High-purity trehalose as well as crystallization method and application thereof

Abstract

The invention relates to the technical field of trehalose preparation, in particular to high-purity trehalose and a crystallization method and application thereof. The crystallization method comprises the following steps: (1) heating a trehalose solution to 60-65 DEG C, and adding a seed crystal to obtain a seed crystal sugar solution; (2) cooling the seed crystal sugar solution to 25-30 DEG C to obtain a trehalose crystal; (3) heating the trehalose crystals to 60-65 DEG C, and keeping the temperature for 10-20 minutes to obtain a trehalose mixture; and (4) repeating the steps (2)-(3) for 0-2 times, cooling the trehalose mixture to 25-30 DEG C, keeping for 9-10 hours, centrifuging, drying and screening to obtain the high-purity trehalose. The high-purity trehalose prepared by the method disclosed by the invention is high in purity, few in impurities, uniform in trehalose crystal particle, stable in quality and high in recovery rate, and can be widely applied to the fields of food, medicine, daily chemical industry and the like.

Description

Technical Field

[0001] The invention relates to the technical field of trehalose preparation, and in particular to high-purity trehalose and a crystallization method and application thereof. Background Art

[0002] Trehalose is a natural non-reducing disaccharide composed of two molecules of glucose residues connected by an α, α-1, 1 glycosidic bond. It has the special function of preserving biological vitality. It can effectively protect the structure of cell membranes and proteins in organisms, so that they can still keep the cells moist in many abnormal conditions (such as high temperature, dry dehydration, high osmotic pressure, freezing), prevent the cells from losing nutrients and cell damage due to water loss, so that the organisms have strong resistance to adversity, drought and frost. Outside the body, trehalose also has the characteristics of stabilizing biological membranes and protein structures. It is often used to protect bioengineering enzymes, various viruses, vaccines, antibodies, protein factors, nucleic acids, etc., and has achieved exciting results. Usually these biological products must be stored under ultra-low temperature conditions, otherwise they will be inactivated. After adding trehalose, they can be dried and stored at room temperature without changing their biological activity. Therefore, the application of trehalose will greatly facilitate the storage, transportation and use of biological macromolecules (including proteins, enzyme preparations, polysaccharides, lipids, etc.), cell membranes and organelles, and medical biological products (including plasma, globulin, antiserum, transfer factor, vaccine, vaccine and drug-loaded liposome, etc.) (eliminating the need for freezing and refrigeration equipment and costs). In addition, replacing human albumin (currently a protective agent for vaccines or protein factors) with trehalose can not only avoid the infection of viruses in the blood, but also solve the problem of limited blood supply. Due to its unique cell membrane and protein structure protection function and anti-drying and anti-dehydration functions, trehalose has the unique function of inhibiting the generation of strange smells such as certain volatile aldehydes, ethyl mercaptan and trimethylamine in food preservation and anti-corrosion, thereby extending the storage period of the product. Therefore, it has a wide range of great application value.

[0003] Trehalose crystallization refers to the process of trehalose molecules arranging in a certain order to form a hard crystal structure. It is an extremely important unit operation that can perform purification and product separation at the same time. During crystallization, high-purity product crystals are formed, and impurities remain in the solution. High-quality trehalose crystallization process directly affects product attributes such as crystal size, shape, yield and purity, and can improve the final product quality and process efficiency. Existing trehalose crystallization methods have problems such as small crystals, different batch sizes, high impurity content and low recovery rate.

[0004] Therefore, it is urgent to develop a mature and stable trehalose crystallization method to improve the particle uniformity, product purity and recovery rate of trehalose crystals. Summary of the invention

[0005] The purpose of the present invention is to provide a high-purity trehalose and a crystallization method and application thereof.

[0006] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:

[0007] The present invention provides a method for crystallizing high-purity trehalose, comprising the following steps:

[0008] (1) heating the trehalose solution to a temperature of 60-65° C., adding seed crystals, and obtaining a seed sugar solution;

[0009] (2) cooling the seed sugar solution to 25-30° C. to obtain trehalose crystals;

[0010] (3) heating the trehalose crystals to 60-65° C. and maintaining the temperature for 10-20 minutes to obtain a trehalose mixture;

[0011] (4) After repeating steps (2) to (3) 0 to 2 times, the trehalose mixture is cooled to 25 to 30° C., maintained for 9 to 10 hours, centrifuged, dried, and screened to obtain high-purity trehalose.

[0012] Preferably, the initial concentration of the trehalose solution in step (1) is 62-70 wt %;

[0013] The size of the seed crystals in step (1) is 80-100 mesh;

[0014] The mass of the added seed crystals is 0.5-1.0% of the mass of the dry matter in the trehalose solution.

[0015] Preferably, the cooling rate in step (2) is 2-3°C / h.

[0016] Preferably, the centrifugal speed in step (4) is 800-1200 rpm, and the centrifugal time is 6-10 min.

[0017] Preferably, the drying temperature in step (4) is 50-77°C.

[0018] Preferably, the proportion of high-purity trehalose with a mesh size of 20 to 60 is ≥ 88%.

[0019] The present invention also provides high-purity trehalose obtained according to the crystallization method, wherein the purity of trehalose in the high-purity trehalose is ≥99.7% and the glucose content is <0.02 mmol / L.

[0020] The present invention also provides high-purity trehalose obtained according to the crystallization method or the use of the high-purity trehalose in preparing products for extending the shelf life of cell membranes, cell organelles and biological products.

[0021] The present invention also provides high-purity trehalose obtained according to the crystallization method or the use of the high-purity trehalose in preparing products for food preservation, antiseptic treatment and food storage period extension.

[0022] The present invention provides a high-purity trehalose and a crystallization method and application thereof. The method of the present invention has the following advantages:

[0023] (1) The crystallization method of the present invention uses trehalose as the main raw material, and no other substances need to be added except for the crystal seed during the crystallization process, and the obtained product has high purity and few impurities;

[0024] (2) The added seed crystals are specially made 80-100 mesh dihalose dihydrate crystals, with a moderate number of crystal nuclei and good crystal growth properties;

[0025] (3) Optimize and control the crystal size distribution by carefully selecting the correct crystallization conditions and process parameters. Purify the seed sugar solution by repeatedly cooling and heating the solution in stages under precise temperature control, which can be used to control the supersaturation of the trehalose solution, improve batch consistency, and optimize the formed product;

[0026] (4) Trehalose crystallization in the crystallization tank can perform purification and product separation at the same time, forming high-purity product crystals, while impurities remain in the solution;

[0027] (5) The existing trehalose crystallization method avoids the problems of too small crystals, different batch sizes, high impurity content and low recovery rate, and improves the particle uniformity of trehalose crystals. The product has high purity, few impurities, stable quality and high recovery rate, and can be widely used in food, medicine, daily chemical industry and other fields. DETAILED DESCRIPTION

[0028] The present invention provides a method for crystallizing high-purity trehalose, comprising the following steps:

[0029] (1) heating the trehalose solution to a temperature of 60-65° C., adding seed crystals, and obtaining a seed sugar solution;

[0030] (2) cooling the seed sugar solution to 25-30° C. to obtain trehalose crystals;

[0031] (3) heating the trehalose crystals to 60-65° C. and maintaining the temperature for 10-20 minutes to obtain a trehalose mixture;

[0032] (4) After repeating steps (2) to (3) 0 to 2 times, the trehalose mixture is cooled to 25 to 30° C., maintained for 9 to 10 hours, centrifuged, dried, and screened to obtain high-purity trehalose.

[0033] In the present invention, the initial concentration of the trehalose solution in step (1) is 62-70wt%, preferably 65wt%; in the present invention, the temperature to which the trehalose solution in step (1) is heated is preferably 63°C; in the present invention, the seed crystals are trehalose dihydrate crystals; the size of the seed crystals in step (1) is 80-100 mesh, preferably 90 mesh; the mass of the seed crystals added is 0.5-1.0% of the mass of the dry matter in the trehalose solution, preferably 0.8%.

[0034] In the present invention, the cooling rate in step (2) is 2-3°C / h, preferably 2.5°C / h, and the cooling includes a stirring step, and the stirring rate is 40-50rpm, preferably 45rpm; the cooling temperature in step (2) is preferably 28°C, and the holding time is preferably 9.5h.

[0035] In the present invention, the temperature of the heating in step (3) is preferably 63° C., and the holding time is preferably 15 minutes; the heating in step (3) also includes a stirring step, and the stirring rate is 100-150 rpm, preferably 120 rpm.

[0036] In the present invention, the purpose of cooling the trehalose mixture to 25-30° C. and maintaining the temperature for 9-10 hours is to allow the trehalose to fully crystallize.

[0037] In the present invention, the centrifugal speed in step (4) is 800-1200 rpm, preferably 1000 rpm, and the centrifugal time is 6-10 min, preferably 8 min.

[0038] In the present invention, the drying temperature in step (4) is 50-77°C, preferably 60°C, and the drying time when the drying temperature is ≥63°C is ≥0.5h; the timing starts when it is ≥63°C and stops when it is <63°C.

[0039] In the present invention, the crystallization method of high-purity trehalose is preferably:

[0040] Take 65% trehalose solution into the crystallizer, add 0.5% dihydrate trehalose crystals of 80 mesh after the temperature stabilizes at 65℃; pass cold water into the jacket of the crystallizer, stir at 40rpm, cool at 2℃ / h, slowly cool to 30℃ for crystallization, and obtain trehalose crystals; pass hot water into the jacket of the crystallizer, stir at 100rpm; heat to 65℃, keep for 10min, partially dissolve the crystals, and obtain trehalose mixture; pass cold water into the jacket of the crystallizer, stir at 40rpm, cool at 2℃ / h, slowly cool the trehalose mixture to 30℃, keep for 10h, and make the crystals complete. Then centrifuge in a flat centrifuge at 1000rpm for 9min. Dry in a double cone dryer, set the drying temperature to 59-67℃, and the time ≥63℃ is 1.5h. Screen with an electric vibrating screen.

[0041] In the present invention, the crystallization method of high-purity trehalose is preferably:

[0042] Take 65% trehalose solution into a crystallizer, and after the temperature is stabilized at 65°C, add 0.5% dihydrate trehalose crystals of 80 mesh in weight of dry matter in the trehalose solution; pass cold water into the jacket of the crystallizer, stir at 40 rpm, cool at 2°C / h, and slowly cool to 30°C for crystallization; pass hot water into the jacket of the crystallizer, stir at 100 rpm, heat to 65°C, and keep for 10 minutes to partially dissolve the crystals; pass cold water into the jacket of the crystallizer, stir at 40 rpm, cool at 2°C / h, and slowly cool to 30°C for crystallization; pass hot water into the jacket of the crystallizer, stir at 100 rpm, heat to 65°C, and keep for 10 minutes to partially dissolve the crystals; pass cold water into the jacket of the crystallizer, and stir at 2°C / h. Under the conditions of stirring speed of 40rpm and cooling rate of 2℃ / h, the trehalose mixture 1 is slowly cooled to 30℃ for crystallization; hot water is passed into the jacket of the crystallization tank, stirring speed is 100rpm, heating to 65℃, and maintaining for 10min to partially dissolve the crystals to obtain a trehalose mixture; cold water is passed into the jacket of the crystallization tank, stirring speed is 40rpm, cooling rate is 2℃ / h, the trehalose mixture is slowly cooled to 30℃, and maintained for 10h to complete the crystallization. Then centrifuge in a flat centrifuge at a speed of 1000rpm for 10min. Dry in a double cone dryer, the drying temperature is set to 62-70℃, and the drying time is 1.5h at ≥63℃. Screen with an electric vibrating screen.

[0043] In the present invention, the proportion of high-purity trehalose with a mesh size of 20 to 60 is ≥ 88%.

[0044] The present invention also provides high-purity trehalose obtained according to the crystallization method, wherein the purity of trehalose in the high-purity trehalose is ≥99.7% and the glucose content is <0.02 mmol / L.

[0045] The present invention also provides high-purity trehalose obtained according to the crystallization method or the use of the high-purity trehalose in preparing products for extending the shelf life of cell membranes, cell organelles and biological products.

[0046] The present invention also provides high-purity trehalose obtained according to the crystallization method or the use of the high-purity trehalose in preparing products for food preservation, antiseptic treatment and food storage period extension.

[0047] The solutions provided by the present invention are described in detail below in conjunction with the embodiments, but they should not be understood as limiting the protection scope of the present invention.

[0048] Example 1

[0049] (1) Take a 65% trehalose solution into a crystallization tank, stabilize the temperature at 65°C, and add 0.5% trehalose dihydrate crystals with a size of 80 mesh in the trehalose solution.

[0050] (2) Cold water was introduced into the jacket of the crystallization tank, the stirring speed was 40 rpm, the cooling rate was 2°C / h, and the temperature was slowly lowered to 30°C for crystallization to obtain trehalose crystals.

[0051] (3) Pass hot water into the jacket of the crystallization tank with a stirring speed of 100 rpm; raise the temperature to 65° C. and maintain for 10 min to partially dissolve the crystals to obtain a trehalose mixture.

[0052] (4) Pass cold water into the jacket of the crystallization tank, slowly cool the trehalose mixture to 30°C at a stirring speed of 40rpm and a cooling rate of 2°C / h, and keep it for 10 hours to allow the trehalose to crystallize completely. Then centrifuge it in a plate centrifuge at a speed of 1000rpm for 9 minutes. Dry it in a double cone dryer, set the drying temperature to 59-67°C, and the drying time at ≥63°C is 1.5h (start timing at ≥63°C and stop timing at <63°C). Screen it with an electric vibrating screen and select crystals of 20-60 mesh as high-purity trehalose crystals.

[0053] In this embodiment, the particle size of trehalose in the high-purity trehalose crystal product is 20-60 mesh accounting for 88%, 60-100 mesh accounting for 12%, the glucose content is 0.019mmol / L, the trehalose purity is 99.8%, and the trehalose recovery rate is 53%, of which the high-purity trehalose with a particle size of 20-60 mesh accounts for 88%.

[0054] Example 2

[0055] (1) Take a 65% trehalose solution into a crystallization tank, stabilize the temperature at 65°C, and add 0.5% trehalose dihydrate crystals with a size of 80 mesh in the trehalose solution.

[0056] (2) Cold water was introduced into the jacket of the crystallization tank, the stirring speed was 40 rpm, the cooling rate was 2 °C / h, and the temperature was slowly lowered to 30 °C for crystallization.

[0057] (3) Hot water was introduced into the jacket of the crystallization tank, the stirring speed was 100 rpm, and the heating time was 10 min. The temperature was raised to 65°C to partially dissolve the crystals.

[0058] (4) Cold water was introduced into the jacket of the crystallization tank, and the trehalose mixture 1 was slowly cooled to 30° C. for crystallization at a stirring speed of 40 rpm and a cooling rate of 2° C. / h.

[0059] (5) Hot water was introduced into the jacket of the crystallization tank, the stirring speed was 100 rpm, the heating time was 10 min, the temperature was raised to 65° C., the crystals were partially dissolved, and a trehalose mixture was obtained.

[0060] (6) Pass cold water into the jacket of the crystallization tank, slowly cool the trehalose mixture to 30°C at a stirring speed of 40rpm and a cooling rate of 2°C / h, and keep it for 10 hours to complete the crystallization of trehalose. Then centrifuge it in a plate centrifuge at a speed of 1000rpm for 10 minutes. Dry it in a double cone dryer, set the drying temperature to 62-70°C, and the drying time at ≥63°C is 1.5h (start timing at ≥63°C and stop timing at <63°C). Screen it with an electric vibrating screen and select crystals of 20-60 mesh as high-purity trehalose crystals.

[0061] In this embodiment, the particle size of trehalose in the high-purity trehalose crystals is 20-30 mesh accounting for 70%, 30-60 mesh accounting for 25%, 60-100 mesh accounting for 5%, the glucose content is 0.017mmol / L, the trehalose purity is 99.9%, and the trehalose recovery rate is 55%, of which the high-purity trehalose with a particle size of 20-60 mesh accounts for 95%.

[0062] Example 3

[0063] (1) Take a 65% trehalose solution into a crystallization tank, stabilize the temperature at 65°C, and add 0.5% trehalose dihydrate crystals with a size of 80 mesh in the trehalose solution.

[0064] (2) Cold water was introduced into the jacket of the crystallization tank, the stirring speed was 40 rpm, the cooling rate was 2 °C / h, and the temperature was slowly lowered to 30 °C for crystallization.

[0065] (3) Hot water was introduced into the jacket of the crystallization tank, the stirring speed was 100 rpm, and the heating time was 10 min. The temperature was raised to 65°C to partially dissolve the crystals.

[0066] (4) Cold water was introduced into the jacket of the crystallization tank, and the trehalose mixture was slowly cooled to 30°C for crystallization at a stirring speed of 40 rpm and a cooling rate of 2°C / h.

[0067] (5) Hot water was introduced into the jacket of the crystallization tank, the stirring speed was 100 rpm, the heating time was 10 min, the temperature was raised to 65° C., the crystals were partially dissolved, and a trehalose mixture was obtained.

[0068] (6) Cold water was introduced into the jacket of the crystallization tank, and the trehalose mixture was slowly cooled to 30°C for crystallization at a stirring speed of 40 rpm and a cooling rate of 2°C / h.

[0069] (7) Hot water was introduced into the jacket of the crystallization tank, the stirring speed was 100 rpm, the heating time was 10 min, the temperature was raised to 65° C., the crystals were partially dissolved, and a trehalose mixture was obtained.

[0070] (8) Pass cold water into the jacket of the crystallization tank, slowly cool the trehalose mixture to 30°C at a stirring speed of 40 rpm and a cooling rate of 2°C / h, and keep it for 10 hours to complete the crystallization of trehalose. Then centrifuge it in a plate centrifuge at a speed of 1000 rpm for 10 minutes. Dry it in a double cone dryer, set the drying temperature to 62-70°C, and the drying time at ≥63°C is 1.5 hours (start timing at ≥63°C and stop timing at <63°C). Screen it with an electric vibrating screen and select crystals of 20-60 mesh as high-purity trehalose crystals.

[0071] In this embodiment, the particle size of trehalose in the high-purity trehalose crystals is 20-30 mesh accounting for 75%, 30-60 mesh accounting for 20%, 60-100 mesh accounting for 5%, the glucose content is 0.016mmol / L, the trehalose purity is 99.9%, the trehalose recovery rate is 55%, of which the high-purity trehalose with a particle size of 20-60 mesh accounts for 95%.

[0072] Comparative Example 1

[0073] (1) Take a 65% trehalose solution into a crystallization tank, stabilize the temperature at 65°C, and then add 0.5% of the dry matter weight of the trehalose solution, dihydrate trehalose crystals with a size of 80 mesh.

[0074] (2) Pass cold water into the jacket of the crystallization tank, stir at 40 rpm, cool at 2°C / h, slowly cool to 30°C, keep for 9 hours, and obtain trehalose crystals. Then centrifuge in a plate centrifuge at 1000 rpm for 8 minutes. Dry in a double cone dryer, set the drying temperature to 61-69°C, and the drying time at ≥63°C is 1 hour (start timing at ≥63°C, stop timing at <63°C). Screen with an electric vibrating screen, and select crystals with 20-60 mesh as high-purity trehalose crystals.

[0075] In this embodiment, the particle size of trehalose in the high-purity trehalose crystal product is 20-60 mesh accounting for 67%, 60-100 mesh accounting for 33%, the glucose content is 0.26mmol / L, the trehalose purity is 99.7%, the trehalose recovery rate is 51%, of which the high-purity trehalose with a particle size of 20-60 mesh accounts for 67%.

[0076] Comparative Example 2

[0077] (1) Take a 65% trehalose solution into a crystallization tank, stabilize the temperature at 58°C, and add 0.5% of the dry matter weight of the trehalose solution, dihydrate trehalose crystals (seed crystals), with a size of 80 mesh.

[0078] (2) Stir and evaporate to make the seed crystal grow, the stirring speed is 40rpm, the cooling rate is 2℃ / h, slowly cool to 30℃ for crystallization, and the crystallization time is 9h. Then centrifuge in a plate centrifuge at a speed of 1000rpm for 8min. Dry in a double cone dryer, the drying temperature is set to 61-67℃, and the time of ≥63℃ is 1h. Screen with an electric vibrating screen machine, and select crystals of 20-60 mesh as high-purity trehalose crystals.

[0079] In this comparative example, the particle size of trehalose in the high-purity trehalose crystals is 20-60 mesh accounting for 30.3%, 60-100 mesh accounting for 69.7%, the glucose content is 0.26mmol / L, the trehalose purity is 99.7%, the trehalose recovery rate is 50%, of which the high-purity trehalose with a particle size of 20-60 mesh accounts for 30%.

[0080] Comparative Example 3

[0081] Take 65% trehalose and dissolve it in a crystallization tank. Stable temperature at 55°C, add 0.5% dihydrate trehalose crystals (seeds) of dry matter mass in the trehalose solution, the seed size is 300 mesh, slowly cool to 30°C at 2°C / h under 40rpm stirring, crystallization time is 9h. Then centrifuge in a plate centrifuge at a speed of 1000rpm for 8min. Dry in a double cone dryer, the drying temperature is set to 60-67°C, and the drying time is 1h at ≥63°C. Screen with an electric vibrating screen, and select crystals of 20-60 mesh as high-purity trehalose crystals.

[0082] In this comparative example, the particle size of trehalose in the high-purity trehalose crystals is 20-60 mesh accounting for 28%, 60-100 mesh accounting for 72%, the glucose content is 0.3mmol / L, the trehalose purity is 99.7%, the trehalose recovery rate is 46%, of which the high-purity trehalose with a particle size of 20-60 mesh accounts for 28%.

[0083] Comparative Example 4

[0084] Take 65% trehalose and dissolve it in a crystallization tank. Stable at 70°C, add 0.5% dihydrate trehalose crystals (seeds) of dry matter mass in the trehalose solution. The seed size is 80 mesh. Stir at 40rpm and slowly cool to 30°C at a rate of 2°C / h for crystallization. The crystallization time is 11h. Then centrifuge in a plate centrifuge at a speed of 1000rpm for 10min. Dry in a double cone dryer, the drying temperature is set to 62-70°C, and the drying time is 1.5h at ≥63°C. Screen with an electric vibrating screen and select crystals of 20-60 mesh as high-purity trehalose crystals.

[0085] In this comparative example, the particle size of trehalose in the high-purity trehalose crystals is 60-100 mesh accounting for 13%, 100-300 mesh accounting for 87%, the glucose content is 0.32mmol / L, the trehalose purity is 99.7%, the trehalose recovery rate is 45%, of which the high-purity trehalose with a particle size of 20-60 mesh accounts for 0%.

[0086] Comparative Example 5

[0087] Take 59% trehalose and dissolve it in a crystallization tank. Stable temperature at 65°C, add 0.5% dihydrate trehalose crystals (seeds) of dry matter mass in the trehalose solution, the seed size is 80 mesh, slowly cool to 30°C at 2°C / h under stirring at 40rpm for crystallization, and the crystallization time is 10h. Then centrifuge in a plate centrifuge at a speed of 1000rpm for 8min. Dry in a double cone dryer, the drying temperature is set to 59-66°C, and the drying time is 1h at ≥63°C. Screen with an electric vibrating screen and select crystals of 20-60 mesh as high-purity trehalose crystals.

[0088] In this comparative example, the particle size of trehalose in the high-purity trehalose crystals is 20-60 mesh accounting for 33%, 60-100 mesh accounting for 67%, the glucose content is 0.28mmol / L, the trehalose purity is 99.7%, the trehalose recovery rate is 49%, of which the high-purity trehalose with a particle size of 20-60 mesh accounts for 33%.

[0089] Comparative Example 6

[0090] Take 65% trehalose and dissolve it in a crystallization tank. Stable temperature at 65°C, add 0.5% dihydrate trehalose crystals (seeds) of dry matter mass in the trehalose solution, the seed size is 80 mesh, slowly cool to 40°C at 2°C / h under stirring at 40rpm for crystallization, the crystallization time is 9h. Then centrifuge in a plate centrifuge at a speed of 1000rpm for 9min. Dry in a double cone dryer, the drying temperature is set to 60-67°C, and the drying time is 1h at ≥63°C. Screen with an electric vibrating screen and select crystals of 20-60 mesh as high-purity trehalose crystals.

[0091] In this comparative example, the particle size of trehalose in the high-purity trehalose crystals is 20-60 mesh accounting for 30%, 60-100 mesh accounting for 70%, the glucose content is 0.27mmol / L, the trehalose purity is 99.7%, the trehalose recovery rate is 48%, of which the high-purity trehalose with a particle size of 20-60 mesh accounts for 30%.

[0092] Comparative Example 7

[0093] (1) Take a 65% trehalose solution into a crystallization tank, stabilize the temperature at 58°C, and add 0.5% trehalose dihydrate crystals with a size of 80 mesh in the trehalose solution.

[0094] (2) Cold water was introduced into the jacket of the crystallization tank, the stirring speed was 40 rpm, the cooling rate was 2°C / h, and the temperature was slowly lowered to 30°C for crystallization to obtain trehalose crystals.

[0095] (3) Pass hot water into the jacket of the crystallization tank with a stirring speed of 100 rpm; raise the temperature to 58° C. and maintain for 10 min to partially dissolve the crystals to obtain a trehalose mixture.

[0096] (4) Pass cold water into the jacket of the crystallization tank, slowly cool the trehalose mixture to 30°C at a stirring speed of 40 rpm and a cooling rate of 2°C / h, and keep it for 10 hours to allow the trehalose to crystallize completely. Then centrifuge it in a plate centrifuge at a speed of 1000 rpm for 9 minutes. Dry it in a double cone dryer, set the drying temperature to 60-68°C, and the drying time at ≥63°C is 1.5 hours (start timing at ≥63°C and stop timing at <63°C). Screen it with an electric vibrating screen and select crystals of 20-60 mesh as high-purity trehalose crystals.

[0097] In this comparative example, the particle size of trehalose in the high-purity trehalose crystal product is 20-60 mesh accounting for 33%, 60-100 mesh accounting for 67%, the glucose content is 0.02mmol / L, the trehalose purity is 99.8%, the trehalose recovery rate is 52%, of which the high-purity trehalose with a particle size of 20-60 mesh accounts for 33%.

[0098] As can be seen from the above embodiments, the present invention provides a high-purity trehalose and its crystallization method and application. The crystallization method of the present invention uses trehalose as the main raw material. In addition to the crystal seeds, no other substances need to be added during the crystallization process, and the obtained product has high purity and few impurities; the added crystal seeds are specially made 80-100 mesh dihydrate trehalose crystals, with a moderate number of crystal nuclei and good crystal growth; by carefully selecting the correct crystallization conditions and process parameters, the crystal size distribution is optimized and controlled. The cooling-heating process is repeated in stages under precise temperature control, which can be used to control the supersaturation of trehalose solution, improve batch consistency and optimize the formed product; trehalose crystals in the crystallization tank can perform purification and product separation at the same time, and high-purity product crystals will be formed, while impurities remain in the solution; it avoids the problems of too small crystals, different batch sizes, high impurity content and low recovery rate in the existing trehalose crystallization method, improves the particle uniformity of trehalose crystals, and the product has high purity and few impurities, stable quality and high recovery rate, which can be widely used in food, medicine, daily chemical industry and other fields.

[0099] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A method for crystallizing high-purity trehalose, characterized in that: The steps include: (1) heating the trehalose solution to a temperature of 60-65° C., adding seed crystals, and obtaining a seed sugar solution; (2) cooling the seed sugar solution to 25-30° C. to obtain trehalose crystals; (3) heating the trehalose crystals to 60-65° C. and maintaining the temperature for 10-20 minutes to obtain a trehalose mixture; (4) After repeating steps (2) to (3) 0 to 2 times, the trehalose mixture is cooled to 25 to 30° C., maintained for 9 to 10 hours, centrifuged, dried, and screened to obtain high-purity trehalose.

2. The crystallization method according to claim 1, characterized in that The initial concentration of the trehalose solution in step (1) is 62-70 wt %; The size of the seed crystals in step (1) is 80-100 mesh; The mass of the added seed crystals is 0.5-1.0% of the mass of the dry matter in the trehalose solution.

3. The crystallization method according to claim 2, characterized in that The cooling rate in step (2) is 2-3°C / h.

4. The crystallization method according to claim 3, characterized in that The centrifugal speed in step (4) is 800-1200 rpm, and the centrifugal time is 6-10 min.

5. The crystallization method according to claim 4, characterized in that The drying temperature in step (4) is 50-77°C.

6. The crystallization method according to any one of claims 1 to 5, characterized in that The proportion of high-purity trehalose of 20-60 mesh is ≥88%.

7. The high-purity trehalose obtained by the crystallization method according to any one of claims 1 to 6, characterized in that: The purity of the trehalose in the high-purity trehalose is ≥99.7% and the glucose content is <0.02 mmol / L.

8. Use of the high-purity trehalose obtained by the crystallization method according to any one of claims 1 to 6 or the high-purity trehalose according to claim 7 in the preparation of products for extending the shelf life of cell membranes, organelles and biological products.

9. Use of the high-purity trehalose obtained by the crystallization method according to any one of claims 1 to 6 or the high-purity trehalose according to claim 7 in the preparation of products for preserving and protecting food and extending the storage period of food.