A method for preparing high-purity β-D-glucose

Abstract

The present invention provides a method for preparing high-purity β-D-glucose, comprising the following steps: (a) dissolving glucose monohydrate in purified water to obtain a glucose solution; (b) decolorizing and removing impurities from the glucose solution, and then concentrating at 60-90°C to obtain a first concentrated solution; the glucose mass concentration of the first concentrated solution is increased to 75-85%; (c) taking 1-5% of the mass of the first concentrated solution as a stock solution, heating it to 120-130°C to concentrate it to a mass concentration of 92%-97% to obtain a second concentrated solution; (d) subjecting the second concentrated solution to ultrasonic-induced nucleation, and then obtaining β-phase seeds through crystal cultivation and seed classification; (e) adding the β-phase seeds to the first concentrated solution for concentrated crystallization, followed by centrifugation and drying. β-D-glucose with high purity and fast dissolution can be obtained.

Description

Technical Field

[0001] The invention belongs to the technical field of glucose preparation, and relates to a method for preparing beta-D-glucose, and in particular to a method for preparing high-purity beta-D-glucose. Background Art

[0002] Glucose is the most widely distributed and important monosaccharide in nature. It is a polyhydroxy aldehyde. Pure glucose is a colorless crystal, sweet but not as sweet as sucrose. It is easily soluble in water, slightly soluble in ethanol, and insoluble in ether. Natural glucose aqueous solution is optically rotated to the right, so it is "dextrose". β-D (+) -glucose refers to the hydroxyl group and aldehyde group generated by the reaction of hydroxyl group and hydroxymethyl group on the same side of the ring, while on the opposite side of the ring is α type.

[0003] At present, the preparation process of glucose mainly involves dissolving monohydrate glucose, decolorizing / removing impurities, and concentrating it, then adding seed crystals for concentrated crystallization, centrifuging, and drying. In the process of adding seed crystals for concentrated crystallization, since the seed crystals are mixed seed crystals and the seed crystals are not accurately graded, the purity of β-D-glucose is low, and β-D-glucose with a single configuration cannot be obtained. Summary of the invention

[0004] In order to solve the above technical problems, the object of the present invention is to provide a method for preparing high-purity β-D-glucose.

[0005] In order to achieve the above technical problem, the present invention provides a method for preparing high-purity β-D-glucose, comprising the following steps:

[0006] (a) dissolving glucose monohydrate in purified water to obtain a glucose solution;

[0007] (b) decolorizing and removing impurities from the glucose solution, and then concentrating the solution at 60-90° C. to obtain a first concentrated solution; the glucose mass concentration of the first concentrated solution is increased to 75-85%;

[0008] (c) taking 1 to 10% of the mass of the first concentrated solution as a stock solution, heating it to 120 to 130° C. and concentrating it to a mass concentration of 92% to 97% to obtain a second concentrated solution;

[0009] (d) subjecting the second concentrated solution to ultrasonic-induced nucleation, followed by crystal growth and seed classification to obtain β-phase seed crystals;

[0010] (e) adding the β-phase seed crystals into the first concentrated solution for concentrated crystallization, followed by centrifugation and drying.

[0011] Optimally, in step (a), the mass concentration of the glucose solution is 70-75%. In step (c), 1-5% of the mass of the first concentrated solution is taken as the stock solution.

[0012] Furthermore, in step (a), the purified water is heated to 75-85°C.

[0013] Furthermore, in step (b), decolorization and impurity removal are carried out while hot.

[0014] Furthermore, in step (b), the concentrated distilled water is used in step (a) to dissolve glucose monohydrate.

[0015] Optimally, in step (d), the ultrasonic induced nucleation is: ultrasonicating at a frequency of 10 KHz to 20 KHz for 5 to 30 minutes at 120 to 130° C. and a mass concentration of 92% to 97%.

[0016] Furthermore, in step (d), the crystal growing is: growing the crystal for 0.5 to 2 hours at 120 to 130° C. and a mass concentration of 92% to 97%.

[0017] Furthermore, in step (d), the seed crystals are classified to select β-phase seeds with a particle size of 30 to 80 μm.

[0018] Optimally, in step (e), the evaporation rate of the concentrated crystallization is 120 to 160 L / h.

[0019] Furthermore, in step (e), the distilled water from the concentrated crystals is used in step (a) to dissolve glucose monohydrate.

[0020] The method for preparing high-purity β-D-glucose of the present invention takes a small amount of concentrated liquid as the stock liquid for further high-temperature concentration and ultrasonic-induced nucleation to form β-phase crystal seeds, which are then added into the first concentrated liquid for concentrated crystallization, thereby obtaining high-purity and fast-dissolving β-D-glucose. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 The present invention is a flow chart of the method for preparing high-purity β-D-glucose. DETAILED DESCRIPTION

[0022] The preparation method of high-purity β-D-glucose of the present invention comprises the following steps: (a) dissolving glucose monohydrate in purified water to obtain a glucose solution; (b) decolorizing and removing impurities from the glucose solution, and then concentrating at 60-90°C to obtain a first concentrated solution; the glucose mass concentration of the first concentrated solution is increased to 75-85%; (c) taking 1-10% of the mass of the first concentrated solution as a stock solution, heating it to 120-130°C and concentrating it to a mass concentration of 92%-97% to obtain a second concentrated solution; (d) subjecting the second concentrated solution to ultrasonic-induced nucleation, and then subjecting it to crystal cultivation and seed classification to obtain β-phase seed crystals; (e) adding the β-phase seed crystals to the first concentrated solution for concentrated crystallization, and then centrifuging and drying. By taking a small amount of concentrated solution as a stock solution for further high-temperature concentration and ultrasonic-induced nucleation to form β-phase seed crystals, and then adding it to the first concentrated solution for concentrated crystallization, high-purity and fast-dissolving β-D-glucose can be obtained.

[0023] Optimally, in step (a), the mass concentration of the glucose solution is 70-75%; the purified water is heated to 75-85° C.; and in step (c), 1-5% of the mass of the first concentrated solution is taken as the stock solution.

[0024] Optimally, in step (b), decolorization and impurity removal are performed while hot; and the concentrated distilled water is used in step (a) to dissolve glucose monohydrate.

[0025] Optimally, in step (d), the ultrasonic induced nucleation is: ultrasonic at a frequency of 10KHz to 20KHz for 5 to 30 minutes at 120 to 130°C and a mass concentration of 92% to 97%; the crystal growing is: crystal growing for 0.5 to 2 hours at 120 to 130°C and a mass concentration of 92% to 97%; the seed classification is to select β-phase seeds with a particle size of 30 to 80μm.

[0026] Optimally, in step (e), the evaporation rate of the concentrated crystals is 120-160 L / h; the evaporated water of the concentrated crystals is used in step (a) to dissolve glucose monohydrate.

[0027] The present invention will be further described below in conjunction with the embodiments shown in the accompanying drawings.

[0028] Example 1

[0029] This embodiment provides a method for preparing high-purity β-D-glucose, comprising the following steps:

[0030] (a) dissolving 2000 kg of glucose monohydrate in 400 L of purified water at 75-85° C. (the temperature of the purified water can be any temperature that can dissolve glucose monohydrate, and the temperature range has little effect on the product quality) to obtain a glucose solution with a mass concentration of 75%;

[0031] (b) decolorizing and removing impurities from the glucose solution (specifically, adding 200 g of activated carbon, keeping warm for 30 minutes, filtering while hot, removing the activated carbon, and obtaining a clarified filtrate), and then concentrating at 80° C. (in actual operation, 60 to 90° C. is acceptable as long as the water can be evaporated) to obtain a first concentrated solution (about 2250 kg; the glucose mass concentration of the first concentrated solution is increased to 80%, and the first concentrated solution is in the α / β coexistence phase region); the concentrated distilled water is used in step (a) to dissolve glucose monohydrate, which can save energy and improve the utilization rate of purified water;

[0032] (c) taking 1% of the mass of the first concentrated solution as a stock solution (about 22.5 kg), heating it to 120° C. at normal pressure (since the glucose content in the first concentrated solution is very high, the stock solution can be heated to 120° C. at normal pressure, the same below) and concentrating it to a mass concentration of 92% to obtain a second concentrated solution (the first concentrated solution is a β phase region);

[0033] (d) subjecting the second concentrated solution to ultrasonic nucleation induction: subjecting the second concentrated solution to ultrasonication at a frequency of 20 kHz for 5 minutes at 120° C. and a mass concentration of 92%; subsequently subjecting the second concentrated solution to crystal growth: subjecting the second concentrated solution to crystal growth at a frequency of 20 kHz for 2 hours at 120° C. and a mass concentration of 92%; and subjecting the second concentrated solution to seed classification (selecting seed crystals with a particle size of 30 to 80 μm) to obtain β-phase seed crystals;

[0034] (e) adding β-phase seed crystals to the first concentrated liquid for concentration and crystallization (evaporation rate is 120-160 L / h), followed by centrifugation (the liquid obtained by centrifugation can be used to prepare a biochemical treatment nutrient) and drying to obtain 1630 kg of β-D-glucose (specific rotation is 22.57, i.e., optical purity is 96.2%, and yield is 90.5%, calculated as anhydrous glucose); the distilled water from the concentrated crystals is used in step (a) to dissolve monohydrate glucose, which can save energy and improve the utilization rate of purified water.

[0035] Example 2

[0036] This embodiment provides a method for preparing high-purity β-D-glucose, comprising the following steps:

[0037] (a) dissolving 2000 kg of glucose monohydrate in 570 L of purified water at 75-85° C. (the temperature of the purified water can be any temperature that can dissolve glucose monohydrate, and the temperature range has little effect on the product quality) to obtain a glucose solution with a mass concentration of 70%;

[0038] (b) decolorizing and removing impurities from the glucose solution (adding 200 g of activated carbon, keeping warm for 30 min, filtering while hot to remove the activated carbon and obtain a clarified filtrate), and then concentrating at 80° C. (in actual operation, 60-90° C. is acceptable as long as the water can be evaporated) to obtain a first concentrated solution (about 2500 kg; the glucose mass concentration of the first concentrated solution is increased to 75%, and the first concentrated solution is in the α / β coexistence phase region); the concentrated distilled water is used in step (a) to dissolve glucose monohydrate, which can save energy and improve the utilization rate of purified water;

[0039] (c) taking 3% of the mass of the first concentrated solution as the stock solution (about 75 kg), heating it to 130° C. at normal pressure and concentrating it to a mass concentration of 97% to obtain a second concentrated solution (the first concentrated solution is the β phase region);

[0040] (d) subjecting the second concentrated solution to ultrasonic nucleation induction: subjecting the second concentrated solution to ultrasonication at a frequency of 15 kHz for 30 minutes at 130° C. and a mass concentration of 97%; subsequently subjecting the second concentrated solution to crystal growth: subjecting the second concentrated solution to crystal growth at a frequency of 15 kHz for 30 minutes at 130° C. and a mass concentration of 97% for 1 hour; and subjecting the second concentrated solution to crystal seed classification (selecting crystal seeds with a particle size of 30 to 80 μm) to obtain β-phase crystal seeds;

[0041] (e) adding β-phase seed crystals to the first concentrated liquid for concentration and crystallization (evaporation rate is 120-160 L / h), followed by centrifugation (the liquid obtained by centrifugation can be used to prepare a biochemical treatment nutrient) and drying to obtain 1658 kg of β-D-glucose (specific rotation is 20.41, i.e., optical purity is 98.5%, and yield is 92.1%, calculated as anhydrous glucose); the distilled water from the concentrated crystals is used in step (a) to dissolve monohydrate glucose, which can save energy and improve the utilization rate of purified water.

[0042] Example 3

[0043] This embodiment provides a method for preparing high-purity β-D-glucose, comprising the following steps:

[0044] (a) dissolving 2000 kg of glucose monohydrate in 500 L of purified water at 75-85° C. (the temperature of the purified water can be any temperature that can dissolve glucose monohydrate, and the temperature range has little effect on the product quality) to obtain a glucose solution with a mass concentration of 72%;

[0045] (b) decolorizing and removing impurities from the glucose solution (adding 200 g of activated carbon, keeping warm for 30 min, filtering while hot to remove the activated carbon and obtain a clarified filtrate), and then concentrating at 80° C. (in actual operation, 60-90° C. is acceptable as long as the water can be evaporated) to obtain a first concentrated solution (about 2305 kg; the glucose mass concentration of the first concentrated solution is increased to 78%, and the first concentrated solution is in the α / β coexistence phase region); the concentrated distilled water is used in step (a) to dissolve glucose monohydrate, which can save energy and improve the utilization rate of purified water;

[0046] (c) taking 5% of the mass of the first concentrated solution as the stock solution (about 115 kg), heating it to 125° C. under normal pressure and concentrating it to a mass concentration of 95% to obtain a second concentrated solution (the first concentrated solution is the β phase region);

[0047] (d) subjecting the second concentrated solution to ultrasonic nucleation induction: subjecting the second concentrated solution to ultrasonic nucleation at a frequency of 10 kHz for 1 hour at 125° C. and a mass concentration of 95%; then subjecting the second concentrated solution to crystal growth: subjecting the second concentrated solution to crystal growth at a frequency of 10 kHz for 1 hour at 125° C. and a mass concentration of 95% for 0.5 hour; and subjecting the second concentrated solution to crystal seed classification (selecting crystal seeds with a particle size of 30 to 80 μm) to obtain β-phase crystal seeds;

[0048] (e) adding β-phase seed crystals to the first concentrated liquid for concentration and crystallization (evaporation rate is 120-160 L / h), followed by centrifugation (the liquid obtained by centrifugation can be used to prepare a biochemical treatment nutrient) and drying to obtain 1605 kg of β-D-glucose (specific rotation is 20.69, i.e., optical purity is 98.2%, and yield is 89.2%, calculated as anhydrous glucose); the distilled water from the concentrated crystals is used in step (a) to dissolve monohydrate glucose, which can save energy and improve the utilization rate of purified water.

[0049] Example 4

[0050] This embodiment provides a method for preparing high-purity β-D-glucose, which is basically the same as that in Example 2, except that: in step (c), 10% of the mass of the first concentrated solution is taken as the stock solution, the product optical purity is 98.7%, and the yield is 89.5%, calculated as anhydrous glucose (at this time, the product purity is basically the same as that in Example 3, but concentrating 10% of the stock solution leads to increased costs).

[0051] Comparative Example 1

[0052] This embodiment provides a method for preparing high-purity β-D-glucose, which is basically the same as that in Example 2, except that in step (c), the stock solution is heated to 110° C. for concentration, and the product has an optical purity of 83.5% and a yield of 91.4%, calculated as anhydrous glucose.

[0053] Comparative Example 2

[0054] This embodiment provides a method for preparing high-purity β-D-glucose, which is basically the same as that in Example 2, except that in step (c), the stock solution is heated to 140° C. for concentration, which fails to crystallize and the condition fails.

[0055] Comparative Example 3

[0056] This embodiment provides a method for preparing high-purity β-D-glucose, which is basically the same as that in Example 2, except that in step (d), ultrasonic-induced nucleation is performed at a frequency of 50 kHz for 5 minutes at 120-130°C and a mass concentration of 90%, and the seed crystallization is difficult and the condition fails.

[0057] Comparative Example 4

[0058] This embodiment provides a method for preparing high-purity β-D-glucose, which is basically the same as that in Example 2, except that: in step (d), ultrasonic induced nucleation is: at 120-130°C, mass concentration of 98%, ultrasound is applied at a frequency of 8 kHz for 25 minutes, the product has an optical purity of 86.3%, and a yield of 89.8%, calculated as anhydrous glucose.

[0059] Comparative Example 5

[0060] This embodiment provides a method for preparing high-purity β-D-glucose, which is basically the same as that in Example 2, except that in step (d), the particle size selected during seed classification is about 100 μm, the product has an optical purity of 93.6%, and a yield of 90.2%, calculated as anhydrous glucose.

[0061] Comparative Example 6

[0062] This embodiment provides a method for preparing high-purity β-D-glucose, which is basically the same as that in Example 2, except that in step (d), the evaporation rate of the concentrated crystallization is 300 L / h, the product optical purity is 78.5%, and the yield is 89.8%, calculated as anhydrous glucose.

[0063] Comparative Example 7

[0064] This embodiment provides a method for preparing high-purity β-D-glucose, which is basically the same as that in Example 2, except that in step (d), the evaporation rate of the concentrated crystallization is 50 L / h, the product optical purity is 92.7%, and the yield is 91.5%, calculated as anhydrous glucose.

[0065] The above embodiments are only for illustrating the technical concept and features of the present invention, and their purpose is to enable people familiar with the technology to understand the content of the present invention and implement it accordingly, and they cannot be used to limit the protection scope of the present invention. Any equivalent changes or modifications made according to the spirit of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for preparing high-purity β-D-glucose, characterized in that: The following steps are involved: (a) dissolving glucose monohydrate in purified water to obtain a glucose solution; (b) decolorizing and removing impurities from the glucose solution, and then concentrating the solution at 60-90° C. to obtain a first concentrated solution; the glucose mass concentration of the first concentrated solution is increased to 75-85%; (c) taking 1-10% of the mass of the first concentrated solution as a stock solution, heating it to 120-130° C. and concentrating it to a mass concentration of 92%-97% to obtain a second concentrated solution; (d) subjecting the second concentrated solution to ultrasonic-induced nucleation, followed by crystal growth and seed classification to obtain β-phase seed crystals; The ultrasonic induced nucleation is as follows: at 120-130°C and a mass concentration of 92%-97%, ultrasonication is performed at a frequency of 10KHz-20KHz for 5-30min; The crystal growing comprises: growing the crystal for 0.5 to 2 hours at 120 to 130° C. and a mass concentration of 92% to 97%; The seed classification is to select β-phase seeds with a particle size of 30-80 μm; (e) adding the β-phase seed crystals into the first concentrated solution for concentrated crystallization, followed by centrifugation and drying.

2. The method for preparing high-purity β-D-glucose according to claim 1, characterized in that: In step (a), the mass concentration of the glucose solution is 70-75%; in step (c), 1-5% of the mass of the first concentrated solution is taken as the stock solution.

3. The method for preparing high-purity β-D-glucose according to claim 1 or 2, characterized in that: In step (a), the purified water is heated to 75-85°C.

4. The method for preparing high-purity β-D-glucose according to claim 3, characterized in that: In step (b), decolorization and impurity removal are carried out while hot.

5. The method for preparing high-purity β-D-glucose according to claim 1 or 4, characterized in that: In step (b), the concentrated distilled water is used in step (a) to dissolve glucose monohydrate.

6. The method for preparing high-purity β-D-glucose according to claim 1, characterized in that: In step (e), the evaporation rate of the concentrated crystallization is 120-160 L / h.

7. The method for preparing high-purity β-D-glucose according to claim 6, characterized in that: In step (e), the distilled water from the concentrated crystals is used in step (a) to dissolve glucose monohydrate.

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