CN1112418A - Preparing method of calcium ascorbate - Google Patents
Preparing method of calcium ascorbate Download PDFInfo
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- CN1112418A CN1112418A CN 94106062 CN94106062A CN1112418A CN 1112418 A CN1112418 A CN 1112418A CN 94106062 CN94106062 CN 94106062 CN 94106062 A CN94106062 A CN 94106062A CN 1112418 A CN1112418 A CN 1112418A
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- ascorbic acid
- calcium carbonate
- calcium
- calcium ascorbate
- ascorbate
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Abstract
A method for preparation of calcium ascorbate from ascorbic acid and calcium carbonate, the ascorbic acid is firstly dissolved in water with their weight ratio of 1:0.8-1, then ascorbic acid is reacted with calcium carbonate (mol ratio=2:1), under temp. 60-80 deg.C for 20-25 min., and under 40-60 deg.C to form crystal calcium ascorbate. The purity of the product is 99.5-99.8%, pH value of the water solution is 7.0-7.4, specific polarization is +95-+97 deg., and the rate of recovery is up to 85-90%.
Description
The present invention relates to a kind of manufacture method of calcium ascorbate.
As everyone knows, vitamin C is being undertaken extremely important role in human body, and demand is very big.The vitamin C of domestic market sale at present is highly acid, and pH reaches 2.0, after taking, makes gastrointestinal upset, is unfavorable for that especially the patient who suffers from gastropathy and duodenal ulcer takes, and healthy people also should not obey more.
It is a kind of neutral vitamin C that calcium ascorbate of the present invention (Calcium Ascorbate) can be described as, pH=7.0～7.4, and it had both had ascorbic activity, contained the calcium of ion-type again.Oxidized part in the product (dehydrogenation type ascorbic acid calcium) has mitigation to the misery of arthritis, phlebitis and patient with gout.
Ruskin at room temperature carries out at U.S.Pat.No.2596103 (1952) and the reaction of mentioning ascorbic acid and calcium carbonate in U.S.Pat.No.2631155 (1953), cleans the calcium ascorbate crystallization with organic solvent ethanol or acetone.The method is at room temperature reacted, and the response time is long, reacts not thorough.With the crystallization of organic solvent purification ascorbic acid, can improve purity, but the response rate is low, have only about 50% approximately.
Clarence Schreur mentions ascorbic acid and calcium carbonate in U.S.Pat.No.4251449 (1981) reaction temperature is 40～60 ℃, is no more than 70 ℃.Use excessive calcium carbonate.Entire reaction course CO
2Topped response surface can prevent the oxidized decomposition that ascorbic acid is too much.Because spontaneous crystallization at room temperature, crystal grain is little, and absorption impurity is many, and crystallization time is long.It is orange-yellow that product is, and its ascorbic acid calcium content has only 85～95%.PH is 5.7～6.0, and product purity is low.
It is short to the purpose of this invention is to provide a kind of response time, the method for the manufacturing calcium ascorbate that the response rate is high.
Another object of the present invention provides a kind of method that improves the purity of calcium ascorbate.
Purpose of the present invention is realized by following measure: ascorbic acid: water (weight ratio)=1: 0.8～1.Under 60 ℃ temperature, make dissolution of ascorbic acid.Press ascorbic acid: calcium carbonate (mol ratio)=2: 1, add calcium carbonate gradually, when adding calcium carbonate reaction temperature is brought up to till 80 ℃.Response time was controlled in 20～25 minutes, and reaction is reduced to room temperature after finishing, and keeps 10 minutes, is warmed up to 40～60 ℃ again, and agitation as appropriate generates the crystallization of big particle calcium ascorbate, removes mother solution, and vacuum and heating drying obtains white calcium ascorbate crystal.
Method of the present invention has following characteristics compared with prior art:
1. adopt to be higher than under the room temperature and dissolve ascorbic acid, can make it abundant dissolving, help reacting completely.
2. select the weight ratio of suitable ascorbic acid and water, the degree of super saturation of deposit is a most important factor in the deposition condition in the solution.The degree of super saturation of deposit is big more in the solution, and aggregation rate is big more, and the nucleus of generation is also many more, and nucleus is many more, and what obtain will be the tiny crystal of granule, adsorb impurity easily.Therefore, select the suitable water yield, control suitable mistake and degree, can generate comparatively thick crystal, be beneficial to purifying products.
3. crystallization process carries out in hot solution, because in hot solution, sedimentary dissolubility is general bigger, degree of super saturation reduction relatively, and the nucleus of generation can reduce, and agitation as appropriate in addition makes crystal grain thick again, and is favourable to raising calcium ascorbate purity.
The ascorbic acid calcium content (detection of standard iodine titrimetry) that adopts the method for the invention to make reaches 99.5～99.8%.The pH=7.0 of its solution～7.4, specific optical rotation :+95 °～+ 97 °.The response rate of this method reaches 85～90%.
The product composition: calcium ascorbate accounts for 85～87%
Dehydrogenation type ascorbic acid calcium accounts for 12～14%
Embodiment one:
With the open rustless steel anticorrosion reactor that has agitator, thermostat and thermometer, about 400 liters of volume.Add 50Kg ascorbic acid (medicinal raw material) and 50Kg distilled water, be warming up to 60 ℃, stirring and dissolving.Progressively add calcium carbonate subsequently, total addition is 14.2Kg.When constantly adding calcium carbonate, reaction temperature is risen to 80 ℃ gradually, the time was controlled within 20～25 minutes, the CO on question response thing surface
2Bubble collapse stops to stir, and product is reduced to room temperature as early as possible, keeps 10 minutes, makes temperature of reactor rise to 60 ℃ again, agitation as appropriate, treat that the big particle crystallization forms after, employing vacuum draw or the centrifugal mother solution of removing, heating in vacuum (40～50 ℃) drying.Overall process needs about 2 hours, obtains white calcium ascorbate crystallization 47.2Kg.Through detecting with the standard iodine titration, content is 99.8%, the pH=7.3 of its solution.
Embodiment two:
Equipment is basic identical with embodiment one with condition.
Ascorbic acid: water (weight ratio) is 1: 0.8, and promptly the 50Kg ascorbic acid adds 40Kg distilled water (60 ℃) dissolving.During crystallization, temperature of reactor rises to 40 ℃.Calcium carbonate adds total amount and is similarly 14.2Kg, obtains calcium ascorbate crystallization 50Kg, and content is 99.5%, its pH value of solution=7.0.
Claims (1)
1, a kind of method of making calcium ascorbate by ascorbic acid and calcium carbonate reaction, it is characterized in that by ascorbic acid: water (weight ratio)=1: 0.8～1, under 60 ℃ temperature, make dissolution of ascorbic acid, press ascorbic acid: calcium carbonate (mol ratio)=2: 1, add calcium carbonate gradually, when adding calcium carbonate reaction temperature is brought up to till 80 ℃, the response time was controlled in 20～25 minutes, after reaction finishes, reduce to room temperature, kept 10 minutes, be warmed up to 40～60 ℃ again, stir, generate the calcium ascorbate white crystals, remove mother solution, vacuum and heating drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94106062 CN1112418A (en) | 1994-05-25 | 1994-05-25 | Preparing method of calcium ascorbate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94106062 CN1112418A (en) | 1994-05-25 | 1994-05-25 | Preparing method of calcium ascorbate |
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| Publication Number | Publication Date |
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| CN1112418A true CN1112418A (en) | 1995-11-29 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 94106062 Pending CN1112418A (en) | 1994-05-25 | 1994-05-25 | Preparing method of calcium ascorbate |
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| CN (1) | CN1112418A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101899030A (en) * | 2010-07-09 | 2010-12-01 | 宜兴市江山生物科技有限公司 | Method for preparing vitamin C calcium salt |
| CN102219767A (en) * | 2011-04-27 | 2011-10-19 | 中国水产科学研究院南海水产研究所 | Method for preparing calcium ascorbate by utilizing shrimp shells |
| CN101322559B (en) * | 2008-07-18 | 2012-01-11 | 李卫平 | Multifunctional high-efficient calcium replenishing agent |
| 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 |
| CN104356101A (en) * | 2014-11-07 | 2015-02-18 | 李玉成 | Calcium acetylsalicylate ascorbate and preparation method thereof |
| CN106866592A (en) * | 2016-12-28 | 2017-06-20 | 安徽泰格生物技术股份有限公司 | A kind of preparation method of L Calcium Ascorbates |
| CN115109017A (en) * | 2022-07-19 | 2022-09-27 | 郑州瑞普生物工程有限公司 | Preparation method and application of calcium ascorbate |
-
1994
- 1994-05-25 CN CN 94106062 patent/CN1112418A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101322559B (en) * | 2008-07-18 | 2012-01-11 | 李卫平 | Multifunctional high-efficient calcium replenishing agent |
| CN101899030A (en) * | 2010-07-09 | 2010-12-01 | 宜兴市江山生物科技有限公司 | Method for preparing vitamin C calcium salt |
| CN102219767A (en) * | 2011-04-27 | 2011-10-19 | 中国水产科学研究院南海水产研究所 | Method for preparing calcium ascorbate by utilizing shrimp shells |
| CN102219767B (en) * | 2011-04-27 | 2013-06-26 | 中国水产科学研究院南海水产研究所 | Method for preparing calcium ascorbate by utilizing shrimp shells |
| 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 |
| CN104356101A (en) * | 2014-11-07 | 2015-02-18 | 李玉成 | Calcium acetylsalicylate ascorbate and preparation method thereof |
| CN106866592A (en) * | 2016-12-28 | 2017-06-20 | 安徽泰格生物技术股份有限公司 | A kind of preparation method of L Calcium Ascorbates |
| CN115109017A (en) * | 2022-07-19 | 2022-09-27 | 郑州瑞普生物工程有限公司 | Preparation method and application of calcium ascorbate |
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