CN102372686A - Method for preparing D-calcium erythorbate - Google Patents
Method for preparing D-calcium erythorbate Download PDFInfo
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- CN102372686A CN102372686A CN2011103948892A CN201110394889A CN102372686A CN 102372686 A CN102372686 A CN 102372686A CN 2011103948892 A CN2011103948892 A CN 2011103948892A CN 201110394889 A CN201110394889 A CN 201110394889A CN 102372686 A CN102372686 A CN 102372686A
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- Prior art keywords
- saccharosonic acid
- calcium
- acid calcium
- erythorbic acid
- saccharosonic
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Abstract
The invention discloses a method for preparing D-calcium erythorbate by taking D-erythorbic acid as a raw material. The method comprises the following steps of: dissolving D-erythorbic acid into water, and neutralizing D-erythorbic acid by adopting CaCO3, CaO or Ca(OH)2 which is 0.4-0.5 time the molar weight of the D-erythorbic acid, wherein the reacting temperature is at 5-6 DEG C; filtering and removing insoluble impurities from a neutralizing liquid, and concentrating a filtrate to slurry state under reduced pressure; and adding absolute methanol or absolute ethanol into slurry till the volume of the absolute methanol or absolute ethanol accounts for over 90 percent of the total volume of the mixed solution, slowly stirring till crystals are separated out, filtering to obtain wet D-calcium erythorbate, and drying to obtain finished D-calcium erythorbate. The yield of the D-calcium erythorbate prepared with the method is over 83 percent, and the purity is over 98 percent.
Description
Technical field
The invention provides a kind of is raw material with the D-saccharosonic acid, prepares the method for D-saccharosonic acid calcium, belongs to field of fine chemical.
Background technology
The D-saccharosonic acid is a kind of optical isomer of L-xitix (vitamins C), and reductibility is strong.The D-saccharosonic acid is similar with vitamins C on chemical property, and antioxidant property is superior to vitamins C, and food and drug administration (FDA) classifies the D-saccharosonic acid as the generally recognized as safe material.Aspect physiological effect, ascorbic 1/20 although the anti-vitamin C deficiency effect of D-saccharosonic acid is merely, it has step-down, diuresis, detoxifcation, the promotion liver is glycogenesis and the effect of chromocrinia and vitamins C much at one.
At present, relevant L-calcium ascorbate preparation method has a small amount of report, but does not see public reported about the synthetic of D-calcium ascorbate, and it is also rare to relate to the application report of D-calcium ascorbate.
Summary of the invention
The object of the invention provides a kind of preparation method of D-saccharosonic acid calcium.
Of the present inventionly take following means:
(1) the D-saccharosonic acid is dissolved in zero(ppm) water or the deionized water, adopts CaCO
3, CaO or Ca (OH)
2In with the D-saccharosonic acid, 5 ℃～60 ℃ of temperature of reaction.Remove by filter the insoluble impurities in the neutralizer, concentrating under reduced pressure is filtrated to pulpous state.Anhydrous methanol or absolute ethyl alcohol are joined in the soup compound, slowly be stirred to crystallization and separate out, through filtration, drying treatment, obtain D-saccharosonic acid calcium finished product again.
(2) the D-saccharosonic acid is dissolved in zero(ppm) water or the deionized water, adopts 0.4～0.5 times of mole dosage to the CaCO of D-saccharosonic acid
3, CaO or Ca (OH)
2Carry out neutralization reaction.
(3) adopt anhydrous methanol or absolute ethyl alcohol to join in the soup compound as recrystallisation solvent, the volume of anhydrous methanol or absolute ethyl alcohol accounts for more than 90% of mixed solution TV.
Reaction conditions of the present invention is gentle, and technological operation is easy, is prone to realize suitability for industrialized production.The calcareous amount of D-saccharosonic acid is stable, and yield is more than 83%, and purity is more than 98%.
Embodiment
Embodiment 1:
Under the room temperature, the D-saccharosonic acid of 180.0g is dissolved in the zero(ppm) water of 1200mL, stirs the light calcium carbonate neutralization that slowly adds 46.0g down.After question response liquid became transparent solution, centrifugal (4000r/min 20min) removed the wherein insoluble impurities of minute quantity.Filtrate to syrupy shape with the rotatory evaporator concentrating under reduced pressure, it is added in the anhydrous methanol of 2000mL, slowly stir 2h, filter the wet article of D-saccharosonic acid calcium that obtain.The drying under reduced pressure D-saccharosonic acid calcium article 8h that wets, D-saccharosonic acid calcium finished product 169.7g.Its yield is 84.50% of a theoretical yield, and product purity is 99.31%.
Embodiment 2:
Under the room temperature, the D-saccharosonic acid of 175.0g is dissolved in the zero(ppm) water of 1150mL, stirs the light calcium carbonate neutralization that slowly adds 45.0g down.After question response liquid became transparent solution, suction filtration was removed the wherein insoluble impurities of minute quantity.Filtrate to syrupy shape with the rotatory evaporator concentrating under reduced pressure, it is added in the absolute ethyl alcohol of 2000mL, slowly stir 2.5h, filter the wet article of D-saccharosonic acid calcium that obtain.The drying under reduced pressure D-saccharosonic acid calcium article 8h that wets, D-saccharosonic acid calcium finished product 165.4g.Its yield is 84.17% of a theoretical yield, and product purity is 98.67%.
Embodiment 3:
Under the room temperature, the D-saccharosonic acid of 175.0g is dissolved in the zero(ppm) water of 1150mL, stirs the quicklime neutralization that slowly adds 27.5g down.After question response liquid became transparent solution, centrifugal (4000r/min 20min) removed the wherein insoluble impurities of minute quantity.Filtrate to syrupy shape with the rotatory evaporator concentrating under reduced pressure, it is added in the anhydrous methanol of 1600mL, slowly stir 2h, filter the wet article of D-saccharosonic acid calcium that obtain.The drying under reduced pressure D-saccharosonic acid calcium article 10h that wets, D-saccharosonic acid calcium finished product 163.6g.Its yield is 83.14% of a theoretical yield, and product purity is 98.54%.
Embodiment 4:
Under the room temperature, the D-saccharosonic acid of 175.0g is dissolved in the zero(ppm) water of 1150mL, stirs the calcium hydroxide neutralization that slowly adds 36.5g down.After question response liquid became transparent solution, centrifugal (4000r/min 20min) removed the wherein insoluble impurities of minute quantity.Filtrate to syrupy shape with the rotatory evaporator concentrating under reduced pressure, it is added in the anhydrous methanol of 1600mL, slowly stir 3h, filter the wet article of D-saccharosonic acid calcium that obtain.The drying under reduced pressure D-saccharosonic acid calcium article 10h that wets, D-saccharosonic acid calcium finished product 164.8g.Its yield is 84.17% of a theoretical yield, and product purity is 99.03%.
Embodiment 5:
Under the room temperature, the D-saccharosonic acid of 25.0g is dissolved in the zero(ppm) water of 300mL, stirs the light calcium carbonate neutralization that slowly adds 6.5g down.After question response liquid became transparent solution, the D-saccharosonic acid with 25.0g added in the reaction solution again, and neutralized with the light calcium carbonate of 6.5g.So repetitive operation is 6 times, and the add-on of D-saccharosonic acid amounts up to 175.0g in reaction solution.After neutralization reaction finished, operation thereupon got D-saccharosonic acid calcium finished product 167.5g with embodiment 2.Its yield is 85.38% of a theoretical yield, and product purity is 98.83%.
Claims (3)
1. a method for preparing D-saccharosonic acid calcium is characterized in that: in the aqueous solution, adopt CaCO
3, CaO or Ca (OH)
2In with the D-saccharosonic acid, 5 ℃～60 ℃ of temperature of reaction; Remove by filter the insoluble impurities in the neutralizer, concentrating under reduced pressure is filtrated to pulpous state; Anhydrous methanol or absolute ethyl alcohol are joined in the soup compound, slowly be stirred to crystallization and separate out, through filtration, drying treatment, obtain D-saccharosonic acid calcium finished product again;
The D-saccharosonic acid calcium yield that adopts this method preparation is more than 83%, and purity is more than 98%.
2. the described a kind of method for preparing high purity D-saccharosonic acid calcium of claim 1, in it is characterized in that with the used CaCO of D-saccharosonic acid
3, CaO or Ca (OH)
2Mole dosage be 0.4～0.5 times of D-saccharosonic acid.
3. the described a kind of method for preparing high purity D-saccharosonic acid calcium of claim 1 is characterized in that accounting for more than 90% of mixed solution TV as the anhydrous methanol of solvent or the volume of absolute ethyl alcohol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103948892A CN102372686A (en) | 2011-12-02 | 2011-12-02 | Method for preparing D-calcium erythorbate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103948892A CN102372686A (en) | 2011-12-02 | 2011-12-02 | Method for preparing D-calcium erythorbate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102372686A true CN102372686A (en) | 2012-03-14 |
Family
ID=45791972
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|---|---|---|---|
| CN2011103948892A Pending CN102372686A (en) | 2011-12-02 | 2011-12-02 | Method for preparing D-calcium erythorbate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103739579A (en) * | 2013-12-20 | 2014-04-23 | 李玉成 | Citric acid dehydrogenated calcium ascorbate and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2596103A (en) * | 1947-03-28 | 1952-05-13 | Simon L Ruskin | Crystalline calcium ascorbate and method of preparing same |
| US2631155A (en) * | 1946-10-03 | 1953-03-10 | Physiological Chemical Company | Crystalline calcium ascorbate |
| CN1112418A (en) * | 1994-05-25 | 1995-11-29 | 广州医学院 | Preparing method of calcium ascorbate |
| 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 |
-
2011
- 2011-12-02 CN CN2011103948892A patent/CN102372686A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2631155A (en) * | 1946-10-03 | 1953-03-10 | Physiological Chemical Company | Crystalline calcium ascorbate |
| US2596103A (en) * | 1947-03-28 | 1952-05-13 | Simon L Ruskin | Crystalline calcium ascorbate and method of preparing same |
| CN1112418A (en) * | 1994-05-25 | 1995-11-29 | 广州医学院 | Preparing method of calcium ascorbate |
| 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 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103739579A (en) * | 2013-12-20 | 2014-04-23 | 李玉成 | Citric acid dehydrogenated calcium ascorbate and preparation method and application thereof |
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Application publication date: 20120314 |