CN118388558B - Anhydrous psicose crystal and preparation method thereof - Google Patents
Anhydrous psicose crystal and preparation method thereof Download PDFInfo
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Abstract
The invention provides a preparation method of anhydrous psicose crystals, which belongs to the technical field of functional sugar preparation, and comprises the steps of mixing raw material psicose liquid and psicose seed crystals, and then performing evaporation crystallization to ensure that the solid mass content of the psicose liquid is 82-84%, so as to obtain a first crystal liquid; adding water into the first crystallization liquid, and performing evaporative crystallization to maintain the solid matter content of the psicose sugar liquid between 84.5 and 85.5 percent to obtain a whole crystal liquid; adding the psicose sugar solution into the whole crystal liquid, and performing steaming and boiling crystallization to maintain the solid matter content of the psicose sugar solution at 85.5-86.5%, so as to obtain a second crystal liquid; and (3) sequentially centrifuging, washing and drying the second crystallization liquid to obtain anhydrous psicose crystals. The preparation method has the advantages of simple preparation process, easy operation, short period and low production cost; the obtained anhydrous psicose crystal has low water activity, good particle fluidity, no grain adhesion and regular crystal form.
Description
Technical Field
The invention relates to the technical field of functional sugar preparation, in particular to an anhydrous psicose crystal and a preparation method thereof.
Background
Psicose (D-psicose) is a six-carbon sugar with very low content in nature, and is an epimer of the C-3 site of D-fructose. D-psicose is hardly digested and absorbed and hardly provides energy for the life activities, and thus is a very useful low-calorie sweetener. In the medical health field, D-psicose can inhibit fatty liver enzyme and intestinal alpha-glycosidase, thereby reducing the accumulation of fat in the body and inhibiting the rise of blood sugar concentration. The D-psicose can be added in the diet to reduce postprandial blood glucose response and improve insulin sensitivity and glucose tolerance. In addition, D-psicose can more effectively scavenge active oxygen free radicals than other rare sugars. In the mouse test, it was found that D-psicose can prevent the bis- (2-ethylhexyl) -phthalic acid-induced injury to testes by inhibiting the production of active oxygen. In addition, the D-psicose has neuroprotective effect on apoptosis induced by 6-hydroxydopamine, and can inhibit the expression of monocyte chemotactic protein MCP-1 induced by high-concentration glucose. This suggests that D-psicose has potential functions for treating diseases related to nerve tissue degeneration, atherosclerosis, and the like.
The majority of the psicose currently marketed is liquid products and powdered solid products. Chinese patent document CN110627847a (application No. 201910876767.3) discloses a preparation method of psicose crystal, comprising the following steps: separating the enzyme-converted psicose liquid by chromatography, and purifying psicose to purity of more than 98.5%; concentrating the purified psicose until the solid mass content is 75-85%, and rapidly cooling to 35-45deg.C; adding seed crystal, maintaining 35-45 deg.c and vacuum degree of-0.03-0.09 MPa, and evaporating to crystallize at constant temperature; and (3) centrifugally separating to obtain crystals with the particle size of more than 60 meshes, and washing and drying to obtain the psicose crystals. Chinese patent document CN109748940a (application No. 201811470319.5) discloses a method for crystallizing psicose from an ethanol solution, comprising: concentrating the purified psicose solution under reduced pressure to obtain a solution I; heating the concentrated solution I, adding absolute ethyl alcohol, concentrating under reduced pressure again to remove water in the psicose solution by the ethyl alcohol, and obtaining an ethyl alcohol solution II of psicose; adding absolute ethyl alcohol into the concentrated solution II, heating until psicose is completely dissolved, slowly cooling, continuously slowly cooling after crystal precipitation until the crystals are no longer increased, and obtaining a mixed solution III; carrying out solid-liquid separation on the mixed liquid III to obtain a solid IV and a clear liquid V; drying the solid IV under reduced pressure to obtain psicose crystals; and (5) continuously concentrating the clear liquid V, repeating the steps, and crystallizing to obtain residual psicose crystals. The water activity of the prepared psicose crystals is about 0.4-0.7, so that the crystals are easy to adhere, and even hard solids are formed.
In the prior art, the problem that the psicose is difficult to crystallize, low in product yield, fine in crystal form, not centralized in crystal mesh distribution and the like often caused by high saturation concentration (more than 80%) of psicose solution, high water activity and high viscosity; in addition, a large amount of organic solvent is needed in the production process, so that the production is troublesome, potential safety hazards exist, the production process is complicated, the yield is low, and the cost is high.
Disclosure of Invention
In view of the above, the present invention aims to provide an anhydrous psicose crystal and a preparation method thereof, wherein the preparation process is simple, the operation is easy, and the crystallization period is short; organic solvent is not needed, so that the production cost can be reduced; the obtained anhydrous psicose crystal has low water activity, good particle mobility, no grain adhesion, smooth crystal surface, mirror surface, good reflectivity and regular crystal form.
In order to achieve the above object, the present invention provides the following technical solutions:
In a first aspect, the present invention provides a method for preparing anhydrous psicose crystals, comprising the steps of:
1) Mixing raw material psicose sugar solution and psicose seed crystal, and then evaporating and crystallizing to ensure that the solid mass content of the psicose sugar solution is 82-84%, thus obtaining a first crystallization solution;
2) Adding water into the first crystallization liquid obtained in the step 1) and performing evaporative crystallization to maintain the solid matter content of the psicose sugar liquid between 84.5 and 85.5 percent, thereby obtaining a whole crystal liquid;
3) Adding the psicose sugar solution into the whole crystal liquid obtained in the step 2) and performing steaming and crystallization to maintain the solid matter content of the psicose sugar solution between 85.5 and 86.5 percent, thereby obtaining a second crystal liquid;
4) And (3) sequentially centrifuging, washing and drying the second crystallization liquid in the step (3) to obtain anhydrous psicose crystals.
Preferably, the solid mass content of the raw material psicose sugar liquid in the step 1) is 75-77%, and the purity is more than or equal to 96%.
Further preferably, when the solid content of the raw material psicose sugar liquid is low, the solid content of the psicose sugar liquid can be increased by adopting a vacuum concentration mode, wherein the vacuum degree of the vacuum concentration is-0.05-0 MPa, and the temperature is 45-50 ℃.
Preferably, the dosage of the psicose seed crystal in the step 1) is 2-3 per mill of the mass of the psicose liquid serving as the raw material; the size of the psicose seed crystal is 200-240 meshes. In the invention, the uniform anhydrous psicose crystals are obtained by adding the controlled mesh number of psicose seed crystals; the aloulose crystal seeds are not suitable for being too large or too small, the crystal seeds are too large, the number of the crystal seeds is insufficient, the crystal seeds are easy to crystallize to form self-formed cores, the size distribution interval of the final crystal is too large, and the crystal size is not uniform; too small a seed tends to slow the crystallization process.
Preferably, the temperature of the evaporative crystallization in the step 1) and the step 2) is 45-50 ℃ respectively and the vacuum degree is-0.05-0 MPa respectively;
further preferably, the vacuum levels are each independently-0.01 MPa.
Preferably, the evaporation crystallization time in the step 2) is 1-2 h.
The purpose of step (2) in the present invention is to complete the crystal, to make the crystal size tend to average, and to make the crystal surface grow smooth, to perfect the crystal morphology.
Preferably, the adding of the psicose sugar solution during the stewing and crystallizing in the step 3) is performed by adopting a partition feeding mode, specifically:
sequentially dividing into 5 sections for material supplementing, steaming and crystallizing;
digestion crystallization 1 zone: the adding amount of the psicose liquid is 1/5-1/4 of the mass of the original feed liquid, the feed is uniformly fed, the feed is fed in 8h, and the sugar concentration of the psicose liquid after the feed is controlled to be 85.5%;
And (3) steaming and crystallizing a zone 2: the adding amount of the psicose liquid is 1/4-1/3 of the mass of the original feed liquid, the feed is uniformly fed, the feed is fed in 8h, and the sugar concentration of the psicose liquid after the feed is controlled to be 86.0%;
And (3) a digestion crystallization area 3: the adding amount of the psicose liquid is 1/3-1/2 of the mass of the original feed liquid, the feed is uniformly fed, the feed is fed in 6h, and the sugar concentration of the psicose liquid after the feed is controlled to be 86.2%;
and (3) steaming and crystallizing a region 4: the adding amount of the psicose liquid is 1/10-1/15 of the mass of the original feed liquid, the feed is uniformly fed, the feed is fed within 1h, and the sugar concentration of the psicose liquid after the feed is controlled to be 86.4%;
and (3) digestion and crystallization 5 area: the addition amount of the psicose sugar liquid is 1/25-1/30 of the mass of the original feed liquid, the feed is uniformly fed, the feed is fed within 1h, and the sugar concentration of the psicose sugar liquid after the feed is controlled to be 86.5%.
Preferably, the solid matter content of the psicose sugar liquid added in the step 3) is more than or equal to 75%.
Preferably, the temperature of the cooking crystallization in the step 3) is 50-55 ℃, and the cooking time is 20-24 h.
In a second aspect, the invention provides an anhydrous psicose crystal prepared by the preparation method.
Preferably, the anhydrous psicose crystals have a water activity of less than 0.2.
The beneficial technical effects are as follows:
1. The anhydrous psicose crystal is prepared by adopting a mode of combining an evaporation crystallization method, a crystal finishing method and a steaming crystallization method, the repeated heating and cooling processes are not needed, the preparation process is simple, the operation is easy, and the crystallization period is short; and the organic solvent is not required to be added, so that the production cost can be reduced, and the preparation process is simplified.
2. The invention does not directly carry out cooling crystallization after the evaporation crystallization is finished, but carries out crystal finishing, and the crystal finishing leads the crystal size to tend to be averaged, simultaneously leads the crystal surface to grow to be smooth and perfects the crystal morphology.
3. According to the invention, after the crystal is integrated, the material is adopted for stewing and crystallizing, so that the crystal shape and the crystal grain size are further stabilized, and the phenomena of spontaneous nucleation, uneven crystal size, long period and high energy consumption in the cooling process are avoided; after the digestion crystallization is finished, more than 80 percent of the crystal size can reach 40 to 80 meshes.
4. After crystallization is finished by the preparation method provided by the invention, the obtained anhydrous psicose crystal has the advantages of low water activity, good particle mobility, no grain adhesion, smooth crystal surface, mirror surface, good reflectivity and regular crystal form.
Drawings
FIG. 1 is a microscopic image of the crystal obtained after completion of the whole crystal of example 1;
FIG. 2 is a microscopic image of the crystal obtained after the crystallization of example 1;
FIG. 3 is a microscopic image of the crystal obtained after completion of the whole crystal of example 2;
FIG. 4 is a microscopic image of the crystal obtained after the crystallization of example 2;
FIG. 5 is a microscopic image of the crystal obtained after completion of the whole crystal of example 3;
FIG. 6 is a microscopic image of the crystal obtained after the crystallization of example 3;
FIG. 7 is a microscopic image of the crystal obtained after the crystallization of comparative example 1 is completed;
FIG. 8 is a microscopic image of the crystal obtained after the crystallization of comparative example 2 is completed;
FIG. 9 is a microscopic image of the crystal obtained after the crystallization of comparative example 3 was completed.
Detailed Description
The present invention will be described in detail with reference to specific examples. These embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art. The technical means used in the examples are conventional means well known to those skilled in the art unless otherwise indicated. The test methods in the following examples are conventional methods unless otherwise specified. The reagents and materials employed, unless otherwise indicated, are commercially available.
The psicose sugar solution used in the examples or comparative examples may be one or a combination of both of chemical synthesis or biocatalytic conversion.
Example 1
The embodiment provides a preparation method of psicose crystals, which comprises the following steps:
1) And (3) evaporating and crystallizing: taking raw material psicose sugar solution, adding psicose seed crystal, evaporating and crystallizing at 50deg.C under vacuum degree of-0.05 MPa until solid mass content of psicose sugar solution is 82%, to obtain first crystal solution;
Wherein the solid mass content of the raw material psicose liquid is 75%, the purity is not less than 96%, the adding amount of the psicose seed crystal is 2 per mill of the mass of the psicose liquid, and the size of the psicose seed crystal is 200 meshes.
2) And (3) crystal preparation: adding water into the first crystallization liquid obtained in the step 1), and simultaneously continuing to perform evaporation crystallization under the conditions of 50 ℃ and vacuum degree of-0.01 MPa, so that the solid mass content of the psicose sugar liquid is maintained at 84.5%, and the crystallization time is 1h, thereby obtaining a crystal liquid;
3) And (3) steaming and crystallizing: sequentially dividing the whole crystal liquid obtained after finishing the whole crystal in the step 2) into 5 intervals, and adding the psicose sugar liquid for stewing and crystallizing to obtain a second crystal liquid;
Wherein the solid mass content of the supplemented psicose sugar solution is 75%; the temperature of the stewing and crystallization is 50 ℃;
the 5 intervals are respectively:
the adding amount of the psicose sugar liquid in the area 1 of the digestion crystallization is 1/4 of the mass of the original feed liquid, the feeding speed is uniform, the feeding is completed in 8 h, and the sugar concentration is controlled to be 85.5%;
In the 2-zone of steaming and crystallizing, the adding amount of the psicose sugar solution is 1/3 of the mass of the original feed liquid, the feeding speed is uniform, the feeding is completed in 8h, and the sugar concentration is controlled to be 86.0%;
the adding amount of the psicose sugar liquid in the 3-zone of the digestion crystallization is 1/2 of the mass of the original feed liquid, the feeding speed is uniform, the feeding is completed in 6h, and the sugar concentration is controlled to be 86.2%;
The adding amount of the psicose sugar liquid in the 4-zone of the digestion crystallization is 1/15 of the mass of the original feed liquid, the feeding speed is uniform, the feeding is completed in 1h, and the sugar concentration is controlled to be 86.4%;
and (3) in a digestion crystallization 5 region, the adding amount of the psicose sugar solution is 1/30 of the mass of the original feed liquid, the feeding speed is uniform, the feed is fed in 1 h, and the crystallization is stopped by controlling the sugar concentration to be 86.5%.
4) And (3) sequentially centrifuging, washing and drying the second crystallization liquid obtained in the step (3) to obtain anhydrous psicose crystals.
A crystal microscope image (100 times) after finishing the whole crystal is shown in fig. 1;
The microscopic image (100 times) of the finally obtained anhydrous psicose crystal is shown in fig. 2, the crystal size distribution is concentrated, the crystal surface is smooth, the crystal form is regular, and the purity of the psicose crystal is 99.62% and the water activity is 0.1742. The size distribution of the obtained crystals is shown in Table 1, and 87% of the crystals can reach 40-80 meshes.
TABLE 1 Crystal size distribution after crystallization of EXAMPLE 1
| Crystal size | Distribution ratio |
| 20 Meshes or more | ------ |
| 20-40 Mesh | 6.71 % |
| 40-60 Mesh | 38.64 % |
| 60-80 Mesh | 49.53 % |
| 80-100 Mesh | 5.12 % |
| 100 Meshes or less | —— |
Example 2
1) And (3) evaporating and crystallizing: taking raw material psicose sugar solution, adding psicose seed crystal, evaporating and crystallizing at 45 ℃ under vacuum degree of-0.01 MPa until the solid mass content of the psicose sugar solution is 83%, and obtaining a first crystallization solution;
Wherein the solid mass content of the raw material psicose liquid is 76%, the purity is not less than 96%, the adding amount of the psicose seed crystal is 2.5 per mill of the mass of the psicose liquid, and the size of the psicose seed crystal is 220 meshes.
2) And (3) crystal preparation: adding water into the first crystallization liquid obtained in the step 1), and simultaneously continuing to perform evaporation crystallization under the conditions of 50 ℃ and vacuum degree of-0.01 MPa, so that the solid mass content of the psicose sugar liquid is maintained between 85%, and the crystallization time is 2h, thereby obtaining a crystal liquid;
3) And (3) steaming and crystallizing: sequentially dividing the whole crystal liquid obtained after finishing the whole crystal in the step 2) into 5 intervals, and adding the psicose sugar liquid for stewing and crystallizing to obtain a second crystal liquid;
Wherein the solid mass content of the supplemented psicose sugar solution is 76%; the temperature of the stewing and crystallization is 55 ℃;
the 5 intervals are respectively:
the adding amount of the psicose sugar liquid in the area 1 of the digestion crystallization is 1/5 of the mass of the original feed liquid, the feeding speed is uniform, the feeding is completed in 8 h, and the sugar concentration is controlled to be 85.5%;
In the 2-zone of steaming and crystallizing, the adding amount of the psicose sugar solution is 1/4 of the mass of the original feed liquid, the feeding speed is uniform, the feeding is completed in 8h, and the sugar concentration is controlled to be 86.0%;
the adding amount of the psicose sugar liquid in the 3-zone of the digestion crystallization is 1/2 of the mass of the original feed liquid, the feeding speed is uniform, the feeding is completed in 6h, and the sugar concentration is controlled to be 86.2%;
the adding amount of the psicose sugar liquid in the 4-zone of the digestion crystallization is 1/10 of the mass of the original feed liquid, the feeding speed is uniform, the feeding is completed in 1h, and the sugar concentration is controlled to be 86.4%;
And (3) in a digestion crystallization area 5, the adding amount of the psicose sugar solution is 1/25 of the mass of the original feed liquid, the feeding speed is uniform, the feed is fed in 1 h, and the crystallization is stopped by controlling the sugar concentration to 86.5%.
4) And (3) sequentially centrifuging, washing and drying the second crystallization liquid obtained in the step (3) to obtain anhydrous psicose crystals.
A crystal microscope image (100 times) after finishing the whole crystal is shown in fig. 3;
The microscopic image (100 times) of the finally obtained anhydrous psicose crystal is shown in fig. 4, the crystal size distribution is concentrated, the crystal surface is smooth and mirror-surface, the crystal form is regular, the purity of the detected psicose crystal is 99.58%, the water activity is 0.1508, the size distribution of the obtained crystal is shown in table 2, and the size of 88% of the crystal can reach 40-80 meshes.
TABLE 2 Crystal size distribution after crystallization of EXAMPLE 2
| Crystal size | Distribution ratio |
| 20 Meshes or more | 0.87 % |
| 20-40 Mesh | 6.43 % |
| 40-60 Mesh | 40.11 % |
| 60-80 Mesh | 48.46 % |
| 80-100 Mesh | 4.13 % |
| 100 Meshes or less | ------ |
Example 3
1) And (3) evaporating and crystallizing: taking raw material psicose sugar solution, adding psicose seed crystal, evaporating and crystallizing at 50deg.C under vacuum degree of-0.01 MPa until solid mass content of psicose sugar solution is 84%, to obtain first crystal solution;
Wherein the solid mass content of the raw material psicose liquid is 77%, the purity is not less than 96%, the adding amount of the psicose seed crystal is 3 per mill of the mass of the psicose liquid, and the size of the psicose seed crystal is 240 meshes.
2) And (3) crystal preparation: adding water into the first crystallization liquid obtained in the step 1), and simultaneously continuing to perform evaporation crystallization at 50 ℃ under the vacuum degree of-0.01 MPa so that the solid mass content of the psicose sugar liquid is maintained between 85.5%, and the crystallization time is 2h, thereby obtaining a crystal liquid;
3) And (3) steaming and crystallizing: sequentially dividing the whole crystal liquid obtained after finishing the whole crystal in the step 2) into 5 intervals, and adding the psicose sugar liquid for stewing and crystallizing to obtain a second crystal liquid;
wherein the solid mass content of the supplemented psicose sugar solution is 77%; the temperature of the stewing and crystallization is 55 ℃;
the 5 intervals are respectively:
the adding amount of the psicose sugar liquid in the area 1 of the digestion crystallization is 1/4 of the mass of the original feed liquid, the feeding speed is uniform, the feeding is completed in 8 h, and the sugar concentration is controlled to be 85.5%;
In the 2-zone of steaming and crystallizing, the adding amount of the psicose sugar solution is 1/3 of the mass of the original feed liquid, the feeding speed is uniform, the feeding is completed in 8h, and the sugar concentration is controlled to be 86.0%;
the adding amount of the psicose sugar liquid in the 3-zone of the digestion crystallization is 1/2 of the mass of the original feed liquid, the feeding speed is uniform, the feeding is completed in 6h, and the sugar concentration is controlled to be 86.2%;
The adding amount of the psicose sugar liquid in the 4-zone of the digestion crystallization is 1/15 of the mass of the original feed liquid, the feeding speed is uniform, the feeding is completed in 1h, and the sugar concentration is controlled to be 86.4%;
and (3) in a digestion crystallization 5 region, the adding amount of the psicose sugar solution is 1/30 of the mass of the original feed liquid, the feeding speed is uniform, the feed is fed in 1 h, and the crystallization is stopped by controlling the sugar concentration to be 86.5%.
4) And (3) sequentially centrifuging, washing and drying the second crystallization liquid obtained in the step (3) to obtain anhydrous psicose crystals.
A crystal microscope image (100 times) after finishing the whole crystal is shown in fig. 5;
The microscopic image (100 times) of the finally obtained anhydrous psicose crystal is shown in fig. 6, the crystal size distribution is concentrated, the crystal surface is smooth, the crystal form is regular, the purity of the detected psicose crystal is 99.64%, the water activity is 0.1615, the size distribution of the obtained crystal is shown in table 3, and the size of 89% of the crystal can reach 40-80 meshes.
TABLE 3 Crystal size distribution after crystallization of EXAMPLE 3
| Crystal size | Distribution ratio |
| 20 Meshes or more | 0.75 % |
| 20-40 Mesh | 6.68 % |
| 40-60 Mesh | 40.79 % |
| 60-80 Mesh | 49.11 % |
| 80-100 Mesh | 2.67 % |
| 100 Meshes or less | ------ |
Comparative example 1
This comparative example was conducted by the production method of example 2 except that the psicose seed crystal was added in step 1) by concentrating the psicose liquid at 45℃under a vacuum of-0.01 MPa to a solid matter content of 80%, and the other steps and operations were the same as in example 2.
Microscopic images (100-fold) of the obtained crystals are shown in FIG. 7, and yield purity of the psicose crystals was detected as 98.97%, and water activity was 0.1954. The size distribution of the obtained crystals is shown in the following table, the crystal sizes are mainly distributed in 40-60 meshes and 60-80 meshes, and the crystals are distributed in other size ranges, so that the crystal size distribution is not concentrated:
TABLE 4 Crystal size distribution after completion of crystallization of comparative example 1
| Crystal size | Distribution ratio |
| 20 Meshes or more | 3.06 % |
| 20-40 Mesh | 8.16 % |
| 40-60 Mesh | 45.24 % |
| 60-80 Mesh | 30.71 % |
| 80-100 Mesh | 8.62 % |
| 100 Meshes or less | 4.21 % |
Comparative example 2
This comparative example was conducted for crystallization of psicose according to the preparation method of example 2, except that the digestion crystallization in step 3) was a fed-batch digestion crystallization, the feeding speed and the feeding amount (total feeding amount and digestion crystallization time are identical) were not distinguished, and the other steps and operations were the same as in example 2.
After the crystallization is completed, a microscopic image (100 times) of the obtained crystal is shown in fig. 8, the purity of the psicose crystal is detected to be 98.91%, the water activity is 0.2315, the size distribution of the obtained crystal is shown in the following table, the crystal size is mainly distributed in 40-80 meshes, the crystal size is distributed in other size ranges, the content of the small-mesh crystals is increased, the crystal size distribution is not concentrated, the crystal form is small, and the partial adhesion condition exists.
TABLE 5 Crystal size distribution after completion of crystallization of comparative example 2
| Crystal size | Distribution ratio |
| 20 Meshes or more | 0.74 % |
| 20-40 Mesh | 6.48 % |
| 40-60 Mesh | 34.44 % |
| 60-80 Mesh | 47.45 % |
| 80-100 Mesh | 10.68 % |
| 100 Meshes or less | 0.21 % |
Comparative example 3
The crystallization of psicose was performed according to the preparation method of example 2, except that the crystallization was performed by cooling in a uniformly decreasing manner in step 3), and the temperature was uniformly decreased from 45 to 30℃at a temperature of 1℃per hour.
After the completion of crystallization, a microscopic image (100 times) of the obtained crystal was shown in FIG. 9, and the purity of the psicose crystal was 98.77%, the water activity 0.5290, and the crystal grains were bonded. The size distribution of the obtained crystals is shown in the following table, the sizes of the crystals are mainly distributed in 40-60 meshes, 60-80 meshes, 80-100 meshes and less than 100 meshes, the crystals are distributed in other size ranges, the size distribution of the crystals is not concentrated, the crystal forms are small, the adhesion phenomenon occurs, and the water activity is high.
TABLE 6 Crystal size distribution after the crystallization of comparative example 3
| Crystal size | Distribution ratio |
| 20 Meshes or more | 0.98 % |
| 20-40 Mesh | 3.1 % |
| 40-60 Mesh | 12.16 % |
| 60-80 Mesh | 27.37 % |
| 80-100 Mesh | 38.21 % |
| 100 Meshes or less | 18.18 % |
According to the invention, the psicose crystal is prepared by adopting a mode of combining evaporative crystallization, crystal finishing and stewing crystallization, the preparation process is simple, the operation is easy, and the crystallization period is short. The prepared crystal has regular crystal form, concentrated mesh number distribution, water activity of psicose crystal below 0.2, good crystal fluidity and no adhesion phenomenon.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (1)
1. The preparation method of the anhydrous psicose crystal is characterized by comprising the following steps of:
(1) Mixing raw material psicose sugar solution and psicose seed crystal, and then evaporating and crystallizing to ensure that the solid mass content of the psicose sugar solution is 82-84%, thus obtaining a first crystallization solution;
(2) Adding water into the first crystallization liquid obtained in the step (1) and performing evaporative crystallization to maintain the solid matter content of the psicose sugar liquid between 84.5 and 85.5 percent, thereby obtaining a whole crystal liquid;
(3) Adding psicose sugar solution into the whole crystal liquid obtained in the step (2) and steaming and crystallizing to maintain the solid matter content of the psicose sugar solution at 85.5-86.5%, so as to obtain a second crystal liquid;
(4) Centrifuging, washing and drying the second crystallization liquid in the step (3) in sequence to obtain anhydrous psicose crystals;
the solid mass content of the raw material psicose sugar liquid in the step (1) is 75-77%, and the purity is more than or equal to 96%;
The dosage of the psicose seed crystal in the step (1) is 2-3 per mill of the mass of the psicose liquid serving as the raw material; the size of the psicose seed crystal is 200-240 meshes;
The temperature of the evaporative crystallization in the step (1) and the step (2) is respectively and independently 45-50 ℃, and the vacuum degree is respectively and independently-0.05-0 MPa;
The evaporation and crystallization time in the step (2) is 1-2 h;
the adding of the psicose sugar liquid during the stewing and crystallizing in the step (3) is performed in a mode of batch feeding, and specifically comprises the following steps:
sequentially dividing into 5 sections for material supplementing, steaming and crystallizing;
digestion crystallization 1 zone: the adding amount of the psicose liquid is 1/5-1/4 of the mass of the original feed liquid, the feed is uniformly fed, the feed is fed in 8h, and the sugar concentration of the psicose liquid after the feed is controlled to be 85.5%;
And (3) steaming and crystallizing a zone 2: the adding amount of the psicose liquid is 1/4-1/3 of the mass of the original feed liquid, the feed is uniformly fed, the feed is fed in 8h, and the sugar concentration of the psicose liquid after the feed is controlled to be 86.0%;
And (3) a digestion crystallization area 3: the adding amount of the psicose liquid is 1/3-1/2 of the mass of the original feed liquid, the feed is uniformly fed, the feed is fed in 6h, and the sugar concentration of the psicose liquid after the feed is controlled to be 86.2%;
and (3) steaming and crystallizing a region 4: the adding amount of the psicose liquid is 1/10-1/15 of the mass of the original feed liquid, the feed is uniformly fed, the feed is fed within 1h, and the sugar concentration of the psicose liquid after the feed is controlled to be 86.4%;
and (3) digestion and crystallization 5 area: the adding amount of the psicose liquid is 1/25-1/30 of the mass of the original feed liquid, the feed is uniformly fed, the feed is fed within 1h, and the sugar concentration of the psicose liquid after the feed is controlled to be 86.5%;
The solid mass content of the psicose sugar liquid added in the step (3) is more than or equal to 75 percent;
The temperature of the stewing and crystallizing in the step (3) is 50-55 ℃, and the stewing time is 20-24 h.
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| 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 |
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| 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 |
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