CN101899030A - Method for preparing vitamin C calcium salt - Google Patents
Method for preparing vitamin C calcium salt Download PDFInfo
- Publication number
- CN101899030A CN101899030A CN 201010223697 CN201010223697A CN101899030A CN 101899030 A CN101899030 A CN 101899030A CN 201010223697 CN201010223697 CN 201010223697 CN 201010223697 A CN201010223697 A CN 201010223697A CN 101899030 A CN101899030 A CN 101899030A
- Authority
- CN
- China
- Prior art keywords
- calcium salt
- preparing vitamin
- vitamin
- salt according
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a method for preparing vitamin C calcium salt, which comprises the following steps of: adding 25 parts of vitamin C into 25 to 50 parts of water, stirring the mixture, gradually adding 10 to 15 parts of slaked lime into the mixture at the temperature of between 15 and 70 DEG C to prepare 5 to 30 percent suspension, and reacting the suspension for 30 to 60 minutes; sealing a feeding hole after the materials are completely fed, introducing nitrogen for protection, and preserving the heat for 30 to 60 minutes; performing vacuum filtration after the reaction is finished to remove excessive materials and water-insoluble substances; concentrating mother solution with reduced pressure till the water content is lower than 50 percent, and stirring, cooling and crystallizing the mother solution; slowly adding 50 to 200 parts of methanol into the solution, continuously stirring the solution to separate out crystals, and naturally cooling the solution to room temperature; centrifuging the solution, washing the solid by using methanol, and drying the solid at the temperature of between 40 and 80 DEG C to obtain a product. The invention provides the method for preparing the vitamin C calcium salt; and during the preparation, the nitrogen is adopted for protection so that oxidative damage of the vitamin C is effectively reduced 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 preparing vitamin C calcium 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 preparing vitamin C calcium 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 preparing vitamin C calcium salt comprises the steps:
The first step, 25 parts of vitamins Cs add in 25-50 part water, stir, and add 3-8 part white lime gradually and be made into the suspension that concentration is 10%-30% under 15 ℃-70 ℃, react 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.
Preferably, in first step, adding the concentration that 3-8 part white lime is made under 25 ℃-55 ℃ gradually is the suspension of 10%-30%.
Preferably, in the first step, the concentration of described suspension is 15%-20%.
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 white lime is between 3: 1 to 5: 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.
Preparing vitamin C calcium 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 basic design of preparing vitamin C calcium salt provided by the invention 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 preparing vitamin C calcium salt that present embodiment provides; the 50kg vitamins C is added in the 70kg water; stir; add concentration that 10kg white lime is made into gradually and be 20% suspension, 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 200 liters methyl alcohol, continue stirring and crystallizing, reduce to room temperature naturally; centrifugation; use methanol wash, get product 58.8kg. yield 98%, purity 99.7% in 40 ℃ of following constant pressure and dries.
Embodiment 2
The preparing vitamin C calcium salt that present embodiment provides; the 50kg vitamins C is added in the 70kg water; stir; adding 10kg white lime gradually, to be made into concentration be 15% suspension, reacted 60 minutes, and 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 57.8kg. yield 97.3%, purity 99.5% in 55 ℃ of following vacuum-dryings.
Embodiment 3
The preparing vitamin C calcium salt that present embodiment provides; the 50kg vitamins C is added in the 65kg water; stir; add concentration that 10.5kg white lime is made into gradually and be 16% suspension, reacted 50 minutes, feeding intake, it is airtight to close charging opening after finishing; feed the 0.015MPa nitrogen protection; be incubated 70 minutes, the reaction solution pH value is 6.3, 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 58.6kg. yield 97%, purity 99.2% in 60 ℃ of following vacuum-dryings.
Embodiment 4
The preparing vitamin C calcium salt that present embodiment provides; the 50kg vitamins C is added in the 68kg water; stir; adding 9.4kg white lime gradually, to be made into concentration be 10% suspension, reacted 45 minutes, and 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 200 liters methyl alcohol, continue stirring and crystallizing, reduce to room temperature naturally; centrifugation; use methanol wash, get product 57.7kg. yield 96.1%, purity 99.6% in 50 ℃ of following vacuum-dryings.
Embodiment 5
The preparing vitamin C calcium salt that present embodiment provides; the 50kg vitamins C is added in the 67kg water; stir, add 9.8kg white lime gradually, be made into concentration and be 5% suspension; reacted 40 minutes; feeding intake, it is airtight to close charging opening after finishing, and feeds the 0.02MPa nitrogen protection, is incubated 70 minutes; the reaction solution pH value is 4.0; react the vacuum filtration that finishes and remove excessive materials and water-insoluble, mother liquor is evaporated to water content and is lower than 50%, stirs crystallisation by cooling. slowly add 200 liters methyl alcohol; continue stirring and crystallizing; naturally reduce to room temperature, methanol wash is used in centrifugation; get product 58.1kg. yield 97.9%, 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. a preparing vitamin C calcium salt is characterized in that, comprises the steps:
The first step, 25 parts of vitamins Cs add in 25-50 part water, stir, and add 3-8 part white lime gradually and be made into the suspension that concentration is 10%-30% under 15 ℃-70 ℃, react 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. preparing vitamin C calcium salt according to claim 1 is characterized in that, in first step, adding the concentration that 3-8 part white lime is made under 25 ℃-55 ℃ gradually is the suspension of 10%-30%.
3. preparing vitamin C calcium salt according to claim 1 is characterized in that, in the first step, the concentration of described suspension is 15%-20%.
4. preparing vitamin C calcium 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. preparing vitamin C calcium salt according to claim 1 is characterized in that, in the first step, the ratio of described vitamins C and white lime is between 3: 1 to 5: 1.
6. preparing vitamin C calcium salt according to claim 1 is characterized in that, in second step, the pressure of described nitrogen is 0.01-0.03MPa.
7. preparing vitamin C calcium salt according to claim 1 is characterized in that, in second step, described reaction solution pH value is 5.0-6.0.
8. preparing vitamin C calcium salt according to claim 1 is characterized in that, in second step, and insulation reaction 40-60 minute.
9. preparing vitamin C calcium salt according to claim 1 is characterized in that, in the 6th step, at 50 ℃-60 ℃ dry down products that get.
10. preparing vitamin C calcium salt according to claim 9 is characterized in that, in the 6th step, adopts vacuum-drying or constant pressure and dry.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010223697 CN101899030A (en) | 2010-07-09 | 2010-07-09 | Method for preparing vitamin C calcium salt |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010223697 CN101899030A (en) | 2010-07-09 | 2010-07-09 | Method for preparing vitamin C calcium salt |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101899030A true CN101899030A (en) | 2010-12-01 |
Family
ID=43224992
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010223697 Pending CN101899030A (en) | 2010-07-09 | 2010-07-09 | Method for preparing vitamin C calcium salt |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101899030A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102349892A (en) * | 2011-08-17 | 2012-02-15 | 江门市新会区光华生物科技有限公司 | High-content vitamin C tablets and preparation method thereof |
| CN102372686A (en) * | 2011-12-02 | 2012-03-14 | 江西省德兴市百勤异Vc钠有限公司 | Method for preparing D-calcium erythorbate |
| CN102584753A (en) * | 2011-11-01 | 2012-07-18 | 江苏江山制药有限公司 | Processing method of low-turbidity vitamin C calcium |
| CN108276368A (en) * | 2018-03-28 | 2018-07-13 | 安徽泰格生物技术股份有限公司 | A method of preparing vitamin C calcium salt |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1107845A (en) * | 1994-01-13 | 1995-09-06 | 中国人民解放军中南新技术研究所 | Preparation method of calcium ascorbate |
| CN1112418A (en) * | 1994-05-25 | 1995-11-29 | 广州医学院 | Preparing method of calcium ascorbate |
| WO2008053437A2 (en) * | 2006-11-02 | 2008-05-08 | Mb Med S.R.L. | A method for preparing ascorbic acid or a salt thereof from plant matrices |
-
2010
- 2010-07-09 CN CN 201010223697 patent/CN101899030A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1107845A (en) * | 1994-01-13 | 1995-09-06 | 中国人民解放军中南新技术研究所 | Preparation method of calcium ascorbate |
| CN1112418A (en) * | 1994-05-25 | 1995-11-29 | 广州医学院 | Preparing method of calcium ascorbate |
| WO2008053437A2 (en) * | 2006-11-02 | 2008-05-08 | Mb Med S.R.L. | A method for preparing ascorbic acid or a salt thereof from plant matrices |
Non-Patent Citations (2)
| Title |
|---|
| 《河北师范大学学报(自然科学版)》 19990331 周友亚 等 抗坏血酸钙的合成及抗氧化作用 94-96 1-10 第23卷, 第1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 |
|---|---|---|---|---|
| CN102349892A (en) * | 2011-08-17 | 2012-02-15 | 江门市新会区光华生物科技有限公司 | High-content vitamin C tablets and preparation method thereof |
| CN102584753A (en) * | 2011-11-01 | 2012-07-18 | 江苏江山制药有限公司 | Processing method of low-turbidity vitamin C calcium |
| CN102372686A (en) * | 2011-12-02 | 2012-03-14 | 江西省德兴市百勤异Vc钠有限公司 | Method for preparing D-calcium erythorbate |
| CN108276368A (en) * | 2018-03-28 | 2018-07-13 | 安徽泰格生物技术股份有限公司 | A method of preparing vitamin C calcium salt |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101899030A (en) | Method for preparing vitamin C calcium salt | |
| CN106588709A (en) | Preparation method for sodium fatty acyl methyl taurate | |
| CN105461579A (en) | Preparation method of imino-disuccinic acid and salt thereof | |
| CN111548291B (en) | Environment-friendly synthetic method of scorch retarder N-phenyl-N-trichloromethylthio benzenesulfonamide | |
| CN103950899A (en) | Calcium peroxide preparation method | |
| CN110697731A (en) | Method for preparing ammonium sulfate and calcium carbonate from desulfurized gypsum | |
| CN101024605A (en) | Method for preparing novel organic calcium using egg shell | |
| CN101899029A (en) | Preparation method of vitamin C sodium salt | |
| CN112552167B (en) | Preparation method of calcium gluconate | |
| CN101781264B (en) | Production method of 1-methyl-5-mercapto-1,2,3,4-tetrazole | |
| KR101952060B1 (en) | Method for preparing furan-2,5-dicarboxylic acid (FDCA) from solid salt | |
| CN1125773C (en) | Production method of feed-level calcium hydrogen phosphate | |
| CN109867587B (en) | Preparation method of 3-chloro-1,2-propanediol | |
| CN102020293B (en) | Method for recovering reagent grade sodium nitrate from waste liquid generated in citric acid bismuth production | |
| CN114736144A (en) | Industrial preparation method of docusate calcium | |
| CN114213456A (en) | Preparation method of spermine | |
| CN114292203A (en) | Preparation method of DL-panthenol | |
| CN110467537B (en) | Preparation process of L-p-hydroxyphenylglycine | |
| CN102863544A (en) | Binding agent with viscosity of 50-80 mPa.s, and preparation method and application thereof | |
| CN114014835A (en) | Glycolide purification process | |
| CN111574387A (en) | P-aminomethyl benzoic acid and preparation method thereof | |
| CN112194110A (en) | Method for preparing industrial-grade potassium dihydrogen phosphate | |
| JPS61155349A (en) | Manufacture of anthraquinone dispersion and use of same for wood alkali digestion | |
| CN106748738A (en) | A kind of Optimized Extraction technique of separating formic sodium | |
| CN105330677B (en) | A kind of preparation method of cefmetazole sodium |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20101201 |