CN110872332B - Crystallization process of psicose - Google Patents
Crystallization process of psicose Download PDFInfo
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- CN110872332B CN110872332B CN201911015344.9A CN201911015344A CN110872332B CN 110872332 B CN110872332 B CN 110872332B CN 201911015344 A CN201911015344 A CN 201911015344A CN 110872332 B CN110872332 B CN 110872332B
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Abstract
The invention discloses a crystallization process of psicose, which comprises the following steps: (1) primary crystallization by using evaporative crystallization equipment; (2) deep crystallization by using cooling crystallization equipment; the process comprises two-step crystallization, including primary crystallization by using an evaporation crystallization device and deep crystallization by using a cooling crystallization device, and can obtain allulose crystals with larger crystal size without using an organic solvent.
Description
Technical Field
The invention belongs to the technical field of allulose, and particularly relates to a crystallization process of allulose.
Background
With the increasing living standard, people pay more attention to food safety, and various functional foods and low-calorie sweeteners have entered the market and received high attention from consumers. Psicose is a naturally occurring but very low-calorie functional sweetener that has a sweetness of 70% of sucrose but an energy of only 0.3% of sucrose and can be used as a sweetener for low-calorie diet foods. Meanwhile, D-psicose has a function of inhibiting the activity of enzymes involved in lipid synthesis in the liver, contributes to the reduction of abdominal fat accumulation, can control body weight to a certain extent, and can be used in various functional foods such as health foods. In addition, the psicose can improve the flavor, appearance and the like of the food and prolong the shelf life of the food. Therefore, allulose, a healthy and safe low-calorie functional sweetener, has gained increasing attention and is one of the most market-competitive new sweeteners. Psicose has a CAS number of 551-68-8. The formal approval of psicose by the U.S. Food and Drug Administration (FDA) in 2014 was Generally Recognized As Safe (GRAS), allowing its use in foods, dietary supplements, and pharmaceutical formulations.
It is reported that allulose powder can be obtained by the method of ethanol precipitation and the method of direct cooling crystallization. However, the use of a large amount of ethanol requires expensive equipment for explosion prevention and recovery of the product, and is liable to cause other problems such as stirrer failure caused by the use of an organic solvent and the presence of foreign materials in the recovered product. And when the fine allulose powder product is obtained, a large amount of problems and losses exist in the processes of dehydration, washing and drying, and the crystallization process of the direct cooling crystallization method is too long in time and low in crystallization yield. Therefore, a method of producing psicose in a crystal form rather than a fine powder form and in high yield and high purity is required.
Disclosure of Invention
The present invention aims to provide a process for the crystallization of psicose, which comprises two-step crystallization including preliminary crystallization using an evaporative crystallization apparatus and deep crystallization using a cooling crystallization apparatus, whereby psicose crystals having a large crystal size can be obtained without using an organic solvent.
The above object of the present invention is achieved by the following technical solutions: a crystallization process of psicose, comprising the following steps:
(1) Primary crystallization is carried out by utilizing evaporative crystallization equipment;
(2) Deep crystallization is carried out by utilizing cooling crystallization equipment;
the primary crystallization performed by using the evaporative crystallization equipment in the step (1) specifically comprises the following steps: selecting allulose sugar solution, adding allulose seed crystals, adjusting the temperature to be 40-60 ℃, performing evaporative crystallization in an evaporative crystallization device in a manner of adding allulose sugar solution while evaporating, and performing primary crystallization to obtain a primary crystallization massecuite containing allulose crystals;
the deep crystallization performed by using the cooling crystallization equipment in the step (2) specifically comprises the following steps: and placing the primarily crystallized massecuite in cooling crystallization equipment, adjusting the temperature of deep crystallization to be uniformly decreased from 40-60 ℃ to 25-35 ℃ for cooling crystallization to obtain deep-crystallized massecuite, and centrifuging, drying and screening the deep-crystallized massecuite to obtain the psicose crystal.
In the crystallization process of psicose described above:
preferably, the dry matter concentration of the allulose sugar solution in the step (1) is 80-84% (w/w), and the purity is more than 98.5% (w/w).
Wherein the dry matter concentration and purity of the allulose sugar solution can be measured by a saccharimeter and HLPC, respectively.
Further, the dry matter concentration of the allulose sugar solution in step (1) is preferably 83% (w/w), and when the dry matter concentration of evaporative crystallization is 84% (w/w) or more, the massecuite obtained by final crystallization may block the pipeline.
Preferably, the allulose seed crystal in the step (1) is the allulose seed crystal treated by a seed crystal mill, and the addition amount of the allulose seed crystal accounts for 0.01-1% of the total mass of the allulose sugar solution.
Preferably, the evaporative crystallization device in step (1) comprises a conventional commercial device with similar functions such as a sugar boiling tank, a vacuum evaporative crystallizer, an external circulation concentrator or a forced circulation vacuum evaporative crystallizer.
Further, the temperature of the primary crystallization of the psicose sugar solution in the step (1) is preferably 45-50 ℃, and when the temperature of evaporation crystallization is lower than 45 ℃ or higher than 50 ℃, the crystallization yield is low and the average size of crystals is small.
Preferably, the time for the evaporative crystallization in the step (1) is 8 to 16 hours.
Further, the time for the evaporation crystallization in step (1) of the present application, i.e., the time for holding the primary crystallization, is preferably 12 hours, and when the time for holding the primary crystallization is less than or greater than 12 hours, the yield of the crystallization is low, and the average size of the crystals is small.
Preferably, the concentration of the primary crystallization massecuite in the step (1) is 15-20% (w/w), namely the mass percentage of the psicose crystals in the psicose crystal primary crystallization massecuite is 15-20%.
Preferably, the cooling crystallization device in step (2) comprises a horizontal cooling crystallizer, a freezing crystallizer, a cooling crystallizer or a vertical cooling crystallizer, and the like.
Preferably, the cooling crystallization time in the step (2) is 36 to 60 hours.
Further, the cooling crystallization time in the step (2) is preferably about 48 hours, and when the time for the crystallization process is less than 48 hours or more than 48 hours, the yield of the crystals is low.
Preferably, the concentration of the deep-crystallization massecuite in the step (2) is 47-56% (w/w), namely the mass percentage of the psicose crystals in the deep-crystallization massecuite is 47-56%.
Preferably, the purity of the allulose crystals in step (2) is 99.5% (w/w) or more, and the crystallization yield is 47 to 56% (w/w). The crystallization yield, namely the mass of the psicose crystals accounts for the mass percentage of the initial psicose sugar solution.
Compared with the prior art, the invention has the following beneficial effects:
(1) The method utilizes evaporative crystallization equipment to carry out primary crystallization, and improves the grain size of crystals in the evaporative crystallization process, thereby obtaining large-particle crystals;
(2) The method improves the crystallization yield by deep crystallization carried out by cooling crystallization equipment, and controlling the speed and time of cooling, and a crystallization mode combining primary crystallization carried out by evaporation crystallization equipment and deep crystallization carried out by cooling crystallization equipment, wherein the crystallization yield can reach over 53 percent under the optimal condition;
(3) The method can save the mode of using a large amount of organic solvent ethanol for precipitation, and can reduce the investment of expensive equipment for explosion prevention and product collection, thereby reducing the production cost.
Detailed Description
The present invention will be further described with reference to specific embodiments, but the scope of the invention as claimed is not limited to the following embodiments.
The raw materials used in the following examples are all commercially available products unless otherwise specified.
Example 1
Primary crystallization: allulose sugar solution with the purity of 98.9% (w/w) and the dry matter concentration of 80% (w/w) is evaporated and crystallized in a vacuum evaporation crystallizer, a small amount of allulose seed crystals processed by a seed crystal mill are added to the allulose sugar solution with the dry matter concentration of 80% (w/w) at the temperature of 45-50 ℃, the allulose sugar solution with the dry matter concentration of 80% is supplemented while evaporation is carried out for evaporation and crystallization, the dry matter concentration is kept at 83% (w/w), the evaporation and crystallization time is 12 hours, and the crystallization rate (concentration of the primary crystallization sugar paste) is 15-20% (w/w), and then the next step of cooling and crystallization is carried out.
Deep crystallization: the allulose massecuite after primary crystallization automatically flows to a horizontal cooling crystallizer for deep crystallization, the deep crystallization temperature is uniformly decreased from 45-50 ℃ to 35 ℃ for crystallization, the time used in the crystallization process is 48 hours, the concentration of the crystallized massecuite is 48-56% (w/w), then the crystallized massecuite is centrifuged, dried and screened, and allulose crystals and mother liquor are centrifuged, so that an allulose crystal product with the purity of 99.9% (w/w) and the average grain size of 352.5 mu m is obtained, and the crystallization yield is 53.6%.
Example 2
The primary crystallization is as follows: allulose sugar solution with the purity of 98.9% (w/w) and the dry matter concentration of 80% (w/w) is evaporated and crystallized in a vacuum evaporation crystallizer, a small amount of allulose seed crystals processed by a seed crystal mill are added to the allulose sugar solution with the dry matter concentration of 80% (w/w) at the temperature of 45-50 ℃, allulose sugar solution with the dry matter concentration of 80% (w/w) is added while evaporation is carried out for evaporation and crystallization, the dry matter concentration is kept at 83% (w/w), the evaporation and crystallization time is 8 hours, the crystallization rate is 15-20% (w/w), and then the solution enters the next step for cooling and crystallization.
Deep crystallization: the allulose massecuite after primary crystallization automatically flows to a horizontal cooling crystallizer for deep crystallization, the deep crystallization temperature is uniformly decreased from 45-50 ℃ to 35 ℃ for crystallization, the time used in the crystallization process is 48 hours, the concentration of the crystallized massecuite is 48-56% (w/w), then the crystallized massecuite is centrifuged, dried and screened, and allulose crystals and mother liquor are centrifuged, so that an allulose crystal product with the purity of 99.7% (w/w) and the average grain size of 175.5 mu m is obtained, and the crystallization yield is 48.4%.
Example 3
Primary crystallization: allulose sugar solution with the purity of 98.9% (w/w) and the dry matter concentration of 80% (w/w) is evaporated and crystallized in a vacuum evaporation crystallizer, a small amount of allulose seed crystals processed by a seed crystal mill are added to the allulose sugar solution with the dry matter concentration of 80% (w/w) at the temperature of 45-50 ℃, and the allulose sugar solution with the dry matter concentration of 80% (w/w) is added while evaporation is carried out for evaporation and crystallization, the dry matter concentration is kept to be 83% (w/w), the evaporation and crystallization time is 16 hours, and the next step of cooling and crystallization is carried out after the crystallization rate reaches 15-20% (w/w).
Deep crystallization: the allulose massecuite after primary crystallization automatically flows to a horizontal cooling crystallizer for deep crystallization, the deep crystallization temperature is uniformly decreased from 45-50 ℃ to 35 ℃ for crystallization, the time used in the crystallization process is 48 hours, the concentration of the crystallized massecuite is 48-56% (w/w), then the crystallized massecuite is centrifuged, dried and sieved, and allulose crystals and mother liquor are centrifuged, so that an allulose crystal product with the purity of 99.9% (w/w) and the average grain size of 267.5 mu m is obtained, and the crystallization yield is 50.8%.
Example 4
Primary crystallization: allulose sugar solution with the purity of 98.9% (w/w) and the dry matter concentration of 80% (w/w) is evaporated and crystallized in a vacuum evaporation crystallizer, a small amount of allulose seed crystals processed by a seed crystal mill are added to the allulose sugar solution with the dry matter concentration of 80% (w/w) at the temperature of 40-45 ℃, the allulose sugar solution with the dry matter concentration of 80% (w/w) is supplemented while evaporation is carried out for evaporation and crystallization, the dry matter concentration is kept to be 83% (w/w), the evaporation and crystallization time is 12 hours, and the next step of cooling and crystallization is carried out after the crystallization rate reaches 15-20% (w/w).
Deep crystallization: the allulose massecuite after primary crystallization automatically flows to a horizontal cooling crystallizer for deep crystallization, the deep crystallization temperature is uniformly decreased from 40-45 ℃ to 35 ℃ for crystallization, the time used in the crystallization process is 48 hours, after the concentration of the crystallized massecuite is 48-56% (w/w), the crystallized massecuite is centrifuged, dried and screened, and allulose crystals and mother liquor are centrifuged, so that an allulose crystal product with the purity of 99.7% (w/w) and the average grain size of 195.5 mu m is obtained, and the crystallization yield is 48.6%.
Example 5
Primary crystallization: allulose sugar solution with the purity of 98.9% (w/w) and the dry matter concentration of 80% (w/w) is evaporated and crystallized in a vacuum evaporation crystallizer, a small amount of allulose seed crystals processed by a seed crystal mill are added to the allulose sugar solution with the dry matter concentration of 80% (w/w) at the temperature of 50-55 ℃, allulose sugar solution with the dry matter concentration of 80% (w/w) is added while evaporation is carried out for evaporation and crystallization, the dry matter concentration is kept to be 83% (w/w), the evaporation and crystallization time is 12 hours, and the next step of cooling and crystallization is carried out after the crystallization rate reaches 15-20% (w/w).
Deep crystallization: the allulose massecuite after primary crystallization automatically flows to a horizontal cooling crystallizer for deep crystallization, the deep crystallization temperature is uniformly decreased from 50 ℃ to 55 ℃ to 35 ℃ for crystallization, the time used in the crystallization process is 48 hours, the concentration of the crystallized massecuite is 48% -56% (w/w), then the crystallized massecuite is centrifuged, dried and sieved, and allulose crystals and mother liquor are centrifuged, so that an allulose crystal product with the purity of 99.7% (w/w) and the average grain size of 231.5 mu m is obtained, and the crystallization yield is 51.3%.
Example 6
Primary crystallization: allulose sugar solution with the purity of 98.9% (w/w) and the dry matter concentration of 80% (w/w) is evaporated and crystallized in a vacuum evaporation crystallizer, a small amount of allulose seed crystals processed by a seed crystal mill are added to the allulose sugar solution with the dry matter concentration of 80% (w/w) at 55-60 ℃, the allulose sugar solution with the dry matter concentration of 80% (w/w) is added while evaporation is carried out for evaporation and crystallization, the dry matter concentration is kept to be 83% (w/w), the evaporation and crystallization time is 12 hours, and the crystallization rate reaches 15-20% (w/w) and then the solution enters the next step for cooling and crystallization.
Deep crystallization: the allulose massecuite after primary crystallization automatically flows to a horizontal cooling crystallizer for deep crystallization, the deep crystallization temperature is uniformly decreased from 55 ℃ to 60 ℃ to 35 ℃ for crystallization, the time used in the crystallization process is 48 hours, after the concentration of the crystallized massecuite is 48% -56% (w/w), the crystallized massecuite is centrifuged, dried and screened, and allulose crystals and mother liquor are centrifuged, so that an allulose crystal product with the purity of 99.7% (w/w) and the average grain size of 202.5 mu m is obtained, and the crystallization yield is 50.2%.
Example 7
Primary crystallization: allulose sugar liquid with the purity of 98.9% (w/w) and the dry matter concentration of 80% (w/w) is evaporated and crystallized in a vacuum evaporation crystallizer, a small amount of allulose seed crystals processed by a seed crystal mill are added to the allulose sugar liquid with the dry matter concentration of 80% (w/w) at 45-50 ℃, evaporation and addition of allulose sugar liquid with the dry matter concentration of 80% (w/w) are carried out, evaporation and crystallization are carried out, the dry matter concentration is kept at 83% (w/w), the evaporation and crystallization time is 12 hours, and the crystallization rate reaches 15-20% (w/w), and then the solution is cooled and crystallized in the next step.
Deep crystallization: the allulose massecuite after primary crystallization automatically flows to a horizontal cooling crystallizer for deep crystallization, the deep crystallization temperature is uniformly decreased from 45-50 ℃ to 35 ℃ for crystallization, the time used in the crystallization process is 36 hours, the concentration of the crystallized massecuite is 48-56% (w/w), then the crystallized massecuite is centrifuged, dried and screened, and allulose crystals and mother liquor are centrifuged, so that an allulose crystal product with the purity of 99.7% (w/w) and the average grain size of 245.5 mu m is obtained, and the crystallization yield is 47.6%.
Example 8
Primary crystallization: allulose sugar solution with the purity of 98.9% (w/w) and the dry matter concentration of 80% (w/w) is evaporated and crystallized in a vacuum evaporation crystallizer, a small amount of allulose seed crystals processed by a seed crystal mill are added to the allulose sugar solution with the dry matter concentration of 80% (w/w) at the temperature of 45-50 ℃, and the allulose sugar solution with the dry matter concentration of 80% (w/w) is added while evaporation is carried out for evaporation and crystallization, the dry matter concentration is kept to be 83% (w/w), the evaporation and crystallization time is 12 hours, and the crystallization rate reaches 15-20% (w/w) and then the solution enters the next step for cooling and crystallization.
Deep crystallization: the allulose massecuite after primary crystallization automatically flows to a horizontal cooling crystallizer for deep crystallization, the deep crystallization temperature is uniformly decreased from 45-50 ℃ to 35 ℃ for crystallization, the time used in the crystallization process is 60 hours, the concentration of the crystallized massecuite is 48-56% (w/w), then the crystallized massecuite is centrifuged, dried and screened, and allulose crystals and mother liquor are centrifuged, so that an allulose crystal product with the purity of 99.7% (w/w) and the average grain size of 235.5 mu m is obtained, and the crystallization yield is 49.1%.
Example 9
The primary crystallization is as follows: allulose sugar solution with the purity of 98.9% (w/w) and the dry matter concentration of 80% (w/w) is evaporated and crystallized in a vacuum evaporation crystallizer, a small amount of allulose seed crystals processed by a seed crystal mill are added to the allulose sugar solution with the dry matter concentration of more than 80% (w/w) at the temperature of 45-50 ℃, allulose solution with the dry matter concentration of 80% (w/w) is supplemented while evaporation is carried out for evaporation and crystallization, the dry matter concentration is kept at 83% (w/w), the evaporation and crystallization time is 12 hours, the crystallization rate is 15-20% (w/w), and then the solution enters the next step for cooling and crystallization.
Deep crystallization: the allulose massecuite after primary crystallization automatically flows to a horizontal cooling crystallizer for deep crystallization, the deep temperature is uniformly decreased from 45-50 ℃ to 30 ℃ for crystallization, the time used in the crystallization process is 48 hours, the concentration of the crystallized massecuite is 48-56% (w/w), then the crystallized massecuite is centrifuged, dried and sieved, and allulose crystals and mother liquor are centrifuged, so that an allulose crystal product with the purity of 99.8% (w/w) and the average grain size of 265.5 mu m is obtained, and the crystallization yield is 51.2%.
Example 10
The primary crystallization is as follows: allulose sugar solution with the purity of 98.9% (w/w) and the dry matter concentration of 80% (w/w) is evaporated and crystallized in a vacuum evaporation crystallizer, a small amount of allulose seed crystals processed by a seed crystal mill are added to the allulose sugar solution with the dry matter concentration of 80% (w/w) at the temperature of 45-50 ℃, and the allulose sugar solution with the dry matter concentration of 80% (w/w) is added while evaporation is carried out for evaporation and crystallization, the dry matter concentration is kept to be 83% (w/w), the evaporation and crystallization time is 12 hours, and the crystallization rate reaches 15-20% (w/w) and then the solution enters the next step for cooling and crystallization.
Deep crystallization: the allulose massecuite after primary crystallization automatically flows to a horizontal cooling crystallizer for deep crystallization, the deep temperature is uniformly decreased from 45-50 ℃ to 25 ℃ for crystallization, the time used in the crystallization process is 48 hours, after the concentration of the crystallized massecuite is 48-56% (w/w), the crystallized massecuite is centrifuged, dried and screened, and allulose crystals and mother liquor are centrifuged, so that an allulose crystal product with the purity of 99.7% (w/w) and the average grain size of 251.5 mu m is obtained, and the crystallization yield is 50.2%.
Example 11
The primary crystallization is as follows: allulose sugar liquid with the purity of 98.5% (w/w) and the dry matter concentration of 80% (w/w) is evaporated and crystallized in a vacuum evaporation crystallizer, a small amount of allulose seed crystals processed by a seed crystal mill are added to the allulose sugar liquid with the dry matter concentration of 80% (w/w) at 45-50 ℃, evaporation and addition of allulose sugar liquid with the dry matter concentration of 80% (w/w) are carried out, evaporation and crystallization are carried out, the dry matter concentration is kept at 83% (w/w), the evaporation and crystallization time is 12 hours, and the crystallization rate reaches 15-20% (w/w), and then the solution is cooled and crystallized in the next step.
Deep crystallization: the allulose massecuite after primary crystallization automatically flows to a horizontal cooling crystallizer for deep crystallization, the deep temperature is uniformly decreased from 45-50 ℃ to 35 ℃ for crystallization, the time used in the crystallization process is 48 hours, the concentration of the crystallized massecuite is 48-56% (w/w), then the crystallized massecuite is centrifuged, dried and screened, and allulose crystals and mother liquor are centrifuged, so that an allulose crystal product with the purity of 99.5% (w/w) and the average grain size of 350.5 mu m is obtained, and the crystallization yield is 53.2%.
Example 12
The primary crystallization is as follows: allulose sugar solution with the purity of 99% (w/w) and the dry matter concentration of 80% (w/w) is evaporated and crystallized in a vacuum evaporation crystallizer, a small amount of allulose seed crystals processed by a seed crystal mill are added to the allulose sugar solution with the dry matter concentration of 80% (w/w) at the temperature of 45-50 ℃, the allulose sugar solution with the dry matter concentration of 80% (w/w) is supplemented while evaporation is carried out for evaporation and crystallization, the dry matter concentration is kept to be 83% (w/w), the evaporation and crystallization time is 12 hours, and the crystallization rate reaches 15-20% (w/w), and then the solution enters the next step for cooling and crystallization.
Deep crystallization: the allulose massecuite after primary crystallization automatically flows to a horizontal cooling crystallizer for deep crystallization, the deep temperature is uniformly decreased from 45-50 ℃ to 35 ℃ for crystallization, the time used in the crystallization process is 48 hours, the concentration of the crystallized massecuite is 48-56% (w/w), then the crystallized massecuite is centrifuged, dried and sieved, and allulose crystals and mother liquor are centrifuged, so that an allulose crystal product with the purity of 99.9% (w/w) and the average grain size of 358.5 mu m is obtained, and the crystallization yield is 53.7%.
Comparative example 1
Primary crystallization: allulose sugar solution with the purity of 98.9% (w/w) and the dry matter concentration of 80% (w/w) is evaporated and crystallized in a vacuum evaporation crystallizer, a small amount of allulose seed crystals processed by a seed crystal mill are added to the allulose sugar solution with the dry matter concentration of 80% (w/w) at the temperature of 45-50 ℃, and the allulose sugar solution with the dry matter concentration of 80% (w/w) is added while evaporation is carried out for evaporation and crystallization, the dry matter concentration is kept at 85% (w/w), the evaporation and crystallization time is 12 hours, and the crystallization rate reaches 15-20% (w/w) and then the solution enters the next step for cooling and crystallization.
Deep crystallization: the allulose massecuite after primary crystallization automatically flows to a horizontal cooling crystallizer for deep crystallization, the deep crystallization temperature is uniformly decreased from 45-50 ℃ to 35 ℃ for crystallization, the time used in the crystallization process is 48 hours, after the concentration of the crystallized massecuite is 48-56% (w/w), the crystallized massecuite is centrifuged, dried and screened, and allulose crystals and mother liquor are centrifuged, so that an allulose crystal product with the purity of 99.9% (w/w) and the average grain size of 215.5 mu m is obtained, and the crystallization yield is 55.1%.
Comparative example 2
Directly cooling and crystallizing by a horizontal cooling crystallizer: directly evaporating the allulose sugar solution with the purity of 98.9% (w/w) and the dry matter concentration of 80% (w/w) by using an evaporation device until the dry matter concentration is 83% (w/w), automatically flowing to a cooling crystallization device, adding a small amount of allulose seed crystals treated by a seed crystal mill for cooling crystallization, wherein the temperature of the cooling crystallization device is uniformly decreased from 45-50 ℃ to 35 ℃ for crystallization, the time used in the crystallization process is 60 hours, after a crystallized massecuite is obtained, centrifuging, drying and screening the crystallized massecuite, and centrifuging allulose crystals and mother liquor to obtain an allulose crystal product with the purity of 99.8% (w/w) and the average grain size of 167.5 microns, wherein the crystallization yield is 42.8%.
Comparative example 3
Directly cooling and crystallizing by a horizontal cooling crystallizer: the allulose sugar solution with the purity of 98.9% (w/w) and the dry matter concentration of 80% (w/w) is directly evaporated by an evaporation device to the dry matter concentration of 83% (w/w), and then flows to a cooling crystallization device automatically, a small amount of allulose seed crystals treated by a seed crystal mill are added to carry out cooling crystallization, the temperature of the cooling crystallization device is uniformly decreased from 45 ℃ to 50 ℃ to 35 ℃ for crystallization, the time used in the crystallization process is 80 hours, after a crystallized massecuite is obtained, the crystallized massecuite is centrifuged, dried and sieved, and the allulose crystals and mother liquor are centrifuged, so that an allulose crystal product with the purity of 99.7% (w/w) and the average grain size of 204.5 mu m is obtained, and the yield is 44.6%.
Example 1 the grain size and crystallization yield of psicose crystals were measured for comparison between examples 2 and 3, only for the difference in the time for which the evaporative crystallization was maintained, to give table 1.
Table 1 comparison of parameters and experimental results for example 1 and example 3
As can be seen from Table 1, the size of the crystal of example 1 and the crystallization yield were both optimized by making a comparison while changing the time for maintaining the evaporative crystallization.
Example 1 the grain size and crystallization yield of psicose crystals were measured by comparing the parameters of example 4, example 5 and example 6, respectively, only for the difference in the temperature maintained during evaporation of the evaporative crystals, to give table 2.
Table 2 comparison of parameters and experimental results for example 1, example 4, example 5 and example 6
As can be seen from Table 2, the comparison was made by changing the temperature maintained during the evaporation for the evaporative crystallization, and it was found that the crystal size and the crystallization yield of the crystal of example 1 were both optimum.
Example 1 the grain size and crystallization yield of psicose crystals were measured by comparing the parameters of example 7 and example 8, respectively, only for the difference in the time taken for cooling the crystallization process, and table 3 was obtained.
Table 3 comparison of parameters and experimental results for example 1, example 7 and example 8
As can be seen from Table 3, when the time taken for the cooling crystallization process was changed for comparison, the size of the crystals of example 1 and the crystallization yield were both optimized.
Example 1 the grain size and crystallization yield of psicose crystals were measured by comparing the parameters of example 9 and example 10, respectively, only for the difference in the final temperature of the cooling crystallization process, and table 4 was obtained.
Table 4 comparison of parameters and experimental results for example 1, example 9 and example 10
As can be seen from Table 4, the crystal size and the crystallization yield of example 1 were optimized by making a comparison while changing the final temperature of the cooling crystallization process.
Example 1 psicose crystal grain size and crystallization yield were measured separately, comparing the parameters of example 11 and example 12, only for the difference in initial psicose purity, to give table 5.
Table 5 comparison of parameters and experimental results for example 1, example 11 and example 12
As can be seen from Table 5, when the comparison was made by changing the initial allulose purity, the crystal size and the crystallization yield were both optimum as a result of crystallization with an allulose purity of 98.5% (w/w) or more.
Comparison of the parameters of example 1 with those of comparative example 1, the crystal grain size and the crystallization yield of psicose were measured for the difference in concentration of evaporated crystals to dry matter, respectively, to obtain Table 6.
Table 6 comparison of parameters and experimental results of example 1 and comparative example 1
As can be seen from Table 6, the crystal size and the crystal yield of comparative example 1 were slightly small and the crystal yield was high when the concentration of evaporated crystals evaporated to a dry matter was changed for comparison, but the crystal massecuite was low in fluidity and clogged the pipeline due to the too high concentration of comparative example 1, which was not suitable for mass production in an industrial scale, so that the crystal size and the crystal yield of example 1 were also optimum.
Example 1 the grain size and the crystallization yield of the psicose crystals were measured by comparing the parameters of comparative example 2 and comparative example 3, respectively, only to reduce the difference between the time for the evaporation crystallization step and the time for directly performing the cooling crystallization, to obtain table 7.
TABLE 7 comparison of parameters and results of experiments for example 1, comparative example 2 and comparative example 3
As can be seen from Table 7, the size of the crystal of example 1 and the crystallization yield were optimized by changing the time for reducing the evaporative crystallization step and the time for directly cooling the crystallization.
In the above embodiment:
the evaporative crystallization equipment can also comprise a conventional commercial equipment with similar functions such as a sugar boiling tank, an external circulation concentrator or a forced circulation vacuum evaporative crystallizer besides the vacuum evaporative crystallizer.
The cooling crystallization equipment may include conventional commercial equipment with similar functions such as a freezing crystallization tank, a cooling crystallizer or a vertical cooling crystallizer in addition to the horizontal cooling crystallizer.
The allulose seed crystals may be added in an amount of from about 0.01% to about 1% of the total mass of the allulose solution.
The dry matter concentration of the allulose liquid can be 80-84% (w/w) besides 80%, and the purity is more than 98.5% (w/w).
The above-mentioned embodiments are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above-mentioned embodiments, for example, the evaporative crystallization apparatus may include a conventional commercial apparatus having similar functions such as a sugar boiling tank, an external circulation concentrator or a forced circulation vacuum evaporative crystallizer in addition to the vacuum evaporative crystallizer, and the cooling crystallization apparatus may also include a conventional commercial apparatus having similar functions such as a freezing crystallization tank, a cooling crystallizer or a vertical cooling crystallizer in addition to the horizontal cooling crystallizer, and any other changes, modifications, substitutions, combinations and simplifications which do not depart from the spirit and principle of the present invention should be regarded as equivalent replacement modes, and all of which are included in the protection scope of the present invention.
Claims (3)
1. A crystallization process of psicose is characterized by comprising the following steps:
primary crystallization: subjecting an allulose sugar solution having a purity of 98.9% w/w and a dry matter concentration of 80% w/w to evaporative crystallization in a vacuum evaporative crystallizer, adding a small amount of allulose seeds treated by a seed mill to the allulose sugar solution having a dry matter concentration of 80% w/w at 45 ℃ to 50 ℃, adding the allulose sugar solution having a dry matter concentration of 80% while evaporating, and subjecting the solution to evaporative crystallization while compensating for the allulose sugar solution having a dry matter concentration of 80%, keeping the dry matter concentration of 83% w/w, and subjecting the solution to evaporative crystallization for 12 hours so that the crystallization rate reaches 15% to 20% w/w, followed by subjecting the solution to further cooling crystallization;
deep crystallization: the psicose after the primary crystallization was self-flowed to a horizontal cooling crystallizer to be deep-crystallized, the deep-crystallization temperature was uniformly decreased from 45 to 50 ℃ to 35 ℃ to conduct crystallization, and after the time taken for this crystallization was 48 hours so that the concentration of the crystallized masse was 48 to 56% w/w, the crystallized masse was centrifuged, dried and sieved, and by centrifuging the psicose crystals and the mother liquor, the psicose crystal product having a purity of 99.9% w/w and a grain average size of 352.5 μm was obtained with a crystallization yield of 53.6%.
2. A crystallization process of psicose is characterized by comprising the following steps:
the primary crystallization is as follows: subjecting an psicose sugar solution having a purity of 98.5% w/w and a dry-matter concentration of 80% w/w to evaporative crystallization in a vacuum evaporative crystallizer, adding a small amount of psicose seed crystals treated by a seed mill to the psicose sugar solution having a dry-matter concentration of 80% w/w at 45 ℃ to 50 ℃, adding the psicose sugar solution having a dry-matter concentration of 80% w/w while evaporating, and subjecting the psicose sugar solution having a dry-matter concentration of 80% w/w to evaporative crystallization while maintaining the dry-matter concentration of 83% w/w, the evaporative crystallization time being 12 hours, allowing the crystallization rate to reach 15% to 20% w/w, and then subjecting the resulting solution to further cooling crystallization;
deep crystallization: the allulose massecuite after the primary crystallization is automatically flowed to a horizontal cooling crystallizer for deep crystallization, the deep temperature is uniformly decreased from 45 ℃ to 50 ℃ to 35 ℃ for crystallization, the time used in the crystallization process is 48 hours, the concentration of the crystallized massecuite is made to be 48% -56% w/w, then the crystallized massecuite is centrifuged, dried and sieved, and allulose crystal products having a purity of 99.5% w/w and an average grain size of 350.5 μm are obtained by centrifuging allulose crystals and mother liquor, and the crystallization yield is 53.2%.
3. A crystallization process of psicose is characterized by comprising the following steps:
the primary crystallization is as follows: subjecting an allulose sugar solution having a purity of 99% w/w and a dry matter concentration of 80% w/w to evaporative crystallization in a vacuum evaporative crystallizer, adding a small amount of allulose seeds treated by a seed mill to the allulose sugar solution having a dry matter concentration of 80% w/w at 45 ℃ to 50 ℃, adding the allulose sugar solution having a dry matter concentration of 80% w/w while evaporating, and subjecting the solution to evaporative crystallization while compensating for the addition of the allulose sugar solution having a dry matter concentration of 80% w/w, keeping the dry matter concentration at 83% w/w, and subjecting the solution to evaporative crystallization for 12 hours so that the crystallization rate reaches 15% to 20% w/w, and then subjecting the solution to cooling crystallization;
deep crystallization: the allulose massecuite after the primary crystallization is automatically flowed to a horizontal cooling crystallizer for deep crystallization, the deep temperature is uniformly decreased from 45 ℃ to 50 ℃ to 35 ℃ for crystallization, the time used in the crystallization process is 48 hours, the concentration of the crystallized massecuite is made to be 48% -56% w/w, then the crystallized massecuite is centrifuged, dried and sieved, and allulose crystal and mother liquor are centrifuged, so that an allulose crystal product with the purity of 99.9% w/w and the average grain size of 358.5 μm is obtained, and the crystallization yield is 53.7%.
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| US20230159579A1 (en) | 2020-05-27 | 2023-05-25 | Savanna Ingredients Gmbh | Crystallization of allulose under reduced pressure |
| CA3192084A1 (en) | 2020-09-07 | 2022-03-10 | Savanna Ingredients Gmbh | Extrusion process for the preparation of a solid allulose composition |
| EP4000419A1 (en) | 2020-11-23 | 2022-05-25 | Savanna Ingredients GmbH | Drying of allulose crystals |
| CN112574263B (en) * | 2020-12-04 | 2021-12-07 | 山东百龙创园生物科技股份有限公司 | Preparation method of psicose crystal |
| CN114456215A (en) * | 2022-03-04 | 2022-05-10 | 河南中大恒源生物科技股份有限公司 | D-psicose crystal and preparation method thereof |
| WO2024047121A1 (en) | 2022-09-01 | 2024-03-07 | Savanna Ingredients Gmbh | Process for the preparation of a particulate allulose composition |
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| CN102250157A (en) * | 2010-03-26 | 2011-11-23 | Cj第一制糖株式会社 | Method of producing d-psicose crystals |
| CN106852145A (en) * | 2014-10-20 | 2017-06-13 | Cj第制糖株式会社 | Method for preparing D psicose crystal |
| CN108290917A (en) * | 2016-02-29 | 2018-07-17 | Cj第制糖株式会社 | The manufacturing method of high-purity D-Psicose |
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| CN102250157A (en) * | 2010-03-26 | 2011-11-23 | Cj第一制糖株式会社 | Method of producing d-psicose crystals |
| CN106852145A (en) * | 2014-10-20 | 2017-06-13 | Cj第制糖株式会社 | Method for preparing D psicose crystal |
| CN108290917A (en) * | 2016-02-29 | 2018-07-17 | Cj第制糖株式会社 | The manufacturing method of high-purity D-Psicose |
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