CN115160218B - Vitamin B6 granule with high flowability and preparation method thereof - Google Patents
Vitamin B6 granule with high flowability and preparation method thereof Download PDFInfo
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- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
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- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
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- C07D213/66—One oxygen atom attached in position 3 or 5 having in position 3 an oxygen atom and in each of the positions 4 and 5 a carbon atom bound to an oxygen, sulphur, or nitrogen atom, e.g. pyridoxal
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Abstract
The invention discloses vitamin B6 particles with high fluidity and a preparation method thereof, wherein the preparation method comprises the following steps: (1) Dissolving a vitamin B6 crude product in water to prepare a saturated solution of vitamin B6; (2) Cooling the saturated solution of vitamin B6 obtained in the step (1) to obtain a supersaturated solution, adding vitamin B6 seed crystals before or after cooling, preserving heat, then cooling and crystallizing under the condition of rapid stirring, and finally filtering and drying to obtain vitamin B6 crystal particles; in the step (2), the size of the vitamin B6 seed crystal is smaller than 150 mu m, the vitamin B6 seed crystal is a seed crystal with regular crystal habit, and the mass ratio of the vitamin B6 seed crystal to the vitamin B6 crude product is 1-10: 100. the method can prepare products with higher fluidity and more concentrated particle size distribution, and has important application value.
Description
Technical Field
The invention belongs to the field of fine chemical industry, relates to a crystallization process of vitamin B6, and in particular relates to a preparation method of vitamin B6 particles with high flowability.
Background
Vitamin B6 is one of vitamins essential to the human body and is an essential substance in the metabolic processes of fat and sugar of the human body. In physiological function, vitamin B6 participates in various enzyme reactions, in the synthesis and decomposition processes of proteins, in amino acid metabolism, heme metabolism, and the like. In addition, vitamin B6 can also prevent arteriosclerosis and improve immunity to cancer. The deficiency of vitamin B6 is manifested by seborrhea, secretion of oil and fat around mouth, eyes and behind ears, and symptoms such as keratitis and glossitis can occur. Therefore, vitamin B6 is often used as a food additive or a medicine for treating vitamin B6 deficiency and other diseases in human bodies.
In order to be able to better apply the vitamin B6 particles to food additives or pharmaceuticals, this requires a suitable particle size distribution and high flowability of the vitamin B6 particles. In the prior art in industry, crystals with large particles are usually subjected to mechanical crushing and then screening to obtain small-particle crystals, but the crystal habit of the crystal particles is irregular and poor in flowability in the mode, a large amount of fine dust is often generated after mechanical crushing, so that a production workshop is not clean, the potential safety hazard of dust explosion is also caused, and in addition, the energy consumption is increased due to mechanical crushing, so that the production cost is increased.
CN102295598B discloses a method for crystallizing vitamin B6, after dissolving vitamin B6 crude product in water, decolorizing with active carbon, filtering, cooling, then adding ethanol for crystallization, by adopting the method, vitamin B6 product particles are smaller, particles below 200 meshes are more, the particle size distribution of the product is not concentrated as a result, and a large amount of ethanol is used, so that the requirement on explosion prevention is met, the investment cost is increased, and the energy consumption is also increased in the process of recovering ethanol.
CN104710352B discloses a method for crystallizing vitamin B6, in which a heated solution is added dropwise to a saturated vitamin B6 refined solution under stirring to obtain vitamin B6 crystals, but the product obtained by this method still has some large-particle crystals, because small-particle crystals can grow into large crystals continuously with the progress of the addition, and in addition, local burst nucleation can be caused to produce fine particles due to the problem of mixing, thus resulting in a wider particle size distribution of the final product, and meanwhile, the product obtained by this method has an octahedral crystal form, and its flowability is not particularly good.
When the vitamin B6 particles are applied to the field of foods or medicines, for convenience in operation, on one hand, the vitamin B6 particles are required to have better flowability (i.e., smaller repose angle), and at the same time, the vitamin B6 particles are required to have proper particle size and concentrated distribution, and the particle size distribution is too wide or too fine. Therefore, in order to meet the downstream application and reduce the production energy consumption, a brand new vitamin B6 crystallization method needs to be provided.
Disclosure of Invention
The invention provides a brand-new and simpler vitamin B6 crystallization method, and the method can prepare products with higher fluidity and more concentrated particle size distribution.
The technical scheme of the invention is as follows:
a method for preparing vitamin B6 granules with high flowability, comprising the following steps:
(1) Dissolving a vitamin B6 crude product in water to prepare a saturated solution of vitamin B6;
(2) Cooling the saturated solution of vitamin B6 obtained in the step (1) to obtain a supersaturated solution, adding vitamin B6 seed crystals, preserving heat, cooling and crystallizing under the condition of rapid stirring, and finally filtering and drying to obtain vitamin B6 crystal particles;
in the step (2), the size of the vitamin B6 seed crystal is smaller than 150 mu m, and the vitamin B6 seed crystal is a seed crystal with regular crystal habit;
the mass ratio of the vitamin B6 seed crystal to the vitamin B6 crude product is 1-10: 100.
the inventor finds that the crystal seeds in different forms and the mixing conditions are adopted in a crystallization system of vitamin B6 to obtain products with great difference, the conditions such as proper crystal seed type, stirring speed, cooling speed and the like are selected to achieve the unprecedented effects, the products with better free-running property (the repose angle can reach 14.8 degrees) and more concentrated particle size distribution are prepared, the products with smaller particle size (the 40-mesh passing rate can reach 99 percent) can be prepared without mechanical crushing, and meanwhile, the organic solvent is not introduced.
The operation mechanism of the invention is as follows: in a crystallization system of vitamin B6, seed crystals are introduced as crystal nucleus, supersaturation degree is generated along with the subsequent cooling process, the added crystal nucleus grows continuously to eliminate the supersaturation degree, the crystallization process is controlled in a crystallization growth area instead of a crystallization nucleation area, and the grain size distribution of a final product is controlled by adjusting the size and the adding amount of the seed crystals; it has surprisingly been found that by introducing seed crystals with a regular habit, vitamin B6 crystal particles with better flowability and a more concentrated particle size distribution can be prepared under rapid stirring conditions.
In the step (1), the saturated solution of vitamin B6 is obtained by dissolving a crude vitamin B6 product in water, or is obtained by decoloring and concentrating an aqueous solution of the crude vitamin B6 product.
Preferably, in the step (1), the purity of the vitamin B6 crude product is more than 98 percent, and the preparation method is the prior art and has no special requirement.
Preferably, in the step (1), the temperature of the saturated solution of vitamin B6 is 50 to 90 ℃, and more preferably the temperature of the saturated solution is 70 to 85 ℃.
Preferably, in the step (2), the temperature difference between the supersaturated solution and the saturated solution in the step (1) is controlled to be 0-10 ℃, not including 0 ℃, more preferably the temperature difference between the supersaturated solution and the saturated solution in the step (1) is controlled to be 1-6 ℃, and still more preferably the temperature difference between the supersaturated solution and the saturated solution in the step (1) is controlled to be 1-3 ℃.
Preferably, in the step (2), the vitamin B6 seed crystal has a size of less than 100 μm, more preferably 40 to 80 μm, and even more preferably a crystal habit, which means that the crystals have a substantially rectangular, hexagonal or octagonal structure, and preferably a rectangular structure.
Preferably, in the step (2), the adding amount of the vitamin B6 seed crystal depends on the particle size requirement of the final product, and the mass ratio of the preferable using amount to the vitamin B6 crude product is 2-10: 100, more preferably 2 to 7:100.
preferably, in the step (2), the temperature is kept for 5 to 15 minutes before cooling and crystallization.
Preferably, in step (2), the rapid stirring is carried out at a speed of 300 to 1200rpm, preferably 500 to 1200rpm, and most preferably 700 to 1200rpm.
Preferably, in the step (2), the temperature is reduced by rapid stirring, and the temperature of the cooling end point is 5-30 ℃, preferably 10-25 ℃, and most preferably 10-15 ℃.
Preferably, in the step (2), the cooling crystallization is performed for 1 to 8 hours, preferably 4 to 6 hours.
The vitamin B6 particles with high fluidity, concentrated particle size distribution and adjustable particle size distribution can be prepared through the process operation of the invention.
The invention also provides vitamin B6 particles, the passing rate of 40 meshes is 90.0-99.9%, the particle ratio between 40 meshes and 100 meshes is 85.0-98.4%, and the repose angle is less than 20.4 degrees.
Preferably, the vitamin B6 particles have a 40 mesh passing rate of 92.0% -99.8%, a particle ratio of between 40 mesh and 100 mesh of 85.0% -98.1%, and an repose angle of 14.8-20.4 degrees.
Preferably, the vitamin B6 particles have a 40 mesh passing rate of 97.8% -99.8%, a particle ratio of between 40 mesh and 100 mesh of 93.2% -98.1%, and an repose angle of 14.8-18.6 degrees.
Compared with the prior art, the invention has the beneficial effects that:
(1) The invention has simple operation process, no use of organic solvent, no need of solvent recovery, low production energy consumption and suitability for industrialization.
(2) The vitamin B6 crystal particles with extremely high fluidity and adjustable particle size distribution can be obtained through a crystallization one-step process, and the particle size distribution can be adjusted according to market demands.
(3) The vitamin B6 crystal particles can be directly obtained in a crystallization mode without using a mechanical crushing procedure, the crystal habit of the particles is round, the particle size distribution is uniform, and the 40-mesh passing rate is over 95 percent.
Drawings
FIG. 1 is a photograph of crystalline particles of vitamin B6 obtained in comparative example 1.
Fig. 2 is a photograph of crystalline irregular vitamin B6 seed particles used in comparative example 2.
Fig. 3 is a photograph of crystalline particles of vitamin B6 obtained in comparative example 2.
Fig. 4 is a photograph of vitamin B6 seed particles of the crystal habit rules used in the present invention.
Fig. 5 is a photograph showing the crystalline particles of vitamin B6 having high flowability characteristics obtained by the present invention.
Detailed Description
The invention is illustrated below in connection with specific examples.
The preparation method of the seed crystal with the crystal habit rule smaller than 150 μm comprises the following steps:
weighing 30g of VB6 refined product, adding into 100g of water, heating to 45 ℃ to obtain VB6 solution, adding the solution into 200g of ethanol which is precooled to 0 ℃, setting the stirring rotation speed to 500rpm, rapidly separating out fine crystals due to the elution and cooling effects, continuing stirring for 10min at 0 ℃, filtering and drying, and sieving the dried product to obtain the seed crystal.
The testing method comprises the following steps:
1. crystal morphology:
vitamin B6 crystals were observed using a Nikon ECLIPSE LV100POL microscope.
2. Angle of repose
The repose angle is the maximum angle formed by the free inclined plane of the powder accumulation layer and the horizontal plane. The smaller the angle of repose, the better the flowability. The fluidity of the powder has great influence on the weight difference of preparations such as granules, capsules, tablets and the like and normal operation. In the invention, the repose angle of the crystal is measured by using a GB 11986-89 standard test method.
3. Pass rate of
Sieving the prepared vitamin B6 crystal particles with a 40-mesh sieve and a 100-mesh sieve respectively, wherein the passing vitamin B6 crystal particles account for the weight proportion of the provitamin B6 crystal particles as the passing rate.
Particle ratio between 40 mesh and 100 mesh = passing ratio of vitamin B6 crystal particles through 40 mesh to passing ratio of vitamin B6 crystal particles through 100 mesh
Comparative example 1 (Cooling crystallization, seeding)
Weighing 210g of vitamin B6 crude product (purity is more than 98%) in a 500ml crystallizer, adding 280g of water into the crystallizer, setting stirring speed to be 150rpm, heating to obtain a saturated solution at 72 ℃, then cooling to 15 ℃,4 hours for cooling, filtering after cooling, eluting a filter cake with a small amount of ethanol, finally drying the filter cake to obtain 160g of vitamin B6 crystals, and crystallizing to obtain a product with a crystal habit shown in figure 1, wherein the 40 mesh passing rate of the obtained product is 30%, the particle ratio between 40 mesh and 100 mesh is 28%, and the repose angle is 34 degrees.
Comparative example 2
Weighing 210g of vitamin B6 crude product (purity is more than 98%) in a 500ml crystallizer, adding 280g of water into the crystallizer, setting stirring speed to be 700rpm, heating to obtain a saturated solution at 72 ℃, cooling to 70 ℃, adding crystal habit irregular seed crystals smaller than 150 mu m, keeping the temperature and stirring for 10min, wherein the adding amount of the seed crystals is 7% of the mass of the added vitamin B6 crude product, the crystal habit is shown in figure 2, cooling to 15 ℃, cooling for 4h, filtering after cooling, eluting a filter cake with a small amount of ethanol, finally drying the filter cake to obtain 176g of vitamin B6 crystal, crystallizing to obtain a product crystal habit of 93%, the particle ratio between 40 mesh and 100 mesh is 81%, and the repose angle is 24.7 degrees.
Comparative example 3
Weighing 210g of vitamin B6 crude product (purity is more than 98%) in a 500ml crystallizer, adding 280g of water into the crystallizer, setting stirring speed to be 700rpm, heating to obtain a saturated solution at 72 ℃, cooling to 60 ℃, then adding crystal seeds with crystal habit of less than 150 mu m, keeping the temperature and stirring for 10min, wherein the adding amount of the crystal seeds is 7% of the mass of the added vitamin B6 crude product, the crystal seeds are shown in figure 4, cooling to 15 ℃, 4h is used for cooling, filtering is carried out after cooling, a small amount of ethanol is used for leaching filter cakes, finally, drying the filter cakes to obtain 175g of vitamin B6 crystals, the 40-mesh passing rate of the obtained product is 78%, the particle ratio between 40 mesh and 100 mesh is 67%, and the repose angle is 27.8 ℃.
Comparative example 4
Weighing 210g of vitamin B6 crude product (purity is more than 98%) in a 500ml crystallizer, adding 280g of water into the crystallizer, setting stirring speed to be 700rpm, heating to obtain a saturated solution at 72 ℃, cooling to 70 ℃, adding crystal seeds with crystal habit of less than 150 mu m, keeping the temperature and stirring for 10min, wherein the adding amount of the crystal seeds is 0.5% of the mass of the added vitamin B6 crude product, the crystal seeds are shown in figure 4, cooling to 15 ℃, 4h after cooling, filtering after cooling, eluting a filter cake with a small amount of ethanol, finally drying the filter cake to obtain 162g of vitamin B6 crystals, wherein the 40-mesh passing rate of the obtained product is 57%, the particle ratio between 40 mesh and 100 mesh is 48%, and the repose angle is 27 ℃.
Example 1
Weighing 210g of vitamin B6 crude product (purity is more than 98%) in a 500ml crystallizer, adding 280g of water into the crystallizer, setting stirring speed to be 700rpm, heating to obtain a saturated solution at 72 ℃, cooling to 70 ℃, adding crystal seeds with crystal habit of less than 150 mu m, keeping the temperature and stirring for 10min, wherein the adding amount of the crystal seeds is 7% of the mass of the added vitamin B6 crude product, the crystal habit is shown in figure 4, cooling to 15 ℃, 4h after cooling, filtering after cooling, eluting a filter cake with a small amount of ethanol, finally drying the filter cake to obtain 177.1g of vitamin B6 crystal, crystallizing to obtain a product crystal habit of 99.5% of 40 meshes, wherein the particle ratio between 40 meshes and 100 meshes is 98.1%, and the repose angle is 14.8 degrees.
Example 2
Weighing 210g of vitamin B6 crude product (purity is more than 98%) in a 500ml crystallizer, adding 280g of water into the crystallizer, setting stirring speed to be 500rpm, heating to obtain a saturated solution at 72 ℃, cooling to 70 ℃, adding crystal seeds with crystal habit of less than 150 mu m, keeping the temperature and stirring for 10min, wherein the adding amount of the crystal seeds is 7% of the mass of the added vitamin B6 crude product, the crystal seeds are shown in figure 4, cooling to 15 ℃, cooling for 4h, filtering after cooling, eluting a filter cake with a small amount of ethanol, and finally drying the filter cake to obtain 176.5g of vitamin B6 crystal, wherein the 40 mesh passing rate of the obtained product is 97.8%, the particle ratio between 40 mesh and 100 mesh is 96.5%, and the repose angle is 16.4 ℃.
Example 3
Weighing 210g of vitamin B6 crude product (purity is more than 98%) in a 500ml crystallizer, adding 280g of water into the crystallizer, setting stirring speed to be 1000rpm, heating to obtain a saturated solution at 72 ℃, cooling to 70 ℃, adding crystal seeds with crystal habit of less than 150 mu m, keeping the temperature and stirring for 10min, wherein the adding amount of the crystal seeds is 7% of the mass of the added vitamin B6 crude product, the crystal seeds are shown in figure 4, cooling to 15 ℃, cooling for 4h, filtering after cooling, eluting a filter cake with a small amount of ethanol, finally drying the filter cake to obtain 175.6g of vitamin B6 crystals, wherein the 40 mesh passing rate of the obtained product is 99.6%, the particle ratio between 40 mesh and 100 mesh is 97.4%, and the repose angle is 15.6.
Example 4
Weighing 210g of vitamin B6 crude product (purity is more than 98%) in a 500ml crystallizer, adding 280g of water into the crystallizer, setting stirring speed to be 700rpm, heating to obtain a saturated solution at 72 ℃, cooling to 70 ℃, adding crystal seeds with crystal habit of less than 150 mu m, keeping the temperature and stirring for 10min, wherein the adding amount of the crystal seeds is 5% of the mass of the added vitamin B6 crude product, the crystal seeds are shown in figure 4, cooling to 15 ℃, cooling for 4h, filtering after cooling, eluting a filter cake with a small amount of ethanol, and finally drying the filter cake to obtain 170.5g of vitamin B6 crystal, wherein the 40-mesh passing rate of the obtained product is 97%, the particle ratio between 40 mesh and 100 mesh is 94.3%, and the repose angle is 18 ℃.
Example 5
Weighing 210g of vitamin B6 crude product (purity is more than 98%) in a 500ml crystallizer, adding 280g of water into the crystallizer, setting stirring speed to be 700rpm, heating to obtain a saturated solution at 72 ℃, cooling to 70 ℃, adding crystal seeds with crystal habit of less than 150 mu m, keeping the temperature and stirring for 10min, wherein the adding amount of the crystal seeds is 2% of the mass of the added vitamin B6 crude product, the crystal habit is shown in figure 4, cooling to 15 ℃, cooling for 4h, filtering after cooling, eluting a filter cake with a small amount of ethanol, and finally drying the filter cake to obtain 164g of vitamin B6 crystal, wherein the 40-mesh passing rate of the obtained product is 92%, the particle ratio between 40 mesh and 100 mesh is 85%, and the repose angle is 20.4 ℃.
Example 6
Weighing 210g of vitamin B6 crude product (purity is more than 98%) in a 500ml crystallizer, adding 280g of water into the crystallizer, setting stirring speed to be 700rpm, heating to obtain a saturated solution at 72 ℃, cooling to 70 ℃, adding crystal seeds with crystal habit of less than 150 mu m, keeping the temperature and stirring for 10min, wherein the adding amount of the crystal seeds is 10% of the mass of the added vitamin B6 crude product, the crystal habit is shown in figure 4, cooling to 15 ℃, cooling for 4h, filtering after cooling, eluting a filter cake with a small amount of ethanol, and finally drying the filter cake to obtain 183g of vitamin B6 crystal, wherein the 40-mesh passing rate of the obtained product is 99.8%, the particle ratio between 40 mesh and 100 mesh is 95.4%, and the repose angle is 17.2 ℃.
Example 7
Weighing 210g of vitamin B6 crude product (purity is more than 98%) in a 500ml crystallizer, adding 280g of water into the crystallizer, setting stirring speed to be 700rpm, heating to obtain a saturated solution at 72 ℃, cooling to 66 ℃, adding crystal seeds with crystal habit of less than 150 mu m, keeping the temperature and stirring for 10min, wherein the adding amount of the crystal seeds is 7% of the mass of the added vitamin B6 crude product, the crystal seeds are shown in figure 4, cooling to 15 ℃, cooling for 4h, filtering after cooling, eluting a filter cake with a small amount of ethanol, finally drying the filter cake to obtain 175.8g of vitamin B6 crystals, wherein the 40 mesh passing rate of the obtained product is 98.3%, the particle ratio between 40 mesh and 100 mesh is 93.2%, and the repose angle is 18.6.
Example 8
Weighing 210g of vitamin B6 crude product (purity is more than 98%) in a 500ml crystallizer, adding 280g of water into the crystallizer, setting stirring speed to be 700rpm, heating to obtain a saturated solution at 72 ℃, cooling to 62 ℃, then adding crystal seeds with crystal habit of less than 150 mu m, keeping the temperature and stirring for 10min, wherein the adding amount of the crystal seeds is 7% of the mass of the added vitamin B6 crude product, the crystal seeds are shown in figure 4, cooling to 15 ℃, 4h is used for cooling, filtering is carried out after cooling, a small amount of ethanol is used for leaching a filter cake, finally, drying the filter cake to obtain 176.8g of vitamin B6 crystal, the 40 mesh passing rate of the obtained product is 93.2%, the particle ratio between 40 mesh and 100 mesh is 87.3%, and the repose angle is 19.4 ℃.
Example 9
Weighing 210g of vitamin B6 crude product (purity is more than 98%) in a 500ml crystallizer, adding 280g of water into the crystallizer, setting stirring speed to be 700rpm, heating to obtain a saturated solution at 72 ℃, cooling to 71 ℃, adding crystal seeds with crystal habit of less than 150 mu m, keeping the temperature and stirring for 10min, wherein the adding amount of the crystal seeds is 7% of the mass of the added vitamin B6 crude product, the crystal seeds are shown in figure 4, cooling to 15 ℃, cooling for 4h, filtering after cooling, eluting a filter cake with a small amount of ethanol, finally drying the filter cake to obtain 174.5g of vitamin B6 crystals, wherein the 40 mesh passing rate of the obtained product is 98.9%, the particle ratio between 40 mesh and 100 mesh is 97.1%, and the repose angle is 16 degrees.
Example 10
Weighing 285g of vitamin B6 crude product (purity is more than 98%) in a 500ml crystallizer, adding 280g of water into the crystallizer, setting stirring speed to be 700rpm, heating to obtain 80 ℃ saturated solution, cooling to 77 ℃, adding crystal seeds with crystal habit of less than 150 mu m, keeping the temperature and stirring for 10min, wherein the adding amount of the crystal seeds is 7% of the mass of the input vitamin B6 crude product, the crystal seeds are shown in figure 4, cooling to 15 ℃, cooling for 4.6h, filtering after cooling, eluting a filter cake with a small amount of ethanol, finally drying the filter cake to obtain 255.3g of vitamin B6 crystals, wherein the 40 mesh passing rate of the obtained product is 96.5%, the particle ratio between 40 mesh and 100 mesh is 93.2%, and the repose angle is 18.9 ℃.
Claims (8)
1. A method for preparing vitamin B6 granules with high flowability, comprising the steps of:
(1) Dissolving a vitamin B6 crude product in water to prepare a saturated solution of vitamin B6;
(2) Cooling the saturated solution of vitamin B6 obtained in the step (1) to obtain a supersaturated solution, adding vitamin B6 seed crystals, preserving heat, cooling and crystallizing under the condition of rapid stirring, and finally filtering and drying to obtain vitamin B6 crystal particles;
in the step (2), the size of the vitamin B6 seed crystal is smaller than 150 mu m, and the vitamin B6 seed crystal is a seed crystal with regular crystal habit;
in the step (1), the temperature of the saturated solution of the vitamin B6 is 50-90 ℃;
in the step (2), the rotating speed of the rapid stirring is 300-1200 rpm;
in the step (2), the mass ratio of the vitamin B6 seed crystal to the vitamin B6 crude product is 2-10: 100, controlling the temperature difference between the supersaturated solution and the saturated solution in the step (1) to be 1-6 ℃;
in the step (2), the end temperature of cooling crystallization is 5-30 ℃;
and cooling and crystallizing for 1-8 hours.
2. The method for preparing vitamin B6 particles with high fluidity according to claim 1, wherein in the step (1), the temperature of the saturated solution of vitamin B6 is 70-85 ℃.
3. The method for producing vitamin B6 particles having high flowability according to claim 1, wherein in step (2), the size of the vitamin B6 seed crystals is 40 to 80 μm.
4. The method for preparing vitamin B6 granules with high fluidity according to claim 1, wherein in the step (2), the rapid stirring speed is 500-1200 rpm.
5. The method for producing vitamin B6 pellets with high fluidity according to claim 1, wherein in step (2), the final temperature of the cooling crystallization is 10 to 25 ℃.
6. The method for preparing vitamin B6 particles with high fluidity according to claim 1, wherein in the step (2), the time for cooling crystallization is 4 to 6 hours.
7. The method for preparing vitamin B6 particles with high flowability according to claim 1, wherein the vitamin B6 particles have a 40 mesh passing rate of 90.0% -99.9%, a 40 mesh-100 mesh particle ratio of 85.0% -98.4% and an repose angle of less than 20.4 degrees.
8. The method for preparing vitamin B6 particles with high flowability according to claim 1, wherein the vitamin B6 particles have a 40 mesh passing rate of 92.0% -99.8%, a 40 mesh-100 mesh particle ratio of 85.0% -98.1% and an repose angle of 14.8-20.4 degrees.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0976757A2 (en) * | 1998-06-11 | 2000-02-02 | Nippon Mitsubishi Oil Corporation | A method of purifying vitamin B12 and/or derivatives thereof |
| CN102295598A (en) * | 2011-07-12 | 2011-12-28 | 湖北惠生药业有限公司 | Crystallization method of vitamin B6 |
| CN102442991A (en) * | 2010-10-12 | 2012-05-09 | 上海睿智化学研究有限公司 | Genistein vitamin B6 eutectic crystal and crystal and preparation method thereof |
| CN104710352A (en) * | 2013-12-13 | 2015-06-17 | 大丰海嘉诺药业有限公司 | Crystallization method of vitamin B6 |
-
2022
- 2022-06-29 CN CN202210751183.5A patent/CN115160218B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0976757A2 (en) * | 1998-06-11 | 2000-02-02 | Nippon Mitsubishi Oil Corporation | A method of purifying vitamin B12 and/or derivatives thereof |
| CN102442991A (en) * | 2010-10-12 | 2012-05-09 | 上海睿智化学研究有限公司 | Genistein vitamin B6 eutectic crystal and crystal and preparation method thereof |
| CN102295598A (en) * | 2011-07-12 | 2011-12-28 | 湖北惠生药业有限公司 | Crystallization method of vitamin B6 |
| CN104710352A (en) * | 2013-12-13 | 2015-06-17 | 大丰海嘉诺药业有限公司 | Crystallization method of vitamin B6 |
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