of the present invention, the proportion of carbohydrate crystals with a diameter less than or equal to 100 μm, particularly less than or equal to 80 μm, particularly less than or equal to 70 μm, particularly less than or equal to 60 μm, particularly less than or equal to 50 μm, particularly less than or equal to 40 μm, particularly less than or equal to 32 μm, particularly less than or equal to 20 μm, particularly less than or equal to 10 μm in the carbohydrate particles provided in step (a) is at least 80 wt.%, particularly at least 85 wt.%, particularly at least 90 wt.%, particularly at least 95 wt.% (all based on the total weight of the carbohydrate particles).

[0099] In a preferred embodiment of the present invention, the carbohydrate particles provided in step (a) are crystalline, preferably fully crystalline.

[0100] In a preferred embodiment of the present invention, the carbohydrate particles provided in step (a) have no or only a small amount of amorphous structure.

[0101] In a preferred embodiment of the present invention, the carbohydrate particles provided in step (a) are measured in step (b) as follows: 2-30 wt.%, particularly 7-30 wt.%, particularly 10-30 wt.%, particularly 7-25 wt.%, particularly 10-25 wt.%, particularly 7-20 wt.%, particularly 10-25 wt.%, particularly 7-15 wt.%, particularly 10-15 wt.%, particularly 7-10 wt.% (all based on the total weight of the carbohydrate starting preparation).

[0102] In a preferred embodiment of the present invention, the carbohydrate particles provided in step (a) are measured in step (b) at 2 to 25 wt.%, particularly 5 to 20 wt.%, particularly 7 to 15 wt.%, particularly 8 to 10 wt.% (based on the total weight of the carbohydrate starting preparation).

[0103] In a preferred embodiment of the present invention, the carbohydrate particles provided in step (a) are measured in step (b) at 4 to 25 wt.%, particularly 4 to 20 wt.%, particularly 4 to 15 wt.%, particularly 4 to 10 wt.% (based on the total weight of the carbohydrate starting preparation).

[0104] In a preferred embodiment of the present invention, the temperature of process step (b) is 20-35°C, particularly 20-30°C.

[0105] In a preferred embodiment of the present invention, in step (b), carbohydrate particles are metered in a drying reactor without overpressure or negative pressure at atmospheric pressure; or in a vacuum drying reactor at reduced pressure, particularly 10–900 mbar, particularly 20–600 mbar, particularly 30–400 mbar, particularly 40–200 mbar, particularly 50–100 mbar, or particularly 600–800 mbar, particularly 650–750 mbar, particularly 700 mbar; or in a pressurized drying reactor at atmospheric pressure to 1100 mbar, particularly at pressures higher than atmospheric pressure to 1100 mbar.

[0106] In a preferred embodiment of the present invention, particularly under overpressure or negative pressure, measurement is performed by a metering device, particularly by a rotary metering system, a vibration or oscillation metering system, or a pneumatic metering system.

[0107] In a preferred embodiment of the present invention, the metering in process step (b) is mechanical metering performed by a rotary metering system, which is a rotary valve, a metering gate, or a screw conveyor.

[0108] In a preferred embodiment of the present invention, the measurement in step (b) is a vibration or oscillation measurement performed by a vibration or oscillation measurement system, which is a vibrating trough (especially a linear vibrating trough) or a screw conveyor.

[0109] In a preferred embodiment of the present invention, the metering in process step (b) is pneumatic metering performed by a pneumatic metering system, which is a flight conveyor system, a dense phase conveyor system, a push conveyor system, or a plug conveyor system.

[0110] In a preferred embodiment of the invention, the pneumatic metering system is attached with at least one, particularly at least two, particularly at least three, particularly at least four, particularly at least five nozzles. Preferably, these nozzles can advantageously improve the distribution of fine-grained carbohydrates.

[0111] If necessary, the measurement can also be manually controlled using a measuring shovel or measuring spoon.

[0112] In a preferred embodiment of the present invention, the mixture obtained in step (b) comprises carbohydrates sucrose, glucose, fructose and water.

[0113] In a preferred embodiment of the present invention, the temperature of the mixture obtained in step (b) in step (c) is 20–80°C, particularly 25–60°C, particularly 30–50°C, particularly 40–50°C, particularly 25–40°C.

[0114] In a preferred embodiment of the present invention, the water content of the dried carbohydrate preparation obtained in step (c) is at most 6.0 wt.%, particularly at most 5.0 wt.%, particularly at most 1.9 wt.%, particularly at most 1.5 wt.%, particularly at most 1.0 wt.%, particularly at most 0.8 wt.%, particularly at most 0.7 wt.%, particularly at most 0.6 wt.%, particularly at most 0.5 wt.%, particularly at most 0.4 wt.%, particularly at most 0.3 wt.%, particularly at most 0.2 wt.%, particularly at most 0.1 wt.%, particularly from 0.01 to 6.00 wt.%, particularly from 0.01 to 5.00 wt.%, particularly... 0.01–0.70 wt.%, particularly 0.05–6.00 wt.%, particularly 0.05–5.00 wt.%, particularly 0.05–0.60 wt.%, particularly 0.10–0.50 wt.%, particularly 0.20–0.40 wt.%, particularly 0.20–0.30 wt.%, particularly 0.12 wt.%, particularly 0.13 wt.%, particularly 0.27 wt.%, particularly 0.29 wt.%, particularly 0.31 wt.%, particularly 0.34 wt.%, particularly 0.42 wt.%, particularly 0.43 wt.%, particularly 0.47 wt.% (all based on the total weight of the dried carbohydrate preparation). Preferably, the water content of the dried carbohydrate preparation obtained in step (c) is only the water of crystallization present in the carbohydrate preparation.

[0115] According to the present invention, the water content of the dried carbohydrate preparation obtained in step (c) is lower than the water content of the water-containing carbohydrate starting preparation provided in step (a).

[0116] In a preferred embodiment of the present invention, the water content of the aqueous crystalline carbohydrate starting preparation provided in step (a) is 0.4–22.5 wt.%, particularly 0.5–22.5 wt.%, particularly 0.7–20 wt.%, particularly 1.0–18 wt.%, particularly 1.5–15 wt.%, particularly 2.0–13 wt.%, particularly 2.5–12 wt.%, particularly 4.0–10 wt.%, particularly 6.0–8.0 wt.%, particularly 0.4–4.0 wt.%, particularly 0.4–3.5 wt.%, particularly 0. 0.4–3.0 wt.%, particularly 0.4–2.5 wt.%, particularly 0.6–2.0 wt.%, particularly 0.8–1.5 wt.%, particularly 1.0 wt.% (all based on the total weight of the carbohydrate starting preparation), and the moisture content of the dried carbohydrate preparation obtained in step (c) is at most 6.0 wt.%, particularly at most 5.0 wt.%, particularly at most 1.9 wt.%, particularly at most 1.5 wt.%, particularly at most 1.0 wt.%, particularly at most 0.8 wt.%, particularly at most 0.7 wt.%, particularly at most 0. 0.6 wt.%, particularly up to 0.5 wt.%, particularly up to 0.4 wt.%, particularly up to 0.3 wt.%, particularly up to 0.2 wt.%, particularly up to 0.1 wt.%, particularly 0.01–6.00 wt.%, particularly 0.01–5.00 wt.%, particularly 0.01–0.70 wt.%, particularly 0.05–6.00 wt.%, particularly 0.05–5.00 wt.%, particularly 0.05–0.60 wt.%, particularly 0.10–0.50 wt.%, particularly 0.20–0.40 wt. The water content of the dried carbohydrate preparation obtained in step (c) is wt.%, particularly 0.20–0.30 wt.%, particularly 0.12 wt.%, particularly 0.13 wt.%, particularly 0.27 wt.%, particularly 0.29 wt.%, particularly 0.31 wt.%, particularly 0.34 wt.%, particularly 0.42 wt.%, particularly 0.43 wt.%, particularly 0.47 wt.% (all based on the total weight of the dried carbohydrate preparation), wherein the water content of the dried carbohydrate preparation obtained in step (c) is lower than the water content of the aqueous crystalline carbohydrate starting preparation provided in step (a). Preferably, the water content of the dried carbohydrate preparation obtained in step (c) is only the amount of water of crystallization present in the carbohydrate preparation.

[0117] In a preferred embodiment of the present invention, the dried carbohydrate preparation obtained in step (c) comprises sucrose, glucose, fructose and water.

[0118] In a preferred embodiment of the present invention, the dried carbohydrate preparation obtained in step (c) comprises: sucrose, particularly 92.0–98.5 wt.%, particularly 92.5–98.2 wt.%, particularly 92.7–98.1 wt.%, particularly 93.0–98.1 wt.% (all based on the total weight of the dried carbohydrate preparation obtained in step (c)); glucose, particularly 0.40–1.00 wt.%, particularly 0.44–0.74 wt.%, particularly 0.46–0.72 wt.%, particularly 0.48–0.69 wt.% (all based on the total weight of the dried carbohydrate preparation obtained in step (c)); fructose, particularly 0.30–0.50 wt.%, particularly 0. 41–0.48 wt.%, particularly 0.43–0.47 wt.%, particularly 0.44–0.45 wt.% (all based on the total weight of the dried carbohydrate preparation obtained in step (c)); and water, particularly 0.40–6.00 wt.%, particularly 0.40–5.00 wt.%, particularly 0.40–2.0 wt.%, particularly 0.58–1.87 wt.%, particularly 0.61–1.82 wt.%, particularly 0.63–1.74 wt.%, particularly 0.33–0.49 wt.%, particularly 0.37–0.46 wt.%, particularly 0.44–0.45 wt.% (all based on the total weight of the dried carbohydrate preparation obtained in step (c)). Preferably, the water content of the dried carbohydrate preparation obtained in step (c) is only the amount of water of crystallization present in the carbohydrate preparation.

[0119] In a preferred embodiment of the present invention, the dried carbohydrate preparation obtained in step (c) comprises: sucrose, particularly 92.0–98.5 wt.%, particularly 92.5–98.2 wt.%, particularly 92.7–98.1 wt.%, particularly 93.0–98.1 wt.% (all based on the total weight of the dried carbohydrate preparation obtained in step (c)); glucose, particularly 0.40–1.00 wt.%, particularly 0.44–0.74 wt.%, particularly 0.46–0.72 wt.%, particularly 0.48–0.69 wt.% (all based on the total weight of the dried carbohydrate preparation obtained in step (c)); fructose, particularly 0.30–0.50 wt.%, particularly 0.41–0.48 wt.%, particularly 0.43–0.47 wt.%, particularly 0.44–0.45 wt.% (all based on the total weight of the dried carbohydrate preparation obtained in step (c)); The total weight of the dried carbohydrate preparation obtained in step (c); minor components, particularly 0.40–4.50 wt.%, particularly 0.40–4.36 wt.%, particularly 0.42–4.24 wt.%, particularly 0.40–4.04 wt.% (all based on the total weight of the dried carbohydrate preparation obtained in step (c)); and water, particularly 0.40–6.00 wt.%, particularly 0.40–5.00 wt.%, particularly 0.40–2.0 wt.%, particularly 0.58–1.87 wt.%, particularly 0.61–1.82 wt.%, particularly 0.63–1.74 wt.%, particularly 0.33–0.49 wt.%, particularly 0.37–0.46 wt.%, particularly 0.44–0.45 wt.% (all based on the total weight of the dried carbohydrate preparation obtained in step (c)). Preferably, the water content of the dried carbohydrate preparation obtained in step (c) is only the water of crystallization present in the carbohydrate preparation.

[0120] In a preferred embodiment of the present invention, the angle of repose of the dried carbohydrate preparation obtained in step (c) is 30.0° to 45.0°, particularly 38.0° to 42.0°, particularly 39.0° to 41.0°, particularly 38.1°, particularly 40.7°, particularly 41.9°.

[0121] In a preferred embodiment of the present invention, the free flowability of the dried carbohydrate preparation obtained in step (c) is 0.1 to 45.0 s / 100g, particularly 0.2 to 45.0 s / 100g, particularly 0.5 to 40.0 s / 100g, particularly 1.5 to 35.0 s / 100g, particularly 2.0 to 25.0 s / 100g.

[0122] In a preferred embodiment of the present invention, under the condition that the outlet size of the test funnel is 6 mm, the free flowability of the dried carbohydrate preparation obtained in step (c) is 20.0–45.0 s / 100g, particularly 30.0–40.0 s / 100g, particularly 32.0–40.0 s / 100g, particularly 34.0–40.0 s / 100g, particularly 34.2 s / 100g, particularly 39.1 s / 100g.

[0123] In a preferred embodiment of the present invention, under the condition that the outlet size of the test funnel is 8 mm, the free flowability of the dried carbohydrate preparation obtained in step (c) is 10.0-25.0 s / 100g, particularly 12.0-23.0 s / 100g, particularly 14.0-18 s / 100g, particularly 15.5 s / 100g, particularly 15.7 s / 100g, particularly 22.5 s / 100g.

[0124] In a preferred embodiment of the present invention, under the condition that the outlet size of the test funnel is 10 mm, the free flowability of the dried carbohydrate preparation obtained in step (c) is 6.0 to 20.0 s / 100g, particularly 7.0 to 19.0 s / 100g, particularly 8.0 to 15.0 s / 100g, particularly 8.2 s / 100g, particularly 8.3 s / 100g, particularly 13.2 s / 100g, particularly 18.1 s / 100g.

[0125] In a preferred embodiment of the present invention, under the condition that the outlet size of the test funnel is 11.3 mm, the free flowability of the dried carbohydrate preparation obtained in step (c) is 3.0 to 15.0 s / 100g, particularly 4.0 to 14.0 s / 100g, particularly 5.0 to 13.0 s / 100g, particularly 5.2 s / 100g, particularly 5.3 s / 100g, particularly 8.1 s / 100g, particularly 12.6 s / 100g.

[0126] In a preferred embodiment of the present invention, under the condition that the outlet size of the test funnel is 15 mm, the free flowability of the dried carbohydrate preparation obtained in step (c) is 1.0 to 8.0 s / 100g, particularly 1.5 to 7.0 s / 100g, particularly 2.0 to 6.5 s / 100g, particularly 2.2 s / 100g, particularly 2.3 s / 100g, particularly 3.9 s / 100g, particularly 6.5 s / 100g.

[0127] In a preferred embodiment of the present invention, under the condition that the outlet size of the test funnel is 25 mm, the free flowability of the dried carbohydrate preparation obtained in step (c) is 0.1 to 4.0 s / 100 g, particularly 0.2 to 3.0 s / 100 g, particularly 0.2 to 2.0 s / 100 g, particularly 0.2 s / 100 g, particularly 0.6 s / 100 g, particularly 1.9 s / 100 g.

[0128] In a preferred embodiment of the present invention, the total water content of the dried carbohydrate preparation obtained in step (c) is 0.1–0.5 g / 100 g, particularly 0.2–0.5 g / 100 g, particularly 0.3–0.5 g / 100 g, particularly 0.33–0.46 g / 100 g, particularly 0.33 g / 100 g, particularly 0.37 g / 100 g, particularly 0.44 g / 100 g, particularly 0.46 g / 100 g.

[0129] In a preferred embodiment of the present invention, the surface water content of the dried carbohydrate preparation obtained in step (c) is 0.2-0.5 g / 100 g, particularly 0.3-0.5 g / 100 g, particularly 0.31-0.43 g / 100 g, particularly 0.31 g / 100 g, particularly 0.34 g / 100 g, particularly 0.42 g / 100 g, particularly 0.43 g / 100 g.

[0130] In a preferred embodiment of the present invention, the mixing device used in step (c) is used to mix the mixture obtained in step (b), thereby homogenizing it, that is, distributing the mixed components as evenly as possible. Therefore, the mixing device is used to mechanically stir the obtained mixture.

[0131] In a preferred embodiment of the present invention, the mixing device in step (c) is a mixing device arranged in the drying reactor, particularly one or more stirring shafts.

[0132] In a preferred embodiment of the present invention, the mixing device in step (c) is integrally connected to the drying reactor or a component of the drying reactor and configured to perform mixing motion (preferably regular mixing motion), particularly to be a drying reactor capable of rotation or pivoting motion, especially when one or more built-in components are present in the drying reactor.

[0133] In one preferred embodiment, process steps (a), (b), and (c) are carried out in a drying reactor configured to perform mixing motion (preferably regular mixing motion), particularly a drying reactor capable of rotational or pivotal motion, especially when one or more built-in components are present in the drying reactor. In one preferred embodiment, the drying reactor and the mixing device represent a single unit.

[0134] In a preferred embodiment of the present invention, the temperature of process step (c) is 20-35°C, particularly 20-30°C.

[0135] In a preferred embodiment of the present invention, modulation is performed in step (d) after step (c).

[0136] In a preferred embodiment of the present invention, the modulation temperature according to process step (d) is at least 30°C, particularly 30–180°C, particularly 35–160°C, particularly 45–100°C, particularly 35–60°C, particularly 40–60°C, particularly 50–60°C.

[0137] In a preferred embodiment of the present invention, the modulation pressure according to process step (d) is 10-1100 mbar, particularly 10-1000 mbar, particularly 10-900 mbar, particularly 20-600 mbar, particularly 30-400 mbar, particularly 40-200 mbar, particularly 50-100 mbar.

[0138] In a preferred embodiment of the present invention, the conditioning performed in step (d) is a drying process, particularly air drying, especially at an air temperature of 85–95°C, particularly 90°C.

[0139] In a preferred embodiment of the present invention, the water content of the modified carbohydrate preparation obtained in step (d) is at most 6.0 wt.%, particularly at most 5.0 wt.%, particularly at most 1.9 wt.%, particularly at most 1.5 wt.%, particularly at most 1.0 wt.%, particularly at most 0.8 wt.%, particularly at most 0.7 wt.%, particularly at most 0.6 wt.%, particularly at most 0.5 wt.%, particularly at most 0.4 wt.%, particularly at most 0.3 wt.%, particularly at most 0.2 wt.%, particularly at most 0.1 wt.%, particularly from 0.01 to 6.00 wt.%, particularly from 0.01 to 5.00 wt.%, particularly... 0.01–0.70 wt.%, particularly 0.05–6.00 wt.%, particularly 0.05–5.00 wt.%, particularly 0.05–0.60 wt.%, particularly 0.10–0.50 wt.%, particularly 0.20–0.40 wt.%, particularly 0.20–0.30 wt.%, particularly 0.12 wt.%, particularly 0.13 wt.%, particularly 0.27 wt.%, particularly 0.29 wt.%, particularly 0.31 wt.%, particularly 0.34 wt.%, particularly 0.42 wt.%, particularly 0.43 wt.%, particularly 0.47 wt.% (all based on the total weight of the dried carbohydrate preparation). Preferably, the water content of the prepared carbohydrate preparation obtained in step (d) is only the amount of water of crystallization present in the carbohydrate preparation.

[0140] In a preferred embodiment of the present invention, the modified carbohydrate preparation obtained in step (d) comprises: sucrose, particularly 94.0–99.0 wt.%, particularly 94.0–98.7 wt.%, particularly 94.1–98.7 wt.%, particularly 94.2–98.6 wt.%, particularly 94.3–98.5 wt.% (all based on the total weight of the modified carbohydrate preparation obtained in step (d)); and glucose, particularly 0.40–1.00 wt.%, particularly 0.45–0.76 wt.%, particularly 0.47–0.73 wt.%, particularly 0.48–0.70 wt.% (all based on the total weight of the modified carbohydrate preparation obtained in step (d)). Fructose, particularly 0.30–0.50 wt.%, particularly 0.41–0.49 wt.%, particularly 0.43–0.47 wt.%, particularly 0.44–0.45 wt.% (all based on the total weight of the modified carbohydrate preparation obtained in step (d)); and water, particularly 0.10–6.00 wt.%, particularly 0.10–5.00 wt.%, particularly 0.40–6.00 wt.%, particularly 0.10–0.50 wt.%, particularly 0.12–0.42 wt.%, particularly 0.13–0.29 wt.%, particularly 0.27–0.28 wt.% (all based on the total weight of the modified carbohydrate preparation obtained in step (d)). Preferably, the water content of the dried carbohydrate preparation obtained in step (c) is only the amount of water of crystallization present in the carbohydrate preparation.

[0141] In a preferred embodiment of the present invention, the modified carbohydrate preparation obtained in step (d) comprises: sucrose, particularly 94.0–99.0 wt.%, particularly 94.0–98.7 wt.%, particularly 94.1–98.7 wt.%, particularly 94.2–98.6 wt.%, particularly 94.3%–98.5 wt.% (all based on the total weight of the modified carbohydrate preparation obtained in step (d)); glucose, particularly 0.40–1.0 wt.%, particularly 0.45–0.76 wt.%, particularly 0.47–0.73 wt.%, particularly 0.48–0.70 wt.% (all based on the total weight of the modified carbohydrate preparation obtained in step (d)); fructose, particularly 0.30–0.50 wt.%, particularly 0. 0.41–0.49 wt.%, particularly 0.43–0.47 wt.%, particularly 0.44–0.45 wt.% (all based on the total weight of the modified carbohydrate preparation obtained in step (d)); minor components, particularly 0.20–4.50 wt.%, particularly 0.40–4.43 wt.%, particularly 0.42–4.30 wt.%, particularly 0.40–4.1 wt.% (all based on the total weight of the modified carbohydrate preparation obtained in step (d)); and water, particularly 0.10–0.50 wt.%, particularly 0.12–0.42 wt.%, particularly 0.13–0.29 wt.%, particularly 0.27–0.28 wt.% (all based on the total weight of the modified carbohydrate preparation obtained in step (d)).

[0142] In a preferred embodiment of the present invention, the angle of repose of the modified carbohydrate preparation obtained in step (d) is 30.0° to 45.0°, particularly 33.0° to 41.0°, particularly 35.0° to 38.5°, particularly 36.0° to 37.0°, particularly 33.7°, particularly 35.1°, particularly 36.4°, particularly 36.6°, particularly 38.5°, particularly 40.8°.

[0143] In a preferred embodiment of the present invention, the free flowability of the modified carbohydrate preparation obtained in step (d) is 0–45.0 s / 100g, particularly 0.1–45.0 s / 100g, particularly 1.3–40.0 s / 100g, particularly 2.0–30.0 s / 100g, particularly 3.0–25.0 s / 100g.

[0144] In a preferred embodiment of the present invention, under the condition that the outlet size of the test funnel is 6 mm, the free flowability of the modified carbohydrate preparation obtained in step (d) is 20.0–45.0 s / 100g, particularly 28.0–37.0 s / 100g, particularly 30.0–37.0 s / 100g, particularly 32.0–36.5 s / 100g, particularly 28.5 s / 100g, particularly 30.6 s / 100g, particularly 32.6 s / 100g, particularly 36.2 s / 100g, particularly 36.4 s / 100g.

[0145] In a preferred embodiment of the present invention, under the condition that the outlet size of the test funnel is 8 mm, the free flowability of the modified carbohydrate preparation obtained in step (d) is 10.0–20.0 s / 100g, particularly 12.0–18.0 s / 100g, particularly 14.0–16.0 s / 100g, particularly 12.6 s / 100g, particularly 14.7 s / 100g, particularly 14.8 s / 100g, particularly 15.0 s / 100g, particularly 15.1 s / 100g, particularly 17.4 s / 100g.

[0146] In a preferred embodiment of the present invention, under the condition that the outlet size of the test funnel is 10 mm, the free flowability of the modified carbohydrate preparation obtained in step (d) is 6.0–12.0 s / 100g, particularly 7.0–10.0 s / 100g, particularly 8.0–9.5 s / 100g, particularly 6.6 s / 100g, particularly 7.7 s / 100g, particularly 8.0 s / 100g, particularly 8.2 s / 100g, particularly 8.3 s / 100g, particularly 9.3 s / 100g, particularly 9.7 s / 100g.

[0147] In a preferred embodiment of the present invention, under the condition that the outlet size of the test funnel is 11.3 mm, the free flowability of the modified carbohydrate preparation obtained in step (d) is 3.5 to 7.0 s / 100g, particularly 5.0 to 6.0 s / 100g, particularly 4.1 s / 100g, particularly 5.0 s / 100g, particularly 5.3 s / 100g, particularly 5.4 s / 100g, particularly 6.1 s / 100g.

[0148] In a preferred embodiment of the present invention, under the condition that the outlet size of the test funnel is 15 mm, the free flowability of the modified carbohydrate preparation obtained in step (d) is 1.0 to 6.0 s / 100g, particularly 1.5 to 5.0 s / 100g, particularly 2.0 to 4.0 s / 100g, particularly 1.7 s / 100g, particularly 2.1 s / 100g, particularly 3.8 s / 100g, particularly 4.6 s / 100g.

[0149] In a preferred embodiment of the present invention, under the condition that the outlet size of the test funnel is 25 mm, the free flowability of the modified carbohydrate preparation obtained in step (d) is 0.0 to 4.0 s / 100 g, particularly 0.0 to 3.0 s / 100 g, particularly 0.1 s / 100 g, particularly 1.3 s / 100 g, particularly 2.5 s / 100 g.

[0150] In a preferred embodiment of the present invention, the total water content of the modified carbohydrate preparation obtained in step (d) is 0.1–6.00 g / 100 g, particularly 0.1–5.00 g / 100 g, particularly 0.1–0.5 g / 100 g, particularly 0.12–0.42 g / 100 g, particularly 0.2–0.42 g / 100 g, particularly 0.3–0.42 g / 100 g, particularly 0.12 g / 100 g, particularly 0.13 g / 100 g, particularly 0.27 g / 100 g, particularly 0.28 g / 100 g, particularly 0.29 g / 100 g, and particularly 0.42 g / 100 g. In particular, the total water content of the obtained carbohydrate preparation consists entirely of water of crystallization.

[0151] In a preferred embodiment of the present invention, the surface water content of the modified carbohydrate preparation obtained in step (d) is 0.050–0.100 g / 100 g, particularly 0.050–0.090 g / 100 g, particularly 0.060–0.080 g / 100 g, particularly 0.070–0.080 g / 100 g, particularly 0.054 g / 100 g, particularly 0.067 g / 100 g, particularly 0.076 g / 100 g, particularly 0.084 g / 100 g, and particularly none.

[0152] In a preferred embodiment of the present invention, a water-containing sucrose starting material, particularly sucrose, is obtained from sugarcane.

[0153] In a preferred embodiment of the present invention, a water-containing sucrose starting material, particularly sucrose, is obtained from sugar beets.

[0154] In a preferred embodiment of the present invention, the aqueous isomaltitol starting formulation contains 1,1-GPM (1-O-α-D-glucopyranosyl-D-mannitol) and 1,6-GPS (6-O-α-D-glucopyranosyl-D-sorbitol) in a content of 95.0-100.0 wt.% (based on the total dry mass of the aqueous isomaltitol starting formulation).

[0155] In a preferred embodiment of the present invention, the hydrated isomaltitol starting formulation contains 45.0 to 50.0 wt.% 1,1-GPM (1-O-α-D-glucopyranosyl-D-mannitol) and 50 to 55 wt.% 1,6-GPS (6-O-α-D-glucopyranosyl-D-sorbitol) (both based on the total dry weight of the hydrated isomaltitol starting formulation).

[0156] In a preferred embodiment of the present invention, the hydrated isomaltitol starting formulation contains 20.0 to 30.0 wt.% 1,1-GPM (1-O-α-D-glucopyranosyl-D-mannitol) and 70.0 to 80.0 wt.% 1,6-GPS (6-O-α-D-glucopyranosyl-D-sorbitol) (both based on the total dry mass of the hydrated isomaltitol starting formulation).

[0157] The aqueous isomaltitol starting formulation contains 1,1-GPS (1-O-α-D-glucopyranosyl-D-sorbitol), sorbitol, mannitol, or GPI, or a mixture of two or more of the above.

[0158] In a preferred embodiment of the present invention, the aqueous isomaltulose-containing trehalose-containing starting preparation comprises fructose, glucose, isomaltose or isomalutose or a mixture of two or more of the above.

[0159] In a preferred embodiment of the present invention, after step (c) or step (d), the dried carbohydrate preparation is packaged in step (x).

[0160] Within the scope of this invention, "water-containing crystalline carbohydrate starting preparation" refers to a carbohydrate starting preparation with a water content of 0.4–22.5 wt.%, particularly 2.5–12 wt.%, (based on the total weight of the carbohydrate starting preparation), wherein the carbohydrates are at least partially, preferably completely, in crystalline form, particularly in a form suspended in or encapsulated in an aqueous solution. In a preferred embodiment of the invention, the water-containing carbohydrate starting preparation may be in liquid form, particularly a suspension, or in a semi-liquid or solid form, particularly a solid form. In a particularly preferred embodiment, the carbohydrates in the water-containing crystalline carbohydrate starting preparation are solid crystalline carbohydrate crystals coated with a liquid film (also referred to as a syrup film within the scope of this invention). The syrup film is an aqueous solution or suspension of one or more carbohydrates in the starting preparation, present on the surface of the crystalline particles of the carbohydrate starting preparation, and may originate from previous steps in carbohydrate processing. Therefore, the water represented by the syrup film is not entirely present in the crystalline particles, but rather on the surface of the crystalline particles; in particular, the water in the syrup film is not water of crystallization. If water of crystallization is present in the carbohydrate, the syrup film represents an additional amount of water in the carbohydrate, i.e., extra water. Therefore, the hydrous crystalline carbohydrate starting formulation of the present invention contains an additional amount of water in the form of a liquid film, even when its carbohydrate (such as isomaltulitol, particularly its component 1,1-GPM or isomaltulose) contains water of crystallization. Thus, considering anhydrous carbohydrates (such as sucrose), the hydrous crystalline carbohydrate starting formulation of the present invention has a water content in the form of a liquid film.

[0161] The water content of the aqueous crystalline carbohydrate starting material is determined by subtracting the dry weight of the aqueous crystalline carbohydrate starting material from the total weight of the starting material (without considering any possible water of crystallization).

[0162] Given that carbohydrates are anhydrous, the hydration of the hydrated crystalline carbohydrate starting formulation of the present invention originates from the water in which the crystalline carbohydrate particles are located, particularly the water that encapsulates the crystalline carbohydrate particles, i.e., the liquid film.

[0163] In view of carbohydrates containing water of crystallization, the water content of the aqueous crystalline carbohydrate starting formulation of the present invention originates from the water in which the crystalline carbohydrate particles are located, especially the water that encapsulates the crystalline carbohydrate particles, i.e., the liquid film, and also from the water of crystallization.

[0164] Water of crystallization refers to water that forms crystalline solids at fixed lattice sites within a crystal structure. The stoichiometric water of crystallization content can be determined by X-ray structural analysis of the solid. The actual water of crystallization content of carbohydrates can be determined based on the difference between total water content and free water content. Total water content is measured by Karl Fischer titration, and the proportion of free water is measured by drying experiments.

[0165] The presence of a syrup film can also be detected, for example, by tests of free flowability, viscosity, and / or agglomeration, particularly according to the example method section, in which uncoated crystalline particles (particularly fully dried or over-dried crystalline particles) are compared with test crystalline particles that may have a syrup film, and the presence of a syrup film is detected by a significant decrease in free flowability, an increase in viscosity, and / or an enhanced tendency to agglomerate, particularly these three changes.

[0166] Over-dried crystal particles refer to crystal particles in which not only surface moisture is evaporated during the drying process, but also water of crystallization is removed from the crystal particles themselves.

[0167] Within the scope of this invention, "Dried Carbohydrate Preparation" refers to a carbohydrate preparation whose water content is reduced by at most 6.0 wt.%, particularly at most 5.0 wt.%, particularly at most 1.9 wt.%, particularly 0.01 to 0.7 wt.% (based on the total weight of the dry carbohydrate preparation) compared to an aqueous crystalline carbohydrate preparation. Preferably, the dried carbohydrate preparation contains no crystalline particles coated with a syrup film, and in particular, any remaining water content is only water of crystallization.

[0168] Within the scope of this invention, "carbohydrate particle" refers to at least one solid granular carbohydrate. Preferably, the carbohydrate particle is in powder form. In particular, the carbohydrate particle is in crystalline form.

[0169] Within the scope of this invention, "semi-crystalline" refers to a material structure that has both ordered crystalline regions and disordered amorphous regions.

[0170] Within the scope of this invention, "amorphous" refers to a material structure in which the building units (especially molecules or atoms) are not arranged in a long-range ordered structure. Preferably, the building units (especially molecules) of amorphous matter form irregular patterns and exhibit short-range order. More preferably, amorphous matter is short-range ordered but long-range disordered.

[0171] Within the scope of this invention, "long-range order" refers to the periodic and regular arrangement of building blocks (particularly molecules or atoms) of a substance outside of its nearest neighbor building blocks (particularly neighboring molecules or atoms). Therefore, the positions of all building blocks (particularly molecules or atoms) in a crystalline substance can be advantageously determined based on the precise positions of a few building blocks (particularly molecules or atoms). According to the invention, preferably, the crystalline substance exhibits at least partial long-range order.

[0172] Within the scope of this invention, "short-range order" refers to the regular grouping of only the nearest neighbor building units (especially molecules or atoms) of a reference building unit (especially a reference molecule or a reference atom). Preferably, short-range order refers to nearest neighbor.

[0173] Within the scope of this invention, "fully crystalline" refers to a material structure in which building blocks (especially molecules or atoms) are regularly arranged in a crystal structure. Preferably, fully crystalline materials exhibit both short-range and long-range order.

[0174] Within the scope of this invention, "powdered" refers to the solid particulate state of a substance.

[0175] Within the scope of this invention, "Angle of Repose" refers to the angle between the inclined surface of the powder cone and the bottom plane. Preferably, the angle of repose is calculated according to the following formula based on the height h of the powder cone, the radius r of the cone, and tanα: tanα=h / r (1).

[0176] Within the scope of this invention, the term "free-flowability" refers to the degree of free flow of a powder or agglomerate. Preferably, free-flowability is determined, for example, using a measuring funnel or a free-flowability tester, wherein the free-flow time is measured for a given mass or volume.

[0177] In particular, “free flow” was measured according to Methods 2.9.16, “Flowability”, of EUROPEAN PHARMACOPOEIA 10.0 (10th edition).

[0178] Within the scope of this invention, the term "viscosity" refers to the properties of a solid carbohydrate formulation as determined by the viscosity test method according to the Example Methods section. This viscosity can be assessed as a measure of the adhesion of the syrup film to the particle surface, and thus as the strength of the interparticle liquid bridge.

[0179] Within the scope of this invention, the term "caking" refers to a substance that was originally free-flowing but has at least partially or completely solidified during storage. Preferably, this solidification is visually perceptible as a caking formation. Within the scope of this invention, caking properties are determined according to the test methods described in the Example Methods section.

[0180] Within the scope of this invention, the term "carbohydrate" (hereinafter also referred to as sugars) shall refer to sugars and / or sugar alcohols in monomeric, dimeric, and polymeric forms. Preferably, "sugar" shall refer to monosaccharides or disaccharides, particularly glucose, fructose, isomaltulose, trehalose, and / or sucrose.

[0181] Within the scope of this invention, "sugar alcohol" should refer to monosaccharide alcohols or disaccharide alcohols, especially isomaltitol, mannitol and sorbitol.

[0182] Within the scope of this invention, if a pressure value is given, it should be expressed as absolute pressure rather than relative pressure to atmospheric pressure. Negative pressure refers to pressure below the dominant atmospheric pressure (1 bar). Vacuum specifically refers to negative pressure. Overpressure refers to pressure above the dominant atmospheric pressure (1 bar).

[0183] Within the scope of this invention, "invert sugar syrup" refers to an aqueous solution of sucrose partially converted through hydrolysis, having a certain dry matter content and a certain proportion of dry matter invert sugar. The dry matter content of the invert sugar syrup is particularly 60%–70%, particularly 65 ± 0.5% (refractive index method), the invert sugar content (i.e., the total content of glucose and fructose) is 95%–99% (HPLC), the glucose content is 47%–50% (HPLC), the fructose content is 47%–50% (HPLC), and the sucrose content is 1%–5% (HPLC).

[0184] Within the scope of this invention, "caramel sugar syrup" refers to a dark brown aqueous solution of carbohydrates and caramel substances prepared by controlled heating based on sugar. Preferably, the caramel syrup has a dry matter content of 70%–80%, particularly 75 ± 0.5% (refractive index), a glucose content of 5%–8% (HPLC), a fructose content of 1%–4% (HPLC), and a sucrose content of 0%–3% (HPLC).

[0185] Within the scope of this invention, "cane sugar syrup" refers to sucrose syrup made from cane sugar, preferably having a dry matter content of 70% to 80%, particularly 75 ± 0.5% (refractive index), a glucose content of 32% to 38% (HPLC), a fructose content of 25% to 30% (HPLC), and a sucrose content (cane sugar) of 10% to 15% (HPLC).

[0186] Within the scope of this invention, the term "Substance X in Form of Y" should refer to substance X as a component of composition Y, that is, X coexists with other unspecified components of Y.

[0187] Within the scope of this invention, the term "minor component" refers to all substances in a carbohydrate preparation that are not selected from monosaccharides or disaccharides of glucose, fructose, isomaltulose, trehalose, isomaltulitol, and sucrose.

[0188] Within the scope of this invention, "individual minor component" refers to a single substance that constitutes the minor component as a whole. These single substances (e.g., isomaltose, glycerol, glucopyranoside, isopyrithiose) are all substances belonging to the groups of monosaccharides, disaccharides, deoxydiols, trisaccharides, glucosylglycerol, glucosylbutanetriol, glucosylpentanetetrol, trisaccharides, glucosyldiol, or hydrogenated oligomers.

[0189] Within the scope of this invention, "isomalt" should refer to 6-O-α-D-glucopyranosyl-D-sorbitol (1,6-GPS) and 1-O-α-D-glucopyranosyl-D-mannitol (1,1-GPM), and optionally 1-O-α-D-glucopyranosyl-D-sorbitol (1,1-GPS), particularly GS type isomalt or ST type isomalt.

[0190] Within the scope of this invention, "GS-type isomalt GS" refers to a mixture of 72-78 wt.%, preferably 75 wt.%, of 1,6-GPS and 22-28 wt.%, particularly 25 wt.%, of 1,1-GPM (all based on the dry matter content of isomalt). Specifically, the GS-type isomalt contains 20.0-30.0 wt.% of 1,1-GPM (1-O-α-D-glucopyranosyl-D-mannitol) and 70.0-80.0 wt.% of 1,6-GPS (6-O-α-D-glucopyranosyl-D-sorbitol) (all based on the total dry mass of isomalt).

[0191] Within the scope of this invention, "ST-type isomalt (Isomalt ST)" refers to a mixture of 54–47 wt.% 1,6-GPS and 46–53 wt.% 1,1-GPM (both based on the dry weight of isomalt). Specifically, the ST-type isomalt contains 45.0–50.0 wt.% 1,1-GPM (1-O-α-D-glucopyranosyl-D-mannitol) and 50–55 wt.% 1,6-GPS (6-O-α-D-glucopyranosyl-D-sorbitol) (both based on the total dry weight of isomalt).

[0192] Within the scope of this invention, the term "isomalt" or "hydrogenated isomaltulose" preferably refers to a mixture comprising 1,1-GPM and 1,6-GPS or thereof, particularly a mixture comprising 35 to 61 wt.% of 1,1-GPM and 65 to 39 wt.% of 1,6-GPS, and especially an equimolar or near-equimolar mixture comprising 1,1-GPM and 1,6-GPS or thereof (all based on the dry matter content of isomalt).

[0193] Therefore, isomaltitol can also refer to a mixture containing 1,1-GPM and 1,6-GPS or composed thereof, wherein the molar ratio of 1,1-GPM to 1,6-GPS is not equal, but rather the content of 1,1-GPM is higher than the content of 1.6-GPM or the content of 1.6-GPM is higher than the content of 1,1-GPM.

[0194] In a preferred embodiment, isomalt contains no other components besides 1,1-GPM and 1,6-GPS.

[0195] In a preferred embodiment, isomaltulitol contains one or more other components besides 1,1-GPM and 1,6-GPS, such as mannitol, sorbitol, sucrose, 1,1-GPS (1-O-α-D-glucopyranosyl-D-sorbitol), glycosides, deoxydiols, GPI (glucopyranosyl-idutitol), isomaltose, isomaltulose, isomalutose, hydrogenated or non-hydrogenated oligosaccharides (especially hydrogenated or non-hydrogenated trisaccharides), and / or other substances.

[0196] Within the scope of this invention, "Isomaltulose-and-trehalulose-Containing Mixture" refers to a mixture containing isomaltulose and trehalulose, particularly obtained by enzymatically reacting sucrose with sucrase to form a mixture of sucrose isomers containing isomaltulose and trehalulose, and optionally containing one or more other substances selected from sucrose, fructose, glucose, melinothiose, Leuconostibhiose, isomaltose, melitriose, isomalthiose, 6-glycoside isomaltulitol, and 1-glycoside isomaltulitol.

[0197] Within the scope of this invention, the solubility of carbohydrates is determined in water (especially distilled water) at 20°C.

[0198] Within the scope of this invention, "poorly-soluble carbohydrate" refers to carbohydrates with a solubility of at most 53 g / 100 g (grams of dry matter per 100 g of solution) in pure water, particularly distilled water, at 20°C. Poorly-soluble carbohydrates include, in particular, isomaltulose, glucose, mannitol, and 1,1-GPM.

[0199] Within the scope of this invention, "well-soluble carbohydrate" refers to carbohydrates with a solubility greater than 53 g / 100 g, particularly at least 66.7 g / 100 g, particularly at least 68.7 g / 100 g, particularly at least 70.0 g / 100 g, particularly at least 78.9 g / 100 g (grams of dry matter per 100 g of solution), in pure water, particularly distilled water, at 20°C. Well-soluble carbohydrates particularly include sucrose, 1,6-GPS, fructose, trehalose, and sorbitol.

[0200] Within the scope of this invention, the diameter of carbohydrate particles is determined by air jet sieve analysis using a sieve with a mesh size of 100 μm.

[0201] The quantitative proportion of particles with a diameter less than or equal to 100 μm is calculated by dividing the proportion of particles passing through a 100 μm sieve in the air jet sieve analysis by the weight.

[0202] Within the scope of this invention, sucrose-containing starting materials derived from sugarcane or sugar beets, while similar, differ even among purified or highly purified sucrose-containing starting materials with a sucrose content exceeding 99.8 wt.%. In particular, these preparations differ in their aroma characteristics, applicability (e.g., solubility), thermal behavior (often accompanied by plant-specific impurities), and sensory properties (see Lu et al., *Journal of Food Engineering*, 2017, Vol. 214, pp. 193-208). This is especially true because sugarcane belongs to the Poaceae family (C4), while sugar beets belong to the Chenopodiaceae family (C3), exhibiting significant physiological and morphological differences. It is particularly well known that sucrose molecules derived from C4 plants differ from those derived from C3 plants (e.g., sugar beets) because… 13 C / 12 Metabolic isotope fractionation due to different C isotope ratios (see Martin et al., *Journal of Science of Food and Agriculture*, 1991, Vol. 56, pp. 419-435). In particular, through... 12 C and 13 C4 isotope determination can distinguish sucrose-containing starting materials derived from C4 plants from those derived from C3 plants. Due to isotopic fractionation, the sucrose-containing starting materials from C3 plants... 13 C / 12 The C isotope ratio is lower in C4 plants 13 C / 12 C isotope ratio.

[0203] In particular, referring to Averill et al.'s *Journal of Thermal Analysis and Calorimetry*, 2019, Vol. 127, pp. 513-538, even with a sucrose purity exceeding 99.8 wt.%, crystalline sucrose derived from sugarcane and crystalline sucrose derived from sugar beets exhibit different thermal behaviors. In some cases, sucrose formulations obtained from sugarcane are characterized by a detectable small signal below the main signal temperature (approximately 185°C–190°C) in Differential Scanning Calorimetry (DSC) measurements. In contrast, commercially available sucrose formulations derived from sugar beets do not exhibit this melting phenomenon, and DSC measurements only show a main signal in the range of 185°C to 190°C (see patent document US 8,273,873B2).

[0204] In principle, the differences between sucrose preparations derived from these different plant varieties can be explained by the metabolism of the plant varieties themselves, the purification processes used for sucrose preparations, and the plant-specific impurities that often remain in the resulting sucrose preparations, such as residual syrup and solids adhering to sucrose crystals. Therefore, preparations containing cane sucrose (especially all of its sucrose molecules) are different from preparations containing beet sucrose (especially all of its sucrose molecules).

[0205] Within the scope of this invention, "wt.%" represents weight percentage, "GC" represents gas chromatography, "HPLC" represents high performance liquid chromatography, "Lfd.No." represents serial number, and "KF" represents Karl Fischer titration.

[0206] Within the scope of this invention, the Karl Fischer titration method is used to determine the water content.

[0207] If the context of this invention explicitly or implicitly states that a certain component "exists," "comprises," "has," or "contains" is present, it means that the corresponding component is present, and in particular, the amount present is measurable.

[0208] If the context of this invention explicitly or implicitly indicates that a certain component is "present", "comprising" or "containing" in an amount of 0 [unit], particularly mg / kg, μg / kg or wt.%, it means that the corresponding component is not present within the measurable range, especially that the corresponding component is completely absent.

[0209] If the context of this invention specifies quantitative information (especially percentages) of certain components of a product or composition, such information, together with other components of the composition or product that are expressly indicated or understood by those skilled in the art, constitutes 100% of the composition and / or product, unless otherwise expressly stated or denied by those skilled in the art.

[0210] Within the scope of this invention, the term "at least one" refers to a number of 1, 2, 3, 4, 5, 6, 7, 8, 9, or 10. In a particularly preferred embodiment, the term "at least one" may precisely indicate a number of 1. In a more preferred embodiment, the term "at least one" may also refer to 2, 3, 4, 5, 6, or 7.

[0211] Specify the number of decimal places corresponding to the precision of the measurement method used.

[0212] Within the scope of this invention, if a number specifies a first or second decimal place or a second decimal place, then that decimal place is set to zero.

[0213] Within the scope of this invention, the term "and / or" shall mean that all members of a group connected by the term "and / or" are either interchangeable or can be arbitrarily combined with each other. The expression "A, B and / or C" shall be understood as: (a) A or B or C; or (b) A and B; or (c) A and C; or (d) B and C; or (e) A and B and C.

[0214] Within the scope of this invention, the terms "comprising" and "having" shall refer to elements other than those explicitly covered by the terms, which may also include elements not explicitly stated. Within the scope of this invention, these terms may also refer to elements that only include the explicitly stated elements and do not include other elements. In this particular embodiment, the terms "comprising" and "having" are synonymous with the term "consisting of". Additionally, the terms "comprising" and "having" also cover compositions that include, in addition to the explicitly stated elements, other elements that are functionally and qualitatively dependent, though not mentioned. In embodiments of this invention, the terms "comprising" and "having" are synonymous with the term "substantially consisting of".

[0215] For more advantageous technical solutions, please refer to the dependent claims. Detailed Implementation

[0216] The present invention will be described in detail below with reference to examples, but this does not limit the overall concept of the invention.

[0217] Example

[0218] Examples 1 and 2 illustrate the composition of the starting materials.

[0219] Unless otherwise stated, all sucrose is derived from sugar beets (sucrose syrup).

[0220] sucrose:

[0221] • Sucrose: Minimum 99.7°Z (polarization)

[0222] • Invert sugar syrup: <0.04% (enzymatic)

[0223] Humidity: <0.06% (KF)

[0224] Invert sugar:

[0225] • Dry matter content: 65±0.5% (refractive index)

[0226] • Invert sugar content: 95%–99% (HPLC)

[0227] glucose content: 47%–50% (HPLC)

[0228] Fructose content: 47%–50% (HPLC)

[0229] Sucrose content: 1%–5% (HPLC)

[0230] Caramel syrup:

[0231] • Dry matter content: 75±0.5% (refractive index)

[0232] • Glucose content: 5%–8% (HPLC)

[0233] • Fructose content: 1%–4% (HPLC)

[0234] • Sucrose content: 0%–3% (HPLC)

[0235] Cane syrup (cane sugar):

[0236] • Dry matter content: 75±0.5% (refractive index)

[0237] • Glucose content: 32%–38% (HPLC)

[0238] • Fructose content: 25%–30% (HPLC)

[0239] • Sucrose content: 10%–15% (HPLC)

[0240] Instance Methods Section - Test Process Description

[0241] Free flow test:

[0242] EUROPEAN PHARMACOPOEIA 10.0 (10th edition of the European Pharmacopoeia) Methods 2.9.16 "Flowability" (abbreviated Ph.Eur.2.9.16) is used to determine free flow.

[0243] Viscosity test:

[0244] Viscosity was determined according to the following literature: Endress and Mattes, *Handbook of Food Science*, CRC Press, December 19, 2005, Volume 3, Chapter 140; Uhlenbrock, *Gordian*, Volume 83, pp. 148-150 (1983); Endress and Dilger, *Food Technology International Europe*, pp. 279-282 (1990); Schilling et al., *Eur Food Res Technol* (2008), 226:1389-1398; Sirisakulwat et al., *International Journal of Food Science and Technology*, 20210, 45, 1647-1658; Zedler, *Dieindustrielle Obst- und "Gemüseverwertung (Industrial Fruit and Vegetable Applications)" Volume 68, Chapter 12 / 83, pp. 523-527; Endreβ et al., "Intern. Zeitschrift für Lebensmittelt-Technologie und-Verfahrenstechnik (International Journal of Food Technology and Processing Engineering)" Volume 38, Issue 5 (1987).

[0245] The gel breaking strength is assessed based on the tensile force that the gel must withstand when a standardized so-called "tear pattern" is inserted into it. This test uses a test cup and a test cup insert (i.e., the tear pattern), with the tear pattern placed in a standard plastic cup.

[0246] SAP product numbers are: Herbstreith Pectinometer MarkIV-901172; Test Cup-900054; Tear Map-901173.

[0247] Place 100 grams of the sample to be tested into an HPE beaker. Gently tap the beaker three times to slightly compact the sample, then let it stand for one hour. Then use a texture analyzer (Winopal) to pull a tear pattern from the sample and determine the required tensile strength.

[0248] This tensile force can be used to measure the strength of a material, thereby measuring the strength of the interactions between crystals.

[0249] Clumping test:

[0250] Each sample was filled to two-thirds capacity using three metal crucibles. A layer of plastic film was then placed on the sample surface, and the surface was compacted using a stamp (7000 Pa weight). The samples were stored in a constant temperature chamber at 25°C and 65% relative humidity for one week. After storage, the stamp and plastic film were carefully removed before measuring the samples.

[0251] To measure the puncture force, a metal needle of a specific geometry is inserted into the sample surface, and the puncture force is recorded along the puncture path. This process is repeated five times for each sample at each untouched point. The required immersion force is an indicator of the sample's compaction or viscosity.

[0252] The measuring instrument used was the AT-XT Plus ExtendedHeight from Stable Micro Systems.

[0253] Example 1: The method for preparing dried and modulated carbohydrate preparations (samples 2 to 4) and a control sample (sample 1) without adding carbohydrate particles according to the present invention.

[0254] The following description uses the sample weight of test 2 in Table 1 as an example to illustrate the process. The following description applies accordingly to the samples of the present invention in tests 3 and 4 in Table 1. Sample 1 represents the control sample without added fine sucrose.

[0255] To prepare a hydrous crystalline carbohydrate starting material, 922.0 g of sucrose (Südzucker EU2 quality, medium particle size) in granulated form was placed in a coating pan used as a drying reactor. 60 g of caramel syrup (component B) and 18 g of cane sugar syrup (component C) were mixed in a heated stirring vessel and heated to approximately (hereinafter “about”) 60°C. The resulting heated syrup mixture was slowly added to the sucrose in the rotating coating pan (step (a1)). The resulting mixture was homogenized for approximately 5 minutes to obtain the hydrous crystalline carbohydrate starting material according to step (a) of the present invention, wherein the crystalline sucrose particles are coated with a syrup film. For samples 2 through 4, according to step (b) of the present invention, the amount of fine sucrose specified in Table 4 (at least 80 wt.% crystals with a diameter less than 100 μm and at least 70 wt.% crystals with a diameter less than 32 μm) was metered into the aqueous crystalline carbohydrate starting formulation at a temperature of 21–22 °C through a vibrating bath at a temperature of 20 °C under an atmospheric pressure of approximately 1000 mbar. In test 1, the metering of fine sucrose was omitted. According to step (c) of the present invention, the mixture was homogenized for 5 minutes at a temperature of 20–21 °C under an atmospheric pressure of approximately 1000 mbar until the distribution of carbohydrate particles was visually identifiable. The dried carbohydrate formulation compositions listed in Tables 5 and 6 can be obtained according to the method of the present invention. During preparation according to step (d) of the present invention, ambient air preheated to approximately 90 °C was blown through the dried carbohydrate formulation using a blower. The temperature of the dried carbohydrate formulation reached approximately 50 °C. When the mixture becomes extremely free-flowing and no longer has any lumps, the dried and prepared carbohydrate formulation is obtained (Table 7). Turn off the blower heating and blow ambient air at room temperature through the dried and prepared carbohydrate formulation until its temperature reaches below 35°C.

[0256] Control sample 1 served as the control group. Since no fine sucrose was added, a free-flowing product was not obtained during the warm air conditioning test; instead, a very viscous substance was obtained. This product could not withstand further testing or measurement (see Tables 7 and 8, n / a indicates unmeasurable).

[0257] Tables 1 to 7 below list the characteristics of the dried and modified carbohydrate formulations obtained by the method of the present invention, and Table 8 lists the test results of the free flowability and angle of repose of various modified carbohydrate formulations. The modified carbohydrate formulations of the present invention exhibit excellent angle of repose and excellent free flowability.

[0258] Table 1: Starting material amounts for preparing sucrose preparations containing water of crystallization

[0259]

[0260] Table 2: Composition of Sucrose Preparations Containing Water of Crystallization

[0261]

[0262] Table 3: Dry matter composition of sucrose preparations containing water of crystallization

[0263]

[0264]

[0265] Table 4: Starting material amounts for preparing dried carbohydrate preparations and control sample No. 1

[0266]

[0267] Table 5: Composition of dried carbohydrate preparations and control sample No. 1

[0268]

[0269] Table 6: Total Dry Matter Composition of Dried Carbohydrate Preparations and Control Sample No. 1

[0270]

[0271] Table 7: Composition of dried and prepared carbohydrate preparations and control sample No. 1

[0272]

[0273]

[0274] n / a: Unmeasurable

[0275] Table 8: Free flow (f.-flow.) and angle of repose (ang.) of dried and prepared carbohydrate formulations and control sample 1.

[0276]

[0277] n / a: Unmeasurable

[0278] Example 2: Comparison of the carbohydrate preparation (Type A brown sugar) obtained according to the present invention (samples 2 to 9) with the control sample (sample 1) without added carbohydrate particles.

[0279] The preparation of the carbohydrate formulation and control sample 1 obtained according to the present invention is similar to that in Example 1. Tables 9 to 15 show the characteristics of control sample 1 (without the addition of fine sucrose, i.e., without process steps (b) and (c)), the dried products prepared according to the present invention (samples 2 to 5), and the dried and modified products prepared according to the present invention (samples 6 to 9).

[0280] Samples should be characterized and compared as much as possible based on total moisture content (KF method) and surface moisture content (KF method), angle of repose, and free flowability. The sugar powder (fine crystalline sucrose) used corresponds to the crystalline sucrose according to Example 1.

[0281] Table 16 summarizes the experimental results. As can be seen from the table, compared to the control example (sample 1, with 0 wt.% carbohydrate particles in the form of fine sucrose), the dried type A brown sugar samples (samples 2 to 5) exhibited significantly increased free flowability by increasing the amount of fine sucrose added from 2 wt.% to 20 wt.% (based on the initial weight of the type A brown sugar sample). For example, Table 16 particularly shows that the measurement time required using the sample of the present invention is significantly reduced compared to using sample 1, especially when the outlet size is 15 mm. Control sample 1 exhibited completely unmeasurable free flowability at an outlet size smaller than 15 mm (n / a in Table 16), while the sample of the present invention, unlike the control sample, showed good free flowability even at a smaller outlet size.

[0282] The results showed that with the increase of the amount of fine-crystalline carbohydrate particles added, the required time decreased from 2.3 seconds (Control Example 1, with 0 wt.% fine-crystalline carbohydrate particles) to 0.2 seconds (Sample 5, with 20 wt.% fine-crystalline carbohydrate particles), i.e., the free flowability was 25 mm. Furthermore, with the increase of the amount of fine-crystalline carbohydrate particles added, both the total water content and the surface water content of the dried samples decreased.

[0283] In addition to steps (b) and (c) of the present invention, samples 6 to 9 also underwent a subsequent conditioning step (d), as described in Example 1. The resulting dried and conditioned formulations exhibited nearly identical behavior to samples 2 to 5, with samples 6 to 9 showing better free flowability and lower total and surface water content compared to samples 2 to 5 when equal amounts of fine-crystalline carbohydrate particles were added, particularly at low amounts (2% and 5%). Samples 6 and 7 showed better free flowability and lower total and surface water content compared to samples 2 and 3. The water content of samples 8 and 9, after drying and conditioning with the addition of 10% fine-crystalline carbohydrate particles, did not decrease further. For the dried and conditioned samples, it was also observed that the angle of repose decreased with increasing amounts of fine-crystalline carbohydrate particles, indicating increased free flowability. In this example, the control sample (sample 1) also underwent a conditioning step. The result was a very soft and viscous product, making it impossible to measure its free flowability.

[0284] Table 9: Starting material amounts for preparing sucrose preparations containing water of crystallization

[0285]

[0286] Table 10: Composition of sucrose preparations containing water of crystallization as shown in Table 9

[0287]

[0288] Table 11: Total dry matter composition of aqueous carbohydrate preparations shown in Table 10

[0289]

[0290]

[0291] Table 12: Starting material amounts for preparing dried crystalline carbohydrate preparations and control sample No. 1

[0292]

[0293] Table 13: Composition of dried carbohydrate preparations No. 2 to No. 9 (samples No. 6 to No. 9 before preparation according to process step (d)) and control sample No. 1 as shown in Table 12

[0294]

[0295]

[0296] Table 14: Total Dry Matter Composition of Carbohydrate Preparations as Shown in Table 13

[0297]

[0298] Table 15: Composition of dried carbohydrate preparations (No. 2 to No. 5), dried and modified carbohydrate preparations (No. 6 to No. 9), and control sample No. 1.

[0299]

[0300] Table 16: Angle of repose, free flowability, water content, and surface water content of various Type A brown sugar samples (control example without added sugar powder (control sample 1) and the dried carbohydrate preparations of the present invention (samples 2 to 5) or the dried and prepared carbohydrate preparations of the present invention (samples 6 to 9)).

[0301]

[0302]

[0303] Example 3: A method for preparing a dried and modulated isomaltulose- and trehalose-containing composition and a control sample without added carbohydrate particles according to the present invention.

[0304] The following describes the preparation of a dried isomaltulose-containing and trehalose-containing formulation from an aqueous crystalline isomaltulose-containing and trehalose-containing starting formulation according to the present invention, and illustrates its free flow and viscosity characteristics.

[0305] First, the starting material of this invention (i.e., the aqueous crystalline carbohydrate starting agent) is prepared from a solid crystalline agent containing isomaltulose and trehalose (hereinafter also referred to as the "crystalline agent") and an aqueous syrup to be coated with the isomaltulose and trehalose agent, thereby forming carbohydrate particles coated with a syrup film. This preparation step provides the starting material for the method of this invention, provides the starting product in this example in a standardized manner, and forms a product as produced in industrial production, which is further processed in a subsequent industrial drying step. Then, according to the invention, steps (b) and (c) (addition of powder) are performed, the obtained syrup-coated particles are dried and then optionally modified.

[0306] Table 17: Glycosylation of solid crystalline preparations containing isomaltulose and trehalose analyzed by gas chromatography (GC-DB5-OTMS)

[0307]

[0308] Trehalose can be abbreviated as "Trehalu".

[0309] The Type I and Type II powders of the isomaltulose- and trehalose-containing solid crystalline preparations have the same composition as the crystalline preparations shown in Table 17 above, but differ in particle size. Type I powder has at least 90 wt.% particles smaller than 0.05 mm. Type II powder has at least 90 wt.% particles smaller than 0.1 mm.

[0310] Table 18: Syrup analysis of isomaltulose- and trehalose-containing preparations (based on GC (HPLC-NH2) glycosylation composition)

[0311]

[0312] No powder was added during preparation (control group):

[0313] Place 1 kg of isomaltulose- and trehalose-containing crystallizing agent into a 3-liter mixer equipped with a flat mixer. Spray an appropriate amount of the aqueous syrup containing isomaltulose- and trehalose-containing agent onto the crystallizing agent in small, slow applications at specified intervals. Then, mix for approximately 5 minutes to ensure even distribution of the syrup. After mixing, use hot air to adjust the mixture. The clump temperature should be approximately 35°C.

[0314] Add powder (according to the present invention):

[0315] One kilogram of isomaltulose- and trehalose-containing crystalline preparation is placed in a 3-liter mixer equipped with a flat mixer. An appropriate amount of aqueous syrup containing isomaltulose- and trehalose-containing preparation is slowly sprayed onto the isomaltulose- and trehalose-containing crystalline preparation in small portions at specified intervals. The mixture is then stirred for approximately 5 minutes to ensure uniform distribution of the syrup. After addition, at atmospheric pressure and room temperature of 21–22°C, fine crystals (powder) of isomaltulose- and trehalose-containing preparation are added to the agglomerate using a metering device. According to step (c) of the present invention, the mixture is homogenized for 5 minutes at approximately 1000 mbar atmospheric pressure and a temperature of 20–21°C until the distribution of carbohydrate particles is visually identifiable.

[0316] A dried carbohydrate formulation composition can be obtained according to the method of the present invention. The mixture is then prepared with hot air. The agglomerate temperature is approximately 35°C.

[0317] In the first series of experiments, the solid crystalline formulation containing isomaltulose and trehalose was treated with 2.0 wt.% and 9.6 wt.% of type A syrup containing isomaltulose and trehalose (based on the total weight of the starting formulation coated with syrup), and then coated with 4.6 wt.% of type I or type II fine crystalline powder containing isomaltulose and trehalose (based on the total weight of the starting formulation coated with syrup, including the powder weight).

[0318] Table 19: First Series of Tests

[0319] g g g g 1 1000 20 0 0 2 1000 106 0 0 3 1000 106 53 0 4 1000 106 0 53

[0320] In the second series of experiments, the solid crystalline formulation containing isomaltulose and trehalose was treated with 2.0 wt.% or 4.8 wt.% type A syrup (based on the total weight of the starting formulation coated with syrup), and then coated with 4.8 wt.% type I or type II fine crystalline powder (based on the total weight of the starting formulation coated with syrup, including the powder weight).

[0321] Table 20: Second Series of Tests

[0322] g g g g 1 1000 20 0 0 5 1000 50 0 0 6 1000 50 0 53 7 1000 50 53 0

[0323] Free flow degree:

[0324] Table 21 summarizes the results of the first series of experiments. In experiments 1 and 2, the free-flow time measured in a 15 mm nozzle increased from the crystalline formulation (control group) to the two syrup-coated aqueous starting formulations. In experiments 3 and 4, the free-flow time decreased again when using the Type I and Type II fine-grained powders of this invention.

[0325] Table 21: Analytical Results of the First Series of Test Products

[0326]

[0327] chronom. refers to the chronometric method, s / 100g: the number of seconds it takes for 100 grams to drip; titrim. refers to the titration method, g / 100g: the number of grams of water per 100 grams.

[0328] The results of the second series of experiments were similar. Table 22 summarizes the results of the second series of experiments. In experiments 1 and 5, the free-flow time increased from the crystalline formulation (control group) to the two aqueous starting formulations containing syrup. In experiments 5 and 6, the free-flow time decreased again when using the Type I and Type II fine-grained powders of this invention.

[0329] Table 22: Analytical Results of the Second Series of Test Products

[0330]

[0331] Viscosity measurement:

[0332] Viscosities were determined for three selected samples: a crystalline preparation containing isomaltulose and trehalose before syrup treatment (Test 1), an aqueous crystalline starting preparation containing isomaltulose and trehalose encapsulated in syrup (Test 2), and an aqueous crystalline starting preparation containing isomaltulose and trehalose encapsulated in syrup. The crystalline preparation was then treated with and dried according to the present invention using a powder of the crystalline preparation containing isomaltulose and trehalose (Test 3).

[0333] The measurements in Table 23 show that the crystalline preparation has the lowest viscosity, with a force value of 84.5 g. Treatment with syrup (Test 2) resulted in a significantly higher force value, indicating a significantly higher viscosity. Treatment of these samples with Type I microcrystalline powder according to the present invention (Test 3) resulted in a significant decrease in viscosity.

[0334] Table 23: Viscosity of Selected Samples

[0335] Crystallization preparations 84.5 2 132.4 3 109.1

[0336] Clumping test:

[0337] Agglomeration tests were performed on the samples according to viscosity tests No. 1 through No. 3. Agglomeration tests can be used to determine the tendency of a material to agglomerate after compaction. Measurements were taken before further storage and immediately after one week of storage. The agglomeration tendency of particulate materials depends on the viscosity of individual particles.

[0338] The measurements taken from samples that were never stored showed almost no significant difference and are therefore not listed. Table 24 shows the measurements taken one week later. The crystalline formulation (Test 1) exhibited an extremely low force value of only 0.26 N. According to Test 2, the aqueous starting formulation coated with syrup showed a significantly increased force value, reaching 6.33 N. In Test 3, after powder treatment, this value decreased significantly to 1.50 N.

[0339] Table 24: Agglomeration of Selected Samples

[0340] Crystallization preparations 0.26 2 6.33 3 1.50

[0341] The experimental results show that by applying a finely crystalline formulation (powder) containing isomaltulose and trehalose, an aqueous starting formulation containing isomaltulose and trehalose can be prepared by coating an isomaltulose and trehalose syrup with a crystalline formulation containing isomaltulose and trehalose. This process improves free flowability, particularly viscosity and agglomeration tendency. Surprisingly, no agglomeration or clumping occurred, while free flowability was significantly improved.

[0342] Example 4: A method for preparing a dried and modulated isomaltitol-containing composition and a control sample without added carbohydrate particles according to the present invention.

[0343] The following describes the preparation of a dried isomaltitol formulation from an aqueous crystalline isomaltitol starting material according to the present invention, and illustrates its free flow and viscosity characteristics.

[0344] Characterization of starting materials:

[0345] Type I crystalline isomaltitol (at least 90% of crystals have a diameter of 0.8–1.5 mm);

[0346] Isomaltulitol solution (syrup);

[0347] Type I isomaltitol powder (at least 90% of crystals have a diameter of less than 0.1 mm) (powder).

[0348] To prepare the aqueous crystalline isomaltitol starting material used in step (a), type I solid crystalline isomaltitol (hereinafter also referred to as the "crystallization preparation") is first coated with an isomaltitol solution to form carbohydrate particles coated with a syrup film. This preparation step provides the starting material for the method of the present invention, provides the starting product in this example in a standardized manner, and forms a product as produced in industrial production, which is further processed in a subsequent industrial drying step. Then, according to the present invention, steps (b) and (c) (addition of powder) are performed to dry these syrup-coated particles, which are then optionally formulated.

[0349] Test without added powder (control group):

[0350] Place 1 kg of crystalline isomalt in a 5 L coating pan. Rotate the coating pan at approximately 21 rpm. Slowly spray small amounts of isomalt solution onto the isomalt at specified time intervals. Between sprays, briefly dry the mixture with hot air to obtain a crystalline aqueous isomalt starter formulation in which isomalt crystals are coated with a syrupy film. After adding the isomalt solution, heat the mixture with hot air for approximately 10 minutes. The agglomerate temperature should be approximately 45°C. Sieve the mixture to remove any agglomerates that may be present.

[0351] Powder addition test (according to the present invention):

[0352] 1 kg of isomalt is placed in a 5 L coating pan. The coating pan is rotated at approximately 21 rpm. A suitable amount of isomalt solution is slowly sprayed onto the isomalt at specified time intervals. Between sprays, the mixture is briefly dried with hot air to obtain a crystalline hydrous isomalt starting formulation, wherein the isomalt crystals are coated with a syrup film. After addition, at atmospheric pressure and room temperature of 21–22°C, 4.6 wt.% (based on the total weight of the syrup-coated starting formulation, including the powder) of the fine-crystalline isomalt component (Type I powder) is added to the agglomerate using a metering device. According to step (c) of the present invention, the mixture is homogenized for 5 minutes at approximately 1000 mbar atmospheric pressure and a temperature of 20–21°C until the distribution of carbohydrate particles is visually identifiable. After addition, the dried isomalt preparation obtained according to the present invention is prepared with hot air for approximately 10 minutes. The agglomerate temperature is approximately 45°C. The mixture is sieved to remove any agglomerates that may be present.

[0353] Table 25: Trial Overview and Formulation Dosage

[0354]

[0355] Table 26: Starting Material Analysis - Part 1

[0356]

[0357] Table 27: Starting Material Analysis - Part 2

[0358]

[0359]

[0360] Table 28: Starting Material Analysis - Part 3

[0361]

[0362] refr. refers to the method of refraction.

[0363] Table 29 shows the results of the experiments. Compared to the two syrup-containing aqueous crystalline isomaltitol starting formulations in experiments 1 and 2, the free-flow time of type I crystalline isomaltitol (control group) was increased. In experiment 3, the free-flow time was again shortened after using the fine-crystal isomaltitol of this invention.

[0364] Table 29: Results of the control experiment and the experiment of the present invention

[0365]

[0366] EUROPEAN PHARMACOPOEIA 10.0 (10th edition of the European Pharmacopoeia) Methods 2.9.16 "Flowability" (abbreviated Ph.Eur.2.9.16) is used to determine free flow.

[0367] Table 29 shows a correlation between free flowability and water content when isomaltitol solution is added to prepare aqueous crystalline isomaltitol starting formulations. Compared to the crystallization control group, poorer free flowability was observed. Free flow time could be extended by up to 20% due to the syrup film coating, depending on the syrup ratio. Water content also increased by approximately 17% due to the use of isomaltitol syrup to coat the syrup film.

[0368] To confirm the success of coating crystalline isomaltitol with a syrup film using syrup, sorbitol content was tested in both control and test samples, as the isomaltitol syrup used had a higher sorbitol content. As described in the starting material product analysis, the isomaltitol syrup contained 4.1% (standard %), while the type I crystalline isomaltitol contained only 0.09 g / 100 g DM (standard % and g / 100 g DM are comparable to the first approximation).

[0369] Table 29 shows that the sorbitol content also increases with the increase of the syrup ratio. The sorbitol content detected in the syrup-coated sample (9.6%) was twice that of the isomaltitol-coated control group. This confirms that the syrup film coating was successful.

[0370] The results showed that, surprisingly, the addition of fine isomaltitol particles did not impair the free flow of the isomaltitol crystals coated with the syrup film, for example, due to clumping; on the contrary, it significantly improved the free flow.

Claims

1. A method for preparing a dried carbohydrate preparation from an aqueous crystalline carbohydrate starting material, comprising the following steps: (a) Provide an aqueous crystalline carbohydrate starting material with a water content of 0.4-22.5 wt.%, based on the total weight of the aqueous crystalline carbohydrate starting material, wherein, The aqueous crystalline carbohydrate starting material has a water content exceeding any possible water of crystallization, and in the drying reactor, the aqueous crystalline carbohydrate starting material is selected from sucrose-containing compositions, isomaltulose-containing trehalose-containing compositions, and isomaltulitol-containing compositions, and provides crystalline carbohydrate particles, wherein the proportion of carbohydrate crystals with a diameter less than or equal to 100 μm in the crystalline carbohydrate particles is at least 80 wt.%, wherein the aqueous crystalline carbohydrate starting material comprises at least one poorly soluble carbohydrate with a solubility of 5-53 g / 100 g in water at 20°C and at least one readily soluble carbohydrate with a solubility of greater than 53 g / 100 g in water at 20°C; wherein the aqueous crystalline carbohydrate starting material provided in step (a) contains crystalline carbohydrate particles with a liquid film, and the water in the aqueous crystalline carbohydrate starting material exists in the form of a liquid film on the crystalline carbohydrate particles of the aqueous crystalline carbohydrate starting material, or if the carbohydrates in the aqueous crystalline carbohydrate starting material contain water of crystallization, the water content is composed of the liquid film water content and the water of crystallization content; (b) Under a pressure of 10-1100 mbar, crystalline carbohydrate particles are metered into the aqueous crystalline carbohydrate starting material within the drying reactor using a metering device, at a dosage of 2-30 wt.% based on the total weight of the aqueous crystalline carbohydrate starting material, wherein the temperature of the aqueous crystalline carbohydrate starting material in the drying reactor is 20-80°C; and (c) Under the conditions mentioned in step (b), the resulting mixture is homogenized by a mixing device to obtain a dry carbohydrate formulation, wherein in step (c), the dry carbohydrate formulation is obtained from crystalline carbohydrate particles without a liquid film.

2. The method according to claim 1, wherein, The method can be performed continuously, semi-continuously, or in batches.

3. The method according to claim 1, wherein, The at least one poorly soluble carbohydrate having a solubility of 5-53 g / 100 g in water at 20°C is 1-O-α-D-glucopyranosyl-D-mannitol, isomaltulose, or mannitol, and the at least one readily soluble carbohydrate having a solubility of greater than 53 g / 100 g in water at 20°C is 6-O-α-D-glucopyranosyl-D-sorbitol, fructose, trehalose, or sorbitol.

4. The method according to claim 1, wherein, The aqueous crystalline carbohydrate starting material is an aqueous sucrose composition containing crystalline sucrose and at least one other carbohydrate component selected from invert sugar, caramel syrup and cane syrup.

5. The method according to claim 1, wherein, The aqueous crystalline carbohydrate starting material is the same as the carbohydrate in the crystalline carbohydrate particles.

6. The method according to claim 1, wherein, The crystalline carbohydrate particles described in process step (b) are measured at 2-25 wt.%, based on the total weight of the starting formulation of hydrated crystalline carbohydrates.

7. The method according to claim 1, wherein, In step (b), the crystalline carbohydrate particles are metered in a drying reactor without overpressure or negative pressure under atmospheric pressure; the crystalline carbohydrate particles are metered in a vacuum drying reactor under reduced pressure of 10-900 mbar; or the crystalline carbohydrate particles are metered in a pressurized drying reactor under atmospheric pressure to 1100 mbar.

8. The method according to claim 1, wherein, Modulation is performed in step (d) after step (c) of the process.

9. The method according to claim 8, wherein, The modulation temperature according to process step (d) is at least 30°C.

10. The method according to claim 8, wherein, The modulation pressure for process step (d) is 10-1100 mbar.

11. The method according to claim 4, wherein, The aqueous sucrose composition is obtained from sugarcane.

12. The method according to claim 1, wherein, The aqueous crystalline carbohydrate starting material is an aqueous isomaltitol starting material, which contains 1-O-α-D-glucopyranosyl-D-mannitol and 6-O-α-D-glucopyranosyl-D-sorbitol, with a content of 95.0-100.0 wt.%, based on the total dry mass of the aqueous isomaltitol starting material.

13. The method according to claim 12, wherein, The aqueous isomaltitol starting formulation contains 45.0-50.0 wt.% 1-O-α-D-glucopyranosyl-D-mannitol and 50-55 wt.% 6-O-α-D-glucopyranosyl-D-sorbitol, both calculated based on the total dry mass of the aqueous isomaltitol starting formulation.

14. The method according to claim 12, wherein, The aqueous isomaltitol starting formulation contains 20.0-30.0 wt.% 1-O-α-D-glucopyranosyl-D-mannitol and 70.0-80.0 wt.% 6-O-α-D-glucopyranosyl-D-sorbitol, both calculated based on the total dry mass of the aqueous isomaltitol starting formulation.

15. The method according to claim 1, wherein, The aqueous crystalline carbohydrate starting material is an aqueous isomaltitol starting material, which contains 1-O-α-D-glucopyranosyl-D-sorbitol, sorbitol, mannitol, or glucopyranosyl-idutitol, or a mixture of two or more of the above.

16. The method according to claim 1, wherein, The aqueous crystalline carbohydrate starting material is an aqueous isomaltulose-containing trehalose-containing starting material, which contains fructose, glucose, isomaltose or isomalutose or a mixture of two or more of the above.

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