CN101899029A - Preparation method of vitamin C sodium salt - Google Patents
Preparation method of vitamin C sodium salt Download PDFInfo
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- CN101899029A CN101899029A CN 201010223684 CN201010223684A CN101899029A CN 101899029 A CN101899029 A CN 101899029A CN 201010223684 CN201010223684 CN 201010223684 CN 201010223684 A CN201010223684 A CN 201010223684A CN 101899029 A CN101899029 A CN 101899029A
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Abstract
The invention discloses a preparation method of vitamin C sodium salt. The method comprises the following steps of: adding 25 parts of vitamin C into 25 to 50 parts of water, stirring, gradually adding 10 to 15 parts of sodium bicarbonate at the temperature of between 15 and 70 DEG C to prepare 5 to 30 percent solution of sodium bicarbonate, and performing reaction for 30 to 60 minutes; closing and sealing a charging hole after charging is finished, introducing nitrogen for protection and keeping the temperature for 30 to 60 minutes; after the reaction is finished, filtering redundant materials and water insoluble matters in vacuum; concentrating mother solution under reduced pressure until water content is lower than 50 percent, stirring, cooling and crystallizing; slowly adding 50 to 200 parts of methanol, continuing stirring and crystallizing, and naturally cooling to room temperature; performing centrifugal separation, washing with the methanol and drying at the temperature of between 40 and 80 DEG C to obtain the product. The preparation method of the vitamin C sodium salt effectively reduces oxidation damage to the vitamin C due to the nitrogen protection in the preparation process and the final product has the advantages of high yield and good purity.
Description
Technical field
The present invention relates to the preparation field of vitamins C salt, relate in particular to a kind of preparation method of vitamin C sodium salt.
Background technology
At present, it is more serious often to find that in the preparation process of the sodium salt of vitamins C (xitix) vitamins C (xitix) content in reaction process that adds by normal amount reduces, and yield is low, causes bigger loss to manufacturer, also is the waste of resource.
Summary of the invention
The objective of the invention is to, a kind of preparation method of vitamin C sodium salt is provided, in preparation process, adopt nitrogen protection, effectively reduce ascorbic oxidation and destroy, thereby make final product have the productive rate height, the advantage that purity is good.
For solving above technical problem, technical scheme of the present invention is that a kind of preparation method of vitamin C sodium salt comprises the steps:
The first step, 25 parts of vitamins Cs add in 25-50 part water, stir, and adding the concentration that 10-15 part sodium bicarbonate is made under 15 ℃-70 ℃ gradually is the sodium hydrogen carbonate solution of 5%-30%, reacts 30-60 minute;
In second step, feeding intake finishes, and to close charging opening airtight, feeds nitrogen protection, is incubated 30-60 minute, and the reaction solution pH value is 4.0-6.5;
In the 3rd step, react the vacuum filtration that finishes and remove excessive materials and water-insoluble;
In the 4th step, mother liquor is evaporated to water content and is lower than 50%, stirs crystallisation by cooling;
In the 5th step, the methyl alcohol that slowly adds 50-200 part continues stirring and crystallizing, reduces to room temperature naturally;
In the 6th step, methanol wash is used in centrifugation, in 40 ℃-80 ℃ dry down products that get.
Preferably, in first step, adding 10-15 part concentration gradually under 25 ℃-55 ℃ is the sodium bicarbonate of 10%-30%.
Preferably, in the first step, described strength of solution is 10%-15%.
Preferably, in the first step, the ratio of described vitamins C and water is between 1: 1.2 to 1: 1.5.
Preferably, in the first step, the ratio of described vitamins C and sodium bicarbonate is between 1.5: 1 to 2: 1.
Preferably, in second step, the pressure of described nitrogen is 0.01-0.03MPa.
Preferably, in second step, described reaction solution pH value is 5.0-6.0.
Preferably, in second step, insulation reaction 40-60 minute.
Preferably, in the 6th step, at 50 ℃-60 ℃ dry down products that get.
Preferably, in the 6th step, adopt vacuum-drying or constant pressure and dry.
The preparation method of vitamin C sodium salt provided by the invention in preparation process, adopts nitrogen protection, effectively reduces ascorbic oxidation and destroys, thereby make final product have the productive rate height, the advantage that purity is good.
Embodiment
The preparation method's of vitamin C sodium salt provided by the invention basic design is that in preparation process, the employing nitrogen protection effectively reduces ascorbic oxidation and destroys, thereby make final product have the productive rate height, the advantage that purity is good.
Room temperature in the literary composition has three kinds of sayings usually: be respectively: (1) 23 ± 2 ℃; (2) 25 ± 5 ℃; (3) 20 ± 5 ℃.Wherein 23 ± 2 ℃ is normal room temperature, and 25 ± 5 ℃ is the room temperature in summer, and 20 ± 5 ℃ is the room temperature in winter.Room temperature among the present invention is meant 23 ± 2 ℃ normal room temperature.
Embodiment 1
The preparation method of the vitamin C sodium salt that present embodiment provides; the 50kg vitamins C is added in the 70kg water; stir; add concentration that the 25kg sodium bicarbonate is made into gradually and be 15% sodium hydrogen carbonate solution, reacted 60 minutes, feeding intake, it is airtight to close charging opening after finishing; feed the 0.01MPa nitrogen protection; be incubated 60 minutes, the reaction solution pH value is 6.5, reacts the vacuum filtration that finishes and removes excessive materials and water-insoluble; mother liquor is evaporated to water content and is lower than 50%; stir crystallisation by cooling. slowly add 2 00 liters methyl alcohol, continue stirring and crystallizing, reduce to room temperature naturally; centrifugation; use methanol wash, get product 55.1kg. yield 98%, purity 99.4% in 40 ℃ of following constant pressure and dries.
Embodiment 2
The preparation method of the vitamin C sodium salt that present embodiment provides; the 50kg vitamins C is added in the 70kg water; stir; add concentration that the 25kg sodium bicarbonate is made into gradually and be 10% sodium hydrogen carbonate solution, reacted 60 minutes, feeding intake, it is airtight to close charging opening after finishing; feed the 0.02MPa nitrogen protection; be incubated 30 minutes, the reaction solution pH value is 6.0, reacts the vacuum filtration that finishes and removes excessive materials and water-insoluble; mother liquor is evaporated to water content and is lower than 50%; stir crystallisation by cooling. slowly add 200 liters methyl alcohol, continue stirring and crystallizing, reduce to room temperature naturally; centrifugation; use methanol wash, get product 54.6kg. yield 97%, purity 99.5% in 55 ℃ of following vacuum-dryings.
Embodiment 3
The preparation method of the vitamin C sodium salt that present embodiment provides; the 50kg vitamins C is added in the 67kg water; stir; add concentration that the 26kg sodium bicarbonate is made into gradually and be 20% sodium hydrogen carbonate solution, reacted 50 minutes, feeding intake, it is airtight to close charging opening after finishing; feed the 0.02MPa nitrogen protection; be incubated 70 minutes, the reaction solution pH value is 5.8, reacts the vacuum filtration that finishes and removes excessive materials and water-insoluble; mother liquor is evaporated to water content and is lower than 50%; stir crystallisation by cooling. slowly add 200 liters methyl alcohol, continue stirring and crystallizing, reduce to room temperature naturally; centrifugation; use methanol wash, make product 54kg. yield 96%, purity 99.3% in 60 ℃ of following vacuum-dryings.
Embodiment 4
The preparation method of the vitamin C sodium salt that present embodiment provides; the 50kg vitamins C is added in the 67kg water; stir; add concentration that the 26kg sodium bicarbonate is made into gradually and be 25% sodium hydrogen carbonate solution; reacted 45 minutes; feeding intake, it is airtight to close charging opening after finishing; feed the 0.03MPa nitrogen protection; be incubated 70 minutes, the reaction solution pH value is 5.5, reacts the vacuum filtration that finishes and removes excessive materials and water-insoluble; mother liquor is evaporated to water content and is lower than 50%; stir crystallisation by cooling. slowly add 2 00 liters methyl alcohol, continue stirring and crystallizing, reduce to room temperature naturally; centrifugation; use methanol wash, get product 55.7kg. yield 98.6%, purity 99.6% in 50 ℃ of following vacuum-dryings.
Embodiment 5
The preparation method of the vitamin C sodium salt that present embodiment provides; the 50kg vitamins C is added in the 67kg water; stir; add concentration that the 23kg sodium bicarbonate is made into gradually and be 5% sodium hydrogen carbonate solution; reacted 40 minutes; feeding intake, it is airtight to close charging opening after finishing; feed the 0.02MPa nitrogen protection; be incubated 70 minutes, the reaction solution pH value is 4.0, reacts the vacuum filtration that finishes and removes excessive materials and water-insoluble; mother liquor is evaporated to water content and is lower than 50%; stir crystallisation by cooling. slowly add 2 00 liters methyl alcohol, continue stirring and crystallizing, reduce to room temperature naturally; centrifugation; use methanol wash, get product 53.7kg. yield 96.4%, purity 98.6% in 80 ℃ of following constant pressure and dries.
Only be preferred implementation of the present invention below, should be pointed out that above-mentioned preferred implementation should not be considered as limitation of the present invention, protection scope of the present invention should be as the criterion with claim institute restricted portion.For those skilled in the art, without departing from the spirit and scope of the present invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. the preparation method of a vitamin C sodium salt is characterized in that, comprises the steps:
The first step, 25 parts of vitamins Cs add in 25-50 part water, stir, and adding the concentration that 10-15 part sodium bicarbonate is made under 15 ℃-70 ℃ gradually is the sodium hydrogen carbonate solution of 5%-30%, reacts 30-90 minute;
In second step, feeding intake finishes, and to close charging opening airtight, feeds nitrogen protection, is incubated 30-90 minute, and the reaction solution pH value is 4.0-6.5;
In the 3rd step, react the vacuum filtration that finishes and remove excessive materials and water-insoluble;
In the 4th step, mother liquor is evaporated to water content and is lower than 50%, stirs crystallisation by cooling;
In the 5th step, the methyl alcohol that slowly adds 50-200 part continues stirring and crystallizing, reduces to room temperature naturally;
In the 6th step, methanol wash is used in centrifugation, in 40 ℃-80 ℃ dry down products that get.
2. the preparation method of vitamin C sodium salt according to claim 1 is characterized in that, in first step, adding 10-15 part concentration gradually under 25 ℃-55 ℃ is the sodium bicarbonate of 10%-30%.
3. the preparation method of vitamin C sodium salt according to claim 1 is characterized in that, in the first step, described strength of solution is 10%-15%.
4. the preparation method of vitamin C sodium salt according to claim 1 is characterized in that, in the first step, the ratio of described vitamins C and water is between 1: 1.2 to 1: 1.5.
5. the preparation method of vitamin C sodium salt according to claim 1 is characterized in that, in the first step, the ratio of described vitamins C and sodium bicarbonate is between 1.5: 1 to 2: 1.
6. the preparation method of vitamin C sodium salt according to claim 1 is characterized in that, in second step, the pressure of described nitrogen is 0.01-0.03MPa.
7. the preparation method of vitamin C sodium salt according to claim 1 is characterized in that, in second step, described reaction solution pH value is 5.0-6.0.
8. the preparation method of vitamin C sodium salt according to claim 1 is characterized in that, in second step, and insulation reaction 40-60 minute.
9. the preparation method of vitamin C sodium salt according to claim 1 is characterized in that, in the 6th step, at 50 ℃-60 ℃ dry down products that get.
10. the preparation method of vitamin C sodium salt according to claim 9 is characterized in that, in the 6th step, adopts vacuum-drying or constant pressure and dry.
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| CN 201010223684 CN101899029A (en) | 2010-07-09 | 2010-07-09 | Preparation method of vitamin C sodium salt |
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| CN 201010223684 CN101899029A (en) | 2010-07-09 | 2010-07-09 | Preparation method of vitamin C sodium salt |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104557822A (en) * | 2015-01-19 | 2015-04-29 | 精晶药业股份有限公司 | Refinement method of vitamin C sodium salt |
| CN105801537A (en) * | 2014-12-27 | 2016-07-27 | 辽宁药联制药有限公司 | Method for preparing sodium ascorbate |
| CN106632170A (en) * | 2016-12-23 | 2017-05-10 | 国家海洋局天津海水淡化与综合利用研究所 | Crystallization method of sodium ascorbate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101550118A (en) * | 2009-05-22 | 2009-10-07 | 徐建涛 | Synthetic process for vitamin C sodium salts |
| CN101735183A (en) * | 2010-01-26 | 2010-06-16 | 河北维尔康制药有限公司 | Method for synthesizing vitamin C sodium salt |
-
2010
- 2010-07-09 CN CN 201010223684 patent/CN101899029A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101550118A (en) * | 2009-05-22 | 2009-10-07 | 徐建涛 | Synthetic process for vitamin C sodium salts |
| CN101735183A (en) * | 2010-01-26 | 2010-06-16 | 河北维尔康制药有限公司 | Method for synthesizing vitamin C sodium salt |
Non-Patent Citations (2)
| Title |
|---|
| 《河北化工》 20100331 安立辉 维生素Ｃ钠盐生产中溶解投料水量的优化 49,73 1-10 第33卷, 第3期 2 * |
| 《辽宁化工》 20030531 张辉等 维生素C钙盐合成工艺的改进 188-189 1-10 第32卷, 第5期 2 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105801537A (en) * | 2014-12-27 | 2016-07-27 | 辽宁药联制药有限公司 | Method for preparing sodium ascorbate |
| CN104557822A (en) * | 2015-01-19 | 2015-04-29 | 精晶药业股份有限公司 | Refinement method of vitamin C sodium salt |
| CN106632170A (en) * | 2016-12-23 | 2017-05-10 | 国家海洋局天津海水淡化与综合利用研究所 | Crystallization method of sodium ascorbate |
| CN106632170B (en) * | 2016-12-23 | 2019-05-31 | 自然资源部天津海水淡化与综合利用研究所 | A kind of method for crystallising of vitamine C sodium |
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