CN109553573B - Method for reducing active carbon dosage in vitamin B6 refining process - Google Patents
Method for reducing active carbon dosage in vitamin B6 refining process Download PDFInfo
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- CN109553573B CN109553573B CN201710881951.8A CN201710881951A CN109553573B CN 109553573 B CN109553573 B CN 109553573B CN 201710881951 A CN201710881951 A CN 201710881951A CN 109553573 B CN109553573 B CN 109553573B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- 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
- C07D213/04—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
- 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
- C07D213/62—Oxygen or sulfur atoms
- C07D213/63—One oxygen atom
- C07D213/65—One oxygen atom attached in position 3 or 5
- 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
- C07D213/67—2-Methyl-3-hydroxy-4,5-bis(hydroxy-methyl)pyridine, i.e. pyridoxine
Abstract
The invention relates to a method for reducing the using amount of activated carbon in a vitamin B6 refining process. Specifically, the invention provides a method for refining a crude vitamin B6 product, which comprises the following steps: 1) providing a first solution; 2) crystallizing the first solution to obtain primary crystallization mother liquor and a primary crystallization material; 3) dissolving the primary crystallization material in water, decoloring the primary crystallization material by using activated carbon, and crystallizing to obtain secondary crystallization mother liquor and a secondary crystallization material; 4) mixing the primary crystallization mother liquor and the secondary crystallization mother liquor, and crystallizing to obtain a tertiary crystallization material; 5) dissolving the tertiary crystallization material in water, decoloring the tertiary crystallization material by using the activated carbon used in the step 3), and crystallizing to obtain a quartic crystallization material; 6) and mixing the secondary crystallization material and the quartic crystallization material to obtain a vitamin B6 refined product. The method has the characteristics of high product quality, high yield, low production cost and small pressure of solid waste treatment.
Description
Technical Field
The invention relates to the technical field of vitamin production, in particular to a method for reducing the using amount of activated carbon in a vitamin B6 refining process.
Background
Vitamin B6 is also known as pyridoxine, a water-soluble vitamin. Vitamin B6 has important effects in preventing or treating vitamin B6 deficiency, preventing and treating isoniazid poisoning, treating infantile convulsion, and reducing leukopenia. In addition, vitamin B6 is an important coenzyme for poultry, and poultry cannot synthesize vitamin B6 and must take the vitamin B from feed. At present, the widely industrially applied method for producing vitamin B6 is an oxazole method, but the product obtained by the method has a darker color, and impurities are relatively close to the physicochemical properties of vitamin B6 and are relatively difficult to remove, so researchers have conducted many research and exploration on the process of vitamin B6, wherein the industrially applied method is mainly activated carbon decolorization and recrystallization.
Weekly Yuan et al (journal of Chinese medicine industry, 1994, 25(9):385-388) adopt two times of activated carbon decolorization and one time of anhydrous ethanol recrystallization, and the yield reaches 95 percent. However, the appearance and the solution color of the product obtained by the method do not completely reach the standard, and the activated carbon is decolorized twice, so that the product loss is more, and the anhydrous ethanol is adopted for recrystallization, so that the production cost is increased.
CN102295598 decolours the crude vitamin B6 product in water by using activated carbon, adds ethanol for recrystallization after cooling, and recovers the recrystallization mother liquor with the yield of 90-95%. However, the method uses a large amount of activated carbon and adopts ethanol for recrystallization, so that the cost and the pressure of solid waste treatment are increased.
Chentianhao et al (journal of Chinese medicine industry, 2004, 35(1):1-2) adopt three times of activated carbon decolorization and two times of aqueous phase recrystallization, and the yield can reach 89%. The method does not use absolute ethyl alcohol for recrystallization, greatly reduces the production cost, but needs active carbon for three times of decolorization, the total consumption of the active carbon is about 18 percent of the refined product, prolongs the suction filtration time, and leads to prolonged production period, increased product loss and increased solid waste.
In 2016, the yield of vitamin B6 in China is 6230 tons, and according to the refining method provided by Chentianhao and the like, the required active carbon dosage is up to 1121 tons, thereby bringing huge solid waste treatment pressure and higher production cost. With the national emphasis on the environmental protection problem of the pharmaceutical industry, the field urgently needs a vitamin B6 refining method which can improve the yield as much as possible, reduce solid waste and reduce the cost on the premise of obtaining qualified products.
Disclosure of Invention
The invention aims to provide a method for refining vitamin B6, which has the advantages of qualified product quality, low cost, less solid waste generation and short production period and is suitable for industrial production.
In a first aspect of the present invention, there is provided a method for refining a crude vitamin B6 product, comprising the steps of:
1) providing a first solution comprising crude vitamin B6 and water;
2) crystallizing the first solution to obtain primary crystallization mother liquor and a primary crystallization material;
3) dissolving the primary crystallization material in water, decoloring the primary crystallization material by using activated carbon, and crystallizing to obtain secondary crystallization mother liquor and a secondary crystallization material;
4) mixing the primary crystallization mother liquor and the secondary crystallization mother liquor, and crystallizing to obtain a tertiary crystallization material;
5) dissolving the tertiary crystallization material in water, decoloring the tertiary crystallization material by using the activated carbon used in the step 3), and crystallizing to obtain a quartic crystallization material;
6) and mixing the secondary crystallization material and the quartic crystallization material to obtain a vitamin B6 refined product.
In another preferred embodiment, the purity of the crude vitamin B6 product is 97% -98%.
In another preferred embodiment, the temperature of the first solution is 70-95 ℃, preferably 75-90 ℃.
In another preferred embodiment, in step 2), said crystallization is carried out at 0-30 ℃, preferably 5-25 ℃.
In another preferred embodiment, in step 3), the amount of the activated carbon is 1 to 5%, preferably 1.5 to 4%, more preferably 2 to 3.5%, and most preferably 2.1 to 3% of the amount of the crude vitamin B6.
In another preferred example, in step 3), the decolorization treatment is carried out at 70 to 95 ℃, preferably 75 to 90 ℃.
In another preferred example, in step 3), the treatment time of the decoloring treatment is 15 to 50min, preferably 20 to 40 min.
In another preferred embodiment, in step 3), said crystallization is carried out at 0-30 ℃, preferably 5-25 ℃.
In another preferred embodiment, in step 4), said crystallization is carried out at 0-30 ℃, preferably 5-25 ℃.
In another preferred embodiment, in step 5), the decolorization treatment is carried out at 70 to 95 ℃, preferably 75 to 90 ℃.
In another preferred example, in step 5), the treatment time of the decoloring treatment is 15 to 50min, preferably 20 to 40 min.
In another preferred embodiment, in step 5), said crystallization is carried out at 0-30 ℃, preferably 5-25 ℃.
In another preferred embodiment, the total yield of the vitamin B6 competitive products is more than or equal to 90 percent, preferably more than or equal to 95 percent.
In another preferred embodiment, the purity of the vitamin B6 competitive product is more than or equal to 99.5%, preferably more than or equal to 99.6%.
In a second aspect of the present invention, there is provided a vitamin B6 refined product, wherein the vitamin B6 refined product is obtained by the method of the first aspect of the present invention.
It is to be understood that within the scope of the present invention, the above-described features of the present invention and those specifically described below (e.g., in the examples) may be combined with each other to form new or preferred embodiments. Not to be reiterated herein, but to the extent of space.
Detailed Description
The inventor of the invention has conducted long-term and intensive research and obtains a method for refining vitamin B6, which has the advantages of meeting the requirements on product quality, low cost, less solid waste generation and short production period and is suitable for industrial production, by optimizing the refining process of vitamin B6. On this basis, the inventors have completed the present invention.
Refining method
The invention provides a method for reducing the using amount of active carbon in the refining process of vitamin B6, which comprises the steps of recrystallizing a vitamin B6 crude product with water, decoloring with the active carbon, concentrating the decolored solution, cooling and crystallizing to obtain vitamin B6 particles. And combining the recrystallization mother liquor and the refined mother liquor, and performing the operation to obtain the vitamin B6 granules again. And combining the two vitamin B6 granules to obtain the refined vitamin B6 product. The purity of the vitamin B6 obtained by the method is more than 99.5 percent, and the quality of the obtained product meets the requirements of BP2015, CP2015 and USP 38; the consumption of the active carbon is reduced, and the yield reaches 95 to 96 percent. The method reduces the consumption of the active carbon, relieves the pressure of solid waste treatment, shortens the production period, saves the production cost and is suitable for industrial production.
Specifically, the method comprises the following steps:
i) adding the vitamin B6 crude product into water, and heating to obtain a solution A of vitamin B6;
ii) cooling the vitamin B6 solution obtained in the step i) to obtain a recrystallized product of vitamin B6 and a filtrate A;
iii) adding the recrystallized product of vitamin B6 obtained in ii) to water to obtain vitamin B6 solution B;
iv) decoloring the solution obtained in the step iii) by using activated carbon;
v) concentrating the decolorized solution obtained in iv) to obtain a concentrated solution A;
vi) cooling the concentrated solution A obtained in the step v) to obtain vitamin B6 granules A and a filtrate B;
vii) combining the filtrate A obtained in the step ii) and the filtrate B obtained in the step vi), concentrating, and heating to obtain a concentrated solution B;
viii) subjecting the concentrate B obtained in vii) to operations ii, iii), iv), v) and vi) to obtain vitamin B6 granules B.
Wherein, the heating temperature in the i) and vii) is 70-90 ℃, and more preferably 90 ℃;
the temperature reduction temperature in the ii) and the vi) is 5-25 ℃, and preferably 20 ℃;
the proportion of the active carbon dosage of the iv) to the vitamin B6 recrystallization product is 3-10 percent, and the better proportion is 3 percent;
the decoloring operation in the iv) is carried out once;
the decolorization time in the iv) is 10 to 60 minutes, and more preferably 30 minutes;
the feed-liquid ratio of the v) concentrated solution A is 1:0.4-1:0.7, and the better feed-liquid ratio is 1: 0.4;
the purity of the vitamin B6 particle A and the vitamin B6 particle B is more than 99.5 percent;
the yield of the vitamin B6 particles is 90-96%.
It is to be understood that in the refining process of the present invention, the activated carbon is reused.
The reduction of the using amount of the active carbon in the refining process of the vitamin B6 can not only solve the problems of difficult suction filtration, increased adsorption loss and large pressure of solid waste treatment caused by large using amount of the active carbon, but also shorten the production period and reduce the production cost.
Compared with the prior art, the invention has the following main advantages:
(1) the method greatly reduces the consumption of the active carbon and reduces the production cost;
(2) the method obviously reduces the consumption of the active carbon (only 2.0-3.0 percent of the fine product) in the treatment process, thereby obviously relieving the pressure of solid waste treatment;
(3) the method has high yield (which can reach more than 95.5 percent and is more than 93 percent of the yield in the prior art);
(4) the purity of the vitamin B6 obtained by the method is more than 99.5%, and the product quality meets the requirements of BP2015, CP2015 and USP 38.
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The experimental procedures, in which specific conditions are not noted in the following examples, are generally carried out according to conventional conditions or according to conditions recommended by the manufacturers. Unless otherwise indicated, percentages and parts are by weight.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. In addition, any methods and materials similar or equivalent to those described herein can be used in the methods of the present invention. The preferred embodiments and materials described herein are intended to be exemplary only.
EXAMPLE 1 preparation of vitamin B6 Top-quality product 1
Adding 150.0g of vitamin B6 crude product 1 (with the purity of 98%) and 130mL of purified water into a reaction bottle, heating to 90 ℃ for dissolving to obtain a vitamin B6 solution 1, cooling to 20 ℃, filtering, and washing a filter cake with 20mL of ethanol to obtain a vitamin B6 primary crystallization mother liquor 1 and a vitamin B6 primary crystallization material 1. 1122.0 g of primary crystallized vitamin B6 material; adding the primary crystallization material 1 into 400mL of purified water, adding 3.4g of activated carbon, heating to 90 ℃, decoloring, preserving heat for 30 minutes, and filtering. Concentrating the hot filtrate until the ratio of the filtrate to the liquid is 1:0.4, and cooling to 20 ℃. Filtering, washing the filter cake with 15ml of 95% ethanol to obtain vitamin B6 secondary crystallization mother liquor 1 and vitamin B6 secondary crystallization material 1112.5 g, and combining the vitamin B6 primary crystallization mother liquor 1 and the vitamin B6 secondary crystallization mother liquor 1 to obtain vitamin B6 solution 1'. After the vitamin B6 solution 1' is concentrated to about 35ml, the concentrated solution is treated according to the treatment mode of the vitamin B6 solution 1, wherein the activated carbon for decolorization is the waste carbon used for the first time, 30.8g of quartic crystallization material 1 is obtained, vitamin B6 refined product 1(143.3g) is obtained by combining the secondary crystallization material 1 and the quartic crystallization material 1, the purity is 99.9%, the total yield is 95.5%, and the quality of the obtained product meets the requirements of BP2015, CP2015 and USP 38.
EXAMPLE 2 preparation of vitamin B6 Top-quality 2
Adding 300g of vitamin B6 crude product 2 (with the purity of 97.5%) and 280ml of purified water into a reaction bottle, heating to 75 ℃ for dissolving to obtain a vitamin B6 solution 2, cooling to 5 ℃, preserving heat for 2 hours at 5 ℃, filtering, washing a filter cake with 30ml of 95% ethanol to obtain vitamin B6 primary crystallization mother liquor 2 and vitamin B6 primary crystallization material 2256.2 g; adding 2 parts of vitamin B6 primary crystallization material and 6.71 parts of activated carbon into 870ml of purified water, heating to 75 ℃, decoloring and preserving heat for 30 minutes, filtering, concentrating the filtrate until the material-liquid ratio is 1:0.7, cooling to 20 ℃, preserving heat for 2 hours at 20 ℃, filtering, and washing a filter cake with 15ml of 95% ethanol to obtain 2225.5 g of vitamin B6 secondary crystallization mother liquor 2 and vitamin B6 secondary crystallization material. The vitamin B6 primary crystallization mother liquor 2 and the vitamin B6 secondary crystallization mother liquor 2 are combined to obtain a vitamin B6 solution 2 ', the vitamin B6 solution 2' is concentrated to about 80ml, the concentrated solution is treated according to the treatment mode of the vitamin B6 solution 2 (wherein activated carbon for decoloring is the waste carbon which is used for one time), so that 261.3 g of a fourth-time crystallization material is obtained, the secondary crystallization material 2 and the fourth-time crystallization material 2 are combined to obtain vitamin B6 refined product 2(286.8g), the purity is 99.5%, the total yield is 95.6%, and the obtained product quality meets the requirements of BP2015, CP2015 and USP 38.
EXAMPLE 3 preparation of vitamin B6 Top-quality product 3
Adding 200g of vitamin B6 crude product 3 (with the purity of 98 percent) and 180ml of purified water into a reaction bottle, heating to 90 ℃ for dissolving to obtain a vitamin B6 solution 3, cooling to 5 ℃, filtering, washing a filter cake with 20ml of 95 percent ethanol to obtain a vitamin B6 primary crystallization mother liquor 3 and a vitamin B6 primary crystallization material 3, 182.0 g; adding 3182.0 g of vitamin B6 primary crystallization material and 5.46g of activated carbon into 600ml of purified water, heating to 90 ℃, decoloring and preserving heat for 30min, filtering, concentrating the filtrate until the material-liquid ratio is 1:0.4, cooling to 5 ℃, filtering, washing the filter cake with 15ml of 95% ethanol, and obtaining 3169.26 g of vitamin B6 secondary crystallization mother liquor 3 and vitamin B6 secondary crystallization material. The vitamin B6 primary crystallization mother liquor 3 and the vitamin B6 secondary crystallization mother liquor 3 are combined to obtain a vitamin B6 solution 3 ', the vitamin B6 solution 3' is concentrated to about 30ml, the concentrated solution is treated according to the treatment mode of the vitamin B6 solution 3 (wherein activated carbon for decoloring is the waste carbon which is used for one time), 22.94g of vitamin B6 fourth-time crystallization material 3 is obtained, the secondary crystallization material 3 and the fourth-time crystallization material 3 are combined to obtain vitamin B6 fine product 3(192.2g), the purity is 99.6 percent, the total yield is 96.1 percent, and the quality of the obtained product meets the requirements of BP2015, CP2015 and USP 38.
Comparative example 1
Adding 150.0g of vitamin B6 crude product 4 (with the purity of 98%) and purified water into a reaction bottle, heating to 80 ℃ for dissolving to obtain vitamin B6 solution 4, adding 8g of used waste carbon for one time, preserving heat and decoloring for 30min, filtering, adding 4g of activated carbon into the filtrate, preserving heat and decoloring for 30min at 80 ℃ and decoloring for the second time. Filtering, concentrating until crystallization is separated out on the surface of the material, cooling, crystallizing, filtering to obtain a vitamin B6 primary crystallization mother liquor 4 and a vitamin B6 primary crystallization material 4, transferring to 600ml of distilled water, adding 4g of activated carbon, keeping the temperature at 80 ℃ for 30 minutes for carrying out third decolorization, filtering, concentrating the filtrate, crystallizing, filtering, washing a filter cake with 20ml of 95% ethanol to obtain a vitamin B6 secondary crystallization mother liquor 4 and a vitamin B6 secondary crystallization material 4110.8 g, wherein the yield is 74.5%, and the purity is 99.0%.
Comparative example 2
Adding 150.0g of vitamin B6 crude product 5 (with the purity of 98%), the primary and secondary crystallization mother liquor and purified water in the comparative example 1 into a reaction bottle, heating to 80 ℃ for dissolving to obtain vitamin B6 solution 5, adding 8g of used waste carbon, preserving heat and decoloring for 30min, filtering, adding 4g of activated carbon into the filtrate, preserving heat and decoloring for 30min at 80 ℃ and decoloring for the second time. Filtering, concentrating until crystallization is separated out on the surface of the material, cooling, crystallizing, filtering to obtain a vitamin B6 primary crystallization mother liquor 5 and a vitamin B6 primary crystallization material 5, transferring to 600ml of distilled water, adding 4g of activated carbon, keeping the temperature at 80 ℃ for 30 minutes for carrying out third decolorization, filtering, concentrating the filtrate, crystallizing, filtering, washing a filter cake with 20ml of 95% ethanol to obtain a vitamin B6 secondary crystallization mother liquor 5 and a vitamin B6 secondary crystallization material 5140.25 g, wherein the yield is 93.5%, and the purity is 98.9%.
All documents referred to herein are incorporated by reference into this application as if each were individually incorporated by reference. Furthermore, it should be understood that various changes and modifications of the present invention can be made by those skilled in the art after reading the above teachings of the present invention, and these equivalents also fall within the scope of the present invention as defined by the appended claims.
Claims (3)
1. A method for refining a vitamin B6 crude product is characterized in that,
adding 150.0g of vitamin B6 crude product 1 with the purity of 98% into a reaction bottle, heating 130mL of purified water to 90 ℃ for dissolving to obtain vitamin B6 solution 1, cooling to 20 ℃, filtering, and washing a filter cake with 20mL of ethanol to obtain vitamin B6 primary crystallization mother liquor 1 and vitamin B6 primary crystallization material 1; vitamin B6 primary crystallization material 1, 122.0 g; adding the primary crystallization material 1 into 400mL of purified water, adding 3.4g of activated carbon, heating to 90 ℃, decoloring, preserving heat for 30 minutes, and filtering; concentrating the hot filtrate until the ratio of the filtrate to the liquid is 1:0.4, and cooling to 20 ℃; filtering, washing a filter cake by 15ml of 95% ethanol to obtain a vitamin B6 secondary crystallization mother liquor 1 and a vitamin B6 secondary crystallization material 1, 112.5g, and combining the vitamin B6 primary crystallization mother liquor 1 and the vitamin B6 secondary crystallization mother liquor 1 to obtain a vitamin B6 solution 1'; after the vitamin B6 solution 1' is concentrated to about 35ml, the concentrated solution is treated according to the treatment mode of the vitamin B6 solution 1, the active carbon for decolorization is the waste carbon used for the first time, 30.8g of quartic crystallization material 1 is obtained, and the second crystallization material 1 and the quartic crystallization material 1 are combined to obtain vitamin B6 refined product 1, 143.3g, the purity is 99.9 percent, and the total yield is 95.5 percent.
2. A method for refining a vitamin B6 crude product is characterized in that,
adding 300g of vitamin B6 crude product 2 with the purity of 97.5 percent and 280ml of purified water into a reaction bottle, heating to 75 ℃ for dissolving to obtain vitamin B6 solution 2, cooling to 5 ℃, preserving the temperature for 2 hours at 5 ℃, filtering, washing a filter cake with 30ml of 95 percent ethanol to obtain vitamin B6 primary crystallization mother liquor 2 and vitamin B6 primary crystallization material 2, 256.2 g; adding 2 parts of vitamin B6 primary crystallization material and 6.71 parts of activated carbon into 870ml of purified water, heating to 75 ℃, decoloring and preserving heat for 30 minutes, filtering, concentrating the filtrate until the material-liquid ratio is 1:0.7, cooling to 20 ℃, preserving heat for 2 hours at 20 ℃, filtering, washing the filter cake with 15ml of 95% ethanol to obtain 2 parts of vitamin B6 secondary crystallization mother liquor and 225.5 parts of vitamin B6 secondary crystallization material; the vitamin B6 primary crystallization mother liquor 2 and the vitamin B6 secondary crystallization mother liquor 2 are combined to obtain a vitamin B6 solution 2 ', the vitamin B6 solution 2' is concentrated to about 80ml, the concentrated solution is treated according to the treatment mode of the vitamin B6 solution 2, wherein activated carbon for decolorization is the waste carbon which is used for the primary crystallization to obtain four-time crystallization materials 2 and 61.3g, and the secondary crystallization materials 2 and the four-time crystallization materials 2 are combined to obtain vitamin B6 refined products 2 and 286.8g, the purity is 99.5%, and the total yield is 95.6%.
3. A method for refining a vitamin B6 crude product is characterized in that,
adding 200g of vitamin B6 crude product 3 with the purity of 98 percent into a reaction bottle, heating 180ml of purified water to 90 ℃ for dissolving to obtain a vitamin B6 solution 3, cooling to 5 ℃, filtering, washing a filter cake with 20ml of 95 percent ethanol to obtain a vitamin B6 primary crystallization mother liquor 3 and a vitamin B6 primary crystallization material 3, 182.0 g; adding 3g, 182.0g of vitamin B6 primary crystallization material and 5.46g of activated carbon into 600ml of purified water, heating to 90 ℃, decoloring and preserving heat for 30min, filtering, concentrating the filtrate until the material-liquid ratio is 1:0.4, cooling to 5 ℃, filtering, washing the filter cake with 15ml of 95% ethanol to obtain 3g, 169.26g of vitamin B6 secondary crystallization mother liquor and 3g, 169.26g of vitamin B6 secondary crystallization material; combining the primary vitamin B6 crystallization mother liquor 3 and the secondary vitamin B6 crystallization mother liquor 3 to obtain a vitamin B6 solution 3 ', concentrating the vitamin B6 solution 3' to about 30ml, and treating the concentrated solution according to the treatment mode of the vitamin B6 solution 3, wherein activated carbon for decolorization is the waste carbon used for the primary use to obtain 22.94g of vitamin B6 quartic crystallization material 3, and combining the secondary crystallization material 3 and the quartic crystallization material 3 to obtain vitamin B6 refined product 3, 192.2g, the purity is 99.6%, and the total yield is 96.1%.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102295598A (en) * | 2011-07-12 | 2011-12-28 | 湖北惠生药业有限公司 | Crystallization method of vitamin B6 |
| WO2013018103A2 (en) * | 2011-08-04 | 2013-02-07 | Ramaswamy Rajendran | Extraction of b-vitamins from plant matter |
| 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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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102295598A (en) * | 2011-07-12 | 2011-12-28 | 湖北惠生药业有限公司 | Crystallization method of vitamin B6 |
| WO2013018103A2 (en) * | 2011-08-04 | 2013-02-07 | Ramaswamy Rajendran | Extraction of b-vitamins from plant matter |
| CN104710352A (en) * | 2013-12-13 | 2015-06-17 | 大丰海嘉诺药业有限公司 | Crystallization method of vitamin B6 |
Non-Patent Citations (1)
| Title |
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| 维生素B6的合成工艺改进;陈天豪等;《中国医药工业杂志》;20041231;第35卷(第1期);第2页右栏第2段 * |
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