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Preparation method of vitamin C magnesium ascorbyl phosphate

A technology of magnesium phosphate and vitamin, applied in the field of preparation of vitamin C derivatives, can solve the problems of difficulty in product separation and purification, low total product yield, complex synthesis process, etc., and achieves high impurity removal efficiency, simple process and simplified operation. effect of the program

Inactive Publication Date: 2014-03-26
WUXI KUAKE MICRONUTRIENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the synthesis route of this method is short, there are many by-products, it is difficult to separate and purify the product, and the total yield of the product is low
The traditional synthetic process of vitamin C magnesium phosphate is complex, with many impurities, and the use of organic solutions such as acetone will cause damage to the environment

Method used

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  • Preparation method of vitamin C magnesium ascorbyl phosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Embodiment one: a kind of preparation method of vitamin C magnesium phosphate, comprises the following processing steps:

[0015] (1) Add 110Kg vitamin C, 8.8Kg anhydrous calcium chloride, and 110Kg deionized water into a 500L reaction kettle at -10°C, stir for 2 hours, then add dropwise a 30% sodium hydroxide aqueous solution to adjust the pH 5, then add 110Kg of sodium trimetaphosphate, keep the temperature at 25°C, and react for 2 hours, and the obtained reactant is vitamin C ester calcium;

[0016] (2) Ascorbic acid ester calcium is added in the 500L bucket cleaner and washed with water, and then the pH is adjusted to 1.5 with sulfuric acid, and the reactant obtained is ascorbic acid phosphate;

[0017] (3) Carrying out nanofiltration membrane filtration of vitamin C phosphate through a roll-type nanofiltration membrane filter, the temperature at the roll-type nanofiltration membrane filter inlet is 120° C., and the temperature at the roll-type nanofiltration membra...

Embodiment 2

[0023] Embodiment two: a kind of preparation method of vitamin C magnesium phosphate, comprises the following processing steps:

[0024] (1) 110Kg vitamin C, 44Kg calcium chloride anhydrous, 550Kg deionized water are added in the 1000L reaction kettle of 20 ℃, stirred for 3 hours, then added dropwise the sodium hydroxide aqueous solution of concentration 70%, regulating pH is 10.5, then Add 275Kg of sodium trimetaphosphate, keep the temperature at 45°C, and react for 6 hours, and the obtained reactant is vitamin C ester calcium;

[0025] (2) Ascorbic acid ester calcium is added in the 1000L bucket cleaner and washed with water, and then the pH is adjusted to 3.5 with sulfuric acid, and the reactant obtained is vitamin C phosphate;

[0026] (3) Vitamin C phosphate is carried out nanofiltration membrane filtration through the roll type nanofiltration membrane filter, the temperature of the roll type nanofiltration membrane filter inlet is 140 ℃, and the temperature of the roll t...

Embodiment 3

[0029] Embodiment three: a kind of preparation method of vitamin C magnesium phosphate, comprises the following processing steps:

[0030] (1) 110Kg vitamin C, 22Kg anhydrous calcium chloride, 330Kg deionized water are added in the 800L reaction kettle of 10 ℃,, stir for 2.5 hours, then add dropwise the sodium hydroxide aqueous solution of concentration 60%, adjust pH to be 8, Then add 150Kg of sodium trimetaphosphate, keep the temperature at 35°C, and react for 4 hours, and the obtained reactant is vitamin C phosphate;

[0031] (2) Ascorbic acid phosphate is added in the 800L bucket cleaner and washed with water, and then the pH is adjusted to 2.5 with sulfuric acid, and the reactant obtained is ascorbic acid phosphate;

[0032] (3) Carry out nanofiltration membrane filtration with vitamin C phosphate through the roll-type nanofiltration membrane filter, the temperature of the roll-type nanofiltration membrane filter inlet is 130 ℃, and the temperature of the roll-type nanofi...

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Abstract

The invention discloses a preparation method of vitamin C magnesium ascorbyl phosphate. The preparation method is characterized by comprising the following process steps: (1), adding vitamin C, anhydrous calcium chloride and deionized water into a reaction kettle, adding sodium hydroxide aqueous liquor, and adding sodium trimetaphosphate to obtain vitamin C calcium ascorbyl phosphate; (2), adding the vitamin C ester calcium into a material barrel, washing by water, regulating pH value by sulfuric acid to obtain the vitamin C phosphate; (3), filtering the vitamin C phosphate by a roll type nanofiltration membrane filter; (4), adding the filtrate into a reaction kettle, passing through alkalescent anion exchange resin, eluting with hydrochloric acid, regulating pH with magnesium oxide to obtain vitamin C magnesium ascorbyl phosphate; and (5), passing the vitamin C magnesium ascorbyl phosphate through an active carbon filter, adding 95% alcohol in filtrate, spraying and drying to obtain a vitamin C magnesium ascorbyl phosphate finished product. According to the preparation method, an organic solvent is not adopted, whole process is simple and reaction time is shortened; moreover, the preparation method is safe to environment, and the finished product vitamin C magnesium ascorbyl phosphate is high in purity and good in stability.

Description

technical field [0001] The invention relates to the field of preparation of vitamin C derivatives, in particular to a preparation method of vitamin C magnesium phosphate. Background technique [0002] Magnesium vitamin C phosphate is a vitamin C derivative, which can improve the stability of vitamin C by derivatizing the 2-hydroxyl group into a phosphate ester, and the formed derivative can regenerate vitamin C after being hydrolyzed by phosphatase widely present in the body. Therefore, it has become the main ingredient of feed additives, food fortifiers and high-grade cosmetics whitening, and is a valuable fine chemical. [0003] So far, vitamin C phosphorylation mainly contains two methods: one is the phosphorylation of phosphorus oxychloride (as described in European Patent Nos. 388869 and 582924, U.S. Patent No. 4179445, Japanese Patent No. 60-69079, etc.), C is the raw material, and the hydroxyl groups on the 5- and 6-carbons are protected before esterification, that i...

Claims

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Application Information

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IPC IPC(8): C07F9/655
Inventor 郁建兴
Owner WUXI KUAKE MICRONUTRIENT
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