CN115043887B - Trehalose crystallization method - Google Patents
Trehalose crystallization method Download PDFInfo
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- CN115043887B CN115043887B CN202210971342.2A CN202210971342A CN115043887B CN 115043887 B CN115043887 B CN 115043887B CN 202210971342 A CN202210971342 A CN 202210971342A CN 115043887 B CN115043887 B CN 115043887B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H3/00—Compounds containing only hydrogen atoms and saccharide radicals having only carbon, hydrogen, and oxygen atoms
- C07H3/04—Disaccharides
Abstract
The invention discloses a trehalose crystallization method, which belongs to the technical field of trehalose crystallization and comprises the following processes: taking the trehalose liquid to a seed crystal tank, adding seed crystals after the temperature is stable; stirring and evaporating and concentrating to pre-grow the seed crystals, and slowly cooling to the same temperature as the trehalose liquid in the main crystallization kettle; adding a surfactant into a crystallization kettle, and uniformly stirring; and adding the seed crystal sugar solution in the seed crystal tank into the trehalose solution in the crystallization kettle, carrying out stage cooling crystallization under an additional magnetic field, and then carrying out centrifugation, washing and drying to obtain the trehalose crystal. The invention reduces the problems of temperature reduction, seed crystal agglomeration, uneven dispersion and the like when adding the seed crystal, improves the uniformity of the crystal, and has high product purity and stable quality.
Description
Technical Field
The invention relates to the technical field of trehalose crystallization, and particularly relates to a trehalose crystallization method.
Background
Trehalose is a non-reducing sugar formed by condensing two glucose molecules through hemiacetal hydroxyl, has the effects of stable property, corrosion resistance, radiation resistance, oxidation resistance and the like, and has a protection effect on various bioactive substances. Due to the unique functional characteristics, the trehalose can be used as an excellent activity protective agent for protein drugs, enzymes, vaccines and other biological products, is an important component of cosmetics for keeping cell activity and moisture, and can be used as a unique food ingredient for preventing food deterioration, keeping fresh flavor of food and improving food quality, so that the trehalose is widely applied to the fields of food, medicine, daily chemical industry and the like.
Since the solubility of trehalose in water varies greatly with temperature (0.55 g trehalose per gram water at 10 ℃ C. And 3.66g trehalose per gram water at 80 ℃ C.), seed crystal is mostly added for cooling crystallization in industrial production of crystalline trehalose. At present, the seed crystal is added in a mode that the seed crystal which meets a certain size and quality is directly added in a medium temperature zone, and then the temperature is slowly reduced for crystallization. The following problems mainly exist in the conventional process: (1) When the seed crystal is directly added, the crystal nucleus is required to be as small as possible and the mass number of the seed crystal is required to be reduced in order to prevent the influence caused by the temperature difference between the seed crystal and the feed liquid. (2) At the initial stage of adding the seed crystal, the trehalose feed liquid is in the highest crystallization temperature region, the temperature is reduced by unit temperature, the crystallization amount is the largest, the crystal quality and size are the smallest, the crystal growth area is small, and the balance between the crystallization amount and the seed crystal is difficult to achieve. The crystal nucleus is easy to burst, and the product quality is reduced. In order to prevent crystal nucleus from bursting, the cooling rate needs to be controlled extremely low, the control is difficult in production, and the production time of the crystal segment is prolonged. (3) Along with the reduction of the temperature, the viscosity of the sugar solution is increased, the mass transfer rate is reduced, and the crystallization efficiency is seriously influenced.
Therefore, the development of an efficient and stable trehalose crystallization method is needed to improve the uniformity of trehalose crystals, reduce the energy consumption for operation, shorten the crystallization period, and improve the product quality.
Disclosure of Invention
In view of the above, the present invention provides a trehalose crystallization method, wherein trehalose is dissolved to absorb heat, a temperature difference exists between seed crystals and sugar solution, the problem of temperature reduction can be solved after pre-growth through evaporation and concentration in a seed crystal tank, and the problems of agglomeration and uneven dispersion can be reduced by adding a surfactant and a magnetic field in a later period.
In order to achieve the purpose, the invention adopts the following technical scheme:
a trehalose crystallization method comprises the following processes:
1) Taking the trehalose liquid to a seed crystal tank, and adding seed crystals after the temperature is stable; obtaining seed crystal sugar liquid;
2) Stirring and evaporating and concentrating to pre-grow the seed crystal, and slowly cooling to the same temperature as the trehalose liquid in the main crystallization kettle;
3) Adding a surfactant into a crystallization kettle, and uniformly stirring;
4) And adding the seed crystal sugar solution in the seed crystal tank into trehalose solution in a crystallization kettle, carrying out staged cooling crystallization under an additional magnetic field, then carrying out centrifugation to obtain trehalose, washing and drying to obtain trehalose crystals.
As a preferable technical scheme of the technical scheme, the mass concentration of the trehalose liquid in the step 1) is 64-72%.
As a preferable technical scheme of the technical scheme, the temperature in the step 1) is 58-70 ℃.
As a preferable technical scheme of the technical scheme, the size of the seed crystal in the step 1) is 200-300 meshes, and the mass of the seed crystal is 0.5-1% of the dry mass of the trehalose sugar solution in the main crystallization kettle in the step 2).
As a preferable technical scheme of the technical scheme, in the step 2), the stirring speed is 100 to 150rpm, the vacuum degree is-0.04 to-0.06 MPa, the crystal size is 180 to 200 meshes, the cooling rate is 0.1 to 1 ℃/h, the mass concentration of the sugar solution in the crystallization kettle is 60 to 70 percent, and the temperature is 53 to 67 ℃.
As a preferable technical scheme of the technical scheme, the surfactant in the step 3) is one or more of C8-C22 sucrose esters, the concentration is 10-100mg/L, and the mixing time is 10-60min.
As a preferable technical scheme of the technical scheme, the magnetic flux density of the electromagnetic field in the step 4) is 0.2-0.7T, the cooling crystallization rate is 0.3-4 ℃/h, and the discharging temperature is 20-25 ℃.
As a preferable technical scheme of the technical scheme, in the step 4), the temperature of water for washing is 7 to 15 ℃, and the water consumption is 0.5 to 1 time of the mass of the trehalose.
As a preferable embodiment of the above-mentioned means, the drying temperature in the step 4) is from 35 to 60 ℃.
Through the technical scheme, compared with the prior art, the invention has the following technical effects:
(1) The crystallization method takes the trehalose as a main raw material, and the crystallization process does not need to add solvents such as ethanol and the like, so the method is natural and environment-friendly;
(2) The addition of the sucrose ester can obviously improve the dispersity of the sugar solution, improve the crystallization efficiency and adsorb impurities in the sugar solution;
(3) The sugar solution is placed in an electromagnetic field for crystallization separation, the aggregation state, the migration speed and the direction of molecules and atoms are influenced through the action of the magnetic field, the viscosity of the sugar solution can be reduced, the crystallization speed of trehalose crystals is improved, the yield is increased under the milder crystallization condition, and the product quality is also ensured;
(4) The trehalose concentration in the crystallization kettle is low, the trehalose concentration and crystallization period is shortened, and the production energy consumption is greatly reduced;
(5) The method reduces the problems of temperature reduction, seed crystal agglomeration, uneven dispersion and the like during seed crystal addition, improves the uniformity of crystals, has high product purity and stable quality, and can be widely applied to the fields of food, medicine, daily chemical industry and the like.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The trehalose liquid is prepared by taking starch milk as a raw material and carrying out enzymatic reaction conversion. Taking 17.5 DEG beta starch milk, adjusting the pH to 5.6, adding 0.02 per mill of high-temperature resistant alpha-amylase, and carrying out liquefaction reaction at 110 ℃ to obtain maltodextrin, wherein the DE value is 8; adjusting the temperature to 58 ℃, adjusting the pH value to 6.0, and adding 1.6 per mill pullulanase for treatment for 4 hours; adjusting the temperature to 37 ℃, adjusting the pH to 6.8, adding 2% of maltooligosyl trehalose synthetase and 3% of maltooligosyl trehalose hydrolase, and stirring for reaction for 12 hours; adjusting the temperature to 58 ℃, adjusting the pH to 4.2, adding 1% of saccharifying enzyme, stirring for 8 hours, adjusting the temperature to 80 ℃, and inactivating the enzyme for 30min to obtain trehalose conversion solution; filtering the trehalose conversion solution by 20 mu m, adding 0.2% volume of activated carbon, and decoloring at 80 ℃ for 60min until the light transmittance of the clear solution is greater than 90%; cooling to 35 ℃, and filtering with ion exchange resin until the conductivity is 10 to 20 mus/cm and the light transmittance is more than 95%; carrying out chromatographic separation on the trehalose liquid at 65 ℃; then the mixture is injected into an I-effect evaporator and evaporated at the temperature of 68 to 73 ℃ and the pressure of-0.073 to-0.065 MPa until the mass concentration is 45 to 50 percent; driving into a II effect evaporator, and evaporating at the temperature of 61 to 66 ℃ and the pressure of-0.08 to-0.075 MPa until the mass concentration is 55 to 60 percent; and (3) driving into a III effect evaporator, and evaporating at 56 to 59 ℃ and-0.084 to-0.082 MPa until the mass concentration is 65 to 72 percent to obtain the trehalose solution.
The reagents are obtained from markets, wherein the high-temperature resistant alpha-amylase activity is 40000U/mL, the pullulanase activity is 2000U/mL, the maltooligosyl trehalose synthase activity is 150U/mL, and the maltooligosyl trehalose hydrolase activity is 350U/mL. The source and the brand are not required, and the method can meet the experimental requirements.
Example 1
A novel trehalose crystallization process comprises the following specific steps:
(1) Taking a 64% mass concentration trehalose solution into a seed crystal tank, stabilizing at 58 ℃, and adding 1% 200 mesh seed crystal;
(2) After the seed crystal grows to 180 meshes under the stirring of the vacuum degree of-0.04MPa and 100rpm, slowly cooling to 53 ℃ which is the same as the temperature of 60 percent of the trehalose solution in the crystallization kettle at the speed of 1 ℃/h;
(3) Adding sucrose stearate into a crystallization kettle to enable the concentration to be 20mg/L, and stirring and uniformly mixing for 10min;
(4) Adding the seed crystal in the seed crystal tank into trehalose liquid in a crystallization kettle, reducing the temperature to 50 ℃ at the speed of 0.5 ℃/h, reducing the temperature to 40 ℃ at the speed of 1 ℃/h, reducing the temperature to 30 ℃ at the speed of 2 ℃/h under the electromagnetic field with the magnetic flux density of 0.2T, finally reducing the temperature to 25 ℃ at the speed of 4 ℃/h, then centrifuging, washing with water at 7 ℃ with the mass of 0.5 time of the trehalose, and drying at 35 ℃ to obtain the trehalose crystal.
In the embodiment, the granularity of the trehalose in the trehalose finished product is 30-60 meshes accounting for 30.3%, 20-30 meshes accounting for 69.7%, and the purity of the trehalose is 99.7%.
Example 2
A novel trehalose crystallization process comprises the following specific steps:
(1) Taking 65% of trehalose solution by mass concentration into a seed crystal tank, stabilizing at 60 ℃, and adding 0.8% of 220-mesh seed crystal;
(2) After the seed crystal is grown to 190 meshes under the conditions of vacuum degree of-0.05MPa and stirring at 120rpm, the temperature is reduced to 58 ℃ at the same temperature of the trehalose liquid in the crystallization kettle with the concentration of 63.5 percent at the speed of 0.8 ℃/h;
(3) Adding sucrose laurate into a crystallization kettle to enable the prepared concentration to be 50mg/L, and stirring and uniformly mixing for 30min;
(4) Adding seed crystals in a seed crystal tank into trehalose liquid in a crystallization kettle, reducing the temperature to 53 ℃ at 0.5 ℃/h, reducing the temperature to 45 ℃ at 1 ℃/h, reducing the temperature to 35 ℃ at 2.5 ℃/h under the condition of an electromagnetic field with the magnetic flux density of 0.3T, finally reducing the temperature to 22 ℃ at 4 ℃/h, centrifuging, washing with water at 10 ℃ and the mass of 0.4 time of the trehalose, and drying at 50 ℃ to obtain the trehalose crystal.
In the embodiment, the granularity of trehalose in the trehalose finished product is 33% from 30 to 60 meshes, 67% from 20 to 30 meshes and the purity of the trehalose is 99.8%.
Example 3
A novel trehalose crystallization process comprises the following specific steps:
(1) Adding the trehalose solution with the mass concentration of 68% into a seed crystal tank, stabilizing at 65 ℃, and adding seed crystals with the content of 0.8 percent and 250 meshes;
(2) After the seed crystal is grown to 200 meshes under the stirring of the vacuum degree of-0.05MPa and 150rpm, the temperature is reduced to 60 ℃ at the same temperature of 65 percent of trehalose solution in a crystallization kettle at the speed of 0.5 ℃/h;
(3) Adding sucrose acetate isobutyrate into a crystallization kettle to enable the concentration to be 20mg/L, and stirring and uniformly mixing for 30min;
(4) Adding the seed crystal in the seed crystal tank into trehalose liquid in a crystallization kettle, reducing the temperature to 53 ℃ at 0.5 ℃/h, reducing the temperature to 45 ℃ at 1 ℃/h, reducing the temperature to 37 ℃ at 2 ℃/h, reducing the temperature to 30 ℃ at 3 ℃/h under the electromagnetic field with the magnetic flux density of 0.5T, finally reducing the temperature to 20 ℃ at 4 ℃/h, centrifuging, washing with water at 15 ℃ and the mass of 0.2 time of the trehalose, and drying at 60 ℃ to obtain the trehalose crystal.
In the embodiment, the granularity of the trehalose in the trehalose finished product is 27.2% from 30 to 60 meshes, 72.8% from 20 to 30 meshes, and the purity of the trehalose is 99.7%.
Example 4
A novel trehalose crystallization process comprises the following specific steps:
(1) Taking the trehalose solution with the mass concentration of 70 percent into a seed crystal tank, stabilizing at 68 ℃, and adding seed crystals with the content of 0.6 percent to 280 meshes;
(2) After the seed crystal grows to 200 meshes under the stirring of the vacuum degree of-0.06MPa and 130rpm, the temperature is reduced to 65 ℃ which is the same as the temperature of 68 percent of trehalose solution in the crystallization kettle at the speed of 0.3 ℃/h;
(3) Adding sucrose octaacetate into a crystallization kettle to prepare a sucrose octaacetate solution with a concentration of 100mg/L, and uniformly stirring for 30min;
(4) Adding the seed crystal in the seed crystal tank into trehalose liquid in a crystallization kettle, reducing the temperature to 60 ℃ at 0.3 ℃/h, reducing the temperature to 50 ℃ at 0.5 ℃/h, reducing the temperature to 40 ℃ at 1 ℃/h, reducing the temperature to 35 ℃ at 2 ℃/h, reducing the temperature to 30 ℃ at 3 ℃/h under the electromagnetic field with the magnetic flux density of 0.6T, finally reducing the temperature to 25 ℃ at 4 ℃/h, centrifuging, washing with water at 10 ℃ which is 0.5 times of the mass of trehalose, and drying at 50 ℃ to obtain the trehalose crystal.
In the embodiment, the trehalose in the trehalose finished product has a granularity of 30 to 60 meshes accounting for 32.1%, a granularity of 20 to 30 meshes accounting for 67.9% and a purity of 99.8%.
Example 5
A novel trehalose crystallization process comprises the following specific steps:
(1) Adding 72% trehalose solution into seed crystal tank, stabilizing at 70 deg.C, and adding 0.5%300 mesh seed crystal;
(2) After the seed crystal is grown to 180 meshes under the conditions of vacuum degree of-0.04MPa and stirring at 120rpm, the temperature is reduced to 68 ℃ at the same temperature of the trehalose liquid in the 70 percent crystallization kettle at the speed of 0.2 ℃/h;
(3) Respectively adding sucrose cinnamate and sucrose stearate into a crystallization kettle to enable the concentration of the surfactant to be 20mg/L and 50mg/L, and uniformly stirring for 60min;
(4) Adding seed crystals in a seed crystal tank into trehalose liquid in a crystallization kettle, reducing the temperature to 60 ℃ at 0.3 ℃/h, reducing the temperature to 52 ℃ at 0.5 ℃/h, reducing the temperature to 43 ℃ at 1 ℃/h, reducing the temperature to 35 ℃ at 2 ℃/h, reducing the temperature to 27 ℃ at 3 ℃/h, reducing the temperature to 21 ℃ at 4 ℃/h, centrifuging, washing with water at 7 ℃ which is 1 time of the mass of the trehalose, and drying at 40 ℃ to obtain the trehalose crystal.
In the embodiment, the granularity of the trehalose in the trehalose finished product is 37.6% in a range from 30 to 60 meshes, 62.4% in a range from 20 to 30 meshes, and the purity of the trehalose is 99.7%.
Comparative example 1
Taking a trehalose solution with the mass concentration of 73%, adding 5% of 80-mesh seed crystal at 73 ℃, stirring at 200rpm, cooling to 25 ℃ at the speed of 1 ℃/h, centrifuging, washing with water at 15 ℃ which is 1 time of the mass of trehalose, and drying at 40 ℃ to obtain trehalose crystals.
In the embodiment, the granularity of trehalose in a finished trehalose product is 42.1% from 60 to 100 meshes, 32.5% from 30 to 60 meshes, 26.4% from 20 to 30 meshes, and the purity of the trehalose is 98.6%.
Comparative example 2
Taking trehalose solution with mass concentration of 58%, adding seed crystal of 3-80 meshes at 50 ℃, cooling to 25 ℃ at the speed of 1 ℃/h under the stirring of 200rpm, centrifuging, washing with water of 7 ℃ with 1 time of the mass of trehalose, and drying at 40 ℃ to obtain trehalose crystals.
In the embodiment, the granularity of the trehalose in the trehalose finished product is 47.3% from 60 to 100 meshes, 47% from 30 to 60 meshes, 5.7% from 20 to 30 meshes and 98.3% of the purity of the trehalose.
Comparative example 3
(1) Taking the trehalose solution with the mass concentration of 70 percent into a seed crystal tank, stabilizing at 68 ℃, and adding seed crystals with the content of 0.6 percent to 280 meshes;
(2) After the seed crystal grows to 200 meshes under the stirring of the vacuum degree of-0.06MPa and 130rpm, the temperature is reduced to 65 ℃ which is the same as the temperature of 68 percent of trehalose solution in the crystallization kettle at the speed of 0.3 ℃/h;
(3) Adding sodium dodecyl benzene sulfonate into a crystallization kettle to enable the concentration to be 100mg/L, and stirring and uniformly mixing for 30min;
(4) Adding the seed crystal in the seed crystal tank into trehalose liquid in a crystallization kettle, reducing the temperature to 60 ℃ at the speed of 0.3 ℃/h, reducing the temperature to 50 ℃ at the speed of 0.5 ℃/h, reducing the temperature to 40 ℃ at the speed of 1 ℃/h, reducing the temperature to 35 ℃ at the speed of 2 ℃/h, reducing the temperature to 30 ℃ at the speed of 3 ℃/h, finally reducing the temperature to 25 ℃ at the speed of 4 ℃/h, centrifuging, washing with water at 10 ℃ with the mass of 0.5 time of trehalose, and drying at 50 ℃ to obtain the trehalose crystal.
In the embodiment, the granularity of trehalose in a finished trehalose product is 3.67% of a particle size of >100 meshes, 52.4% of a particle size of 60 to 100 meshes, 38.3% of a particle size of 30 to 60 meshes, 5.63% of a particle size of 20 to 30 meshes, and 97.6% of the purity of the trehalose.
Comparative example 4
(1) Taking the trehalose solution with the mass concentration of 70 percent into a seed crystal tank, stabilizing at 68 ℃, and adding 0.6 percent of 250-mesh seed crystal;
(2) After the seed crystal grows to 180 meshes under the stirring of the vacuum degree of-0.06MPa and 130rpm, the temperature is reduced to 65 ℃ which is the same as the temperature of 68 percent of trehalose solution in the crystallization kettle at the speed of 0.3 ℃/h;
(3) Adding the seed crystal in the seed crystal tank into trehalose liquid in a crystallization kettle, reducing the temperature to 60 ℃ at 0.3 ℃/h, reducing the temperature to 50 ℃ at 0.5 ℃/h, reducing the temperature to 40 ℃ at 1 ℃/h, reducing the temperature to 35 ℃ at 2 ℃/h, reducing the temperature to 30 ℃ at 3 ℃/h under the electromagnetic field with the magnetic flux density of 0.5T, finally reducing the temperature to 25 ℃ at 4 ℃/h, centrifuging, washing with water at 10 ℃ which is 0.5 times of the mass of trehalose, and drying at 50 ℃ to obtain the trehalose crystal.
The granularity of the trehalose in the trehalose finished product is 60-100 meshes and accounts for 22.1%, 30-60 meshes and 45.4%, 20-30 meshes and 20.4%, and the purity of the trehalose is 99.2%.
Comparative example 5
(1) Adding 72% trehalose solution into a seed crystal tank, stabilizing at 70 deg.C, and adding 0.5%300 mesh seed crystal;
(2) After the seed crystal grows to 180 meshes under the stirring of the vacuum degree of-0.04MPa and 120rpm, the temperature is reduced to 68 ℃ at the speed of 0.2 ℃/h, which is the same as the temperature of the trehalose liquid in the 70 percent crystallization kettle;
(3) Respectively adding sucrose cinnamate and sucrose stearate into a crystallization kettle to enable the concentration of the surfactant to be 20mg/L and 50mg/L, and uniformly stirring for 60min;
(4) Adding seed crystals in a seed crystal tank into trehalose liquid in a crystallization kettle, reducing the temperature to 55 ℃ at 0.8 ℃/h, reducing the temperature to 50 ℃ at 1 ℃/h, reducing the temperature to 40 ℃ at 2 ℃/h, reducing the temperature to 35 ℃ at 3 ℃/h, reducing the temperature to 25 ℃ at 4 ℃/h, reducing the temperature to 20 ℃ at 5 ℃/h, centrifuging, washing with water at 7 ℃ which is 1 time of the mass of the trehalose, and drying at 40 ℃ to obtain the trehalose crystal.
In the embodiment, the granularity of trehalose in a trehalose finished product is 12.2% of >100 meshes, 49.4% of 60-100 meshes, 30.1% of 30-60 meshes, 8.3% of 20-30 meshes and 97.2% of trehalose purity.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (6)
1. A trehalose crystallization method is characterized by comprising the following processes:
1) Taking the trehalose liquid into a seed crystal tank, adding seed crystals after the temperature is stable, wherein the size of the seed crystals is 200-300 meshes, and obtaining seed crystal sugar liquid; the mass concentration of the trehalose liquid is 64-72%;
2) Stirring and evaporating and concentrating to pre-grow the seed crystals, and slowly cooling to the same temperature as the trehalose liquid in the main crystallization kettle;
3) Adding a surfactant into a crystallization kettle, and uniformly stirring; the surfactant is one or more of sucrose esters C8-C22, the concentration is 10 to 100mg/L, and the mixing time is 10 to 60min;
4) Adding the seed crystal sugar solution in the seed crystal tank into trehalose solution in a crystallization kettle, carrying out stage cooling crystallization under an additional magnetic field, then centrifuging to obtain trehalose, washing and drying to obtain trehalose crystals; the magnetic flux density of the electromagnetic field is 0.2-0.7T, the cooling crystallization rate is 0.3-4 ℃/h, and the discharging temperature is 20-25 ℃.
2. The method for crystallizing trehalose according to claim 1, wherein the temperature in step 1) is from 58 ℃ to 70 ℃.
3. The trehalose crystallization method according to claim 1, wherein in the step 2), the stirring rotation speed is 100 to 150rpm, the vacuum degree is-0.04 to-0.06 MPa, the crystal size is 180 to 200 meshes, the cooling rate is 0.1 to 1 ℃/h, the mass concentration of the sugar solution in the crystallization kettle is 60 to 70 percent, and the temperature is 53 to 67 ℃.
4. The trehalose crystallization method according to claim 1, wherein the mass of the seed crystal in the step 1) is 0.5-1% of the dry mass of the trehalose sugar solution in the main crystallization kettle in the step 2).
5. The method for crystallizing trehalose according to claim 1, wherein the temperature of water for washing in step 4) is from 7 to 15 ℃, and the amount of water for washing is from 0.5 to 1 time the mass of trehalose.
6. The process for crystallizing trehalose according to claim 1, wherein the drying temperature in step 4) is from 35 ℃ to 60 ℃.
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| US5403727A (en) * | 1990-11-15 | 1995-04-04 | Kabushiki Kaisha Hayashibara Seibutsu Kagaku Kenkyujo | Process for preparing neotrehalose and its uses |
| US5916881A (en) * | 1996-10-07 | 1999-06-29 | Kabushiki Kaisha Hayashibara Seibutsu Kagaku Kenkyujo | High trehalose content syrup |
| CN102924539A (en) * | 2012-10-31 | 2013-02-13 | 南京工业大学 | Method for preparing trehalose crystals |
| CN106381347A (en) * | 2016-11-22 | 2017-02-08 | 保龄宝生物股份有限公司 | Crystallization technical method for industrially producing trehalose |
| CN108774273A (en) * | 2018-08-24 | 2018-11-09 | 湖南汇升生物科技有限公司 | A kind of trehalose crystallization processes |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5403727A (en) * | 1990-11-15 | 1995-04-04 | Kabushiki Kaisha Hayashibara Seibutsu Kagaku Kenkyujo | Process for preparing neotrehalose and its uses |
| US5916881A (en) * | 1996-10-07 | 1999-06-29 | Kabushiki Kaisha Hayashibara Seibutsu Kagaku Kenkyujo | High trehalose content syrup |
| CN102924539A (en) * | 2012-10-31 | 2013-02-13 | 南京工业大学 | Method for preparing trehalose crystals |
| CN106381347A (en) * | 2016-11-22 | 2017-02-08 | 保龄宝生物股份有限公司 | Crystallization technical method for industrially producing trehalose |
| CN108774273A (en) * | 2018-08-24 | 2018-11-09 | 湖南汇升生物科技有限公司 | A kind of trehalose crystallization processes |
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