Preparation method of sodium ascorbyl phosphate

A technology of sodium phosphate and vitamins, applied in the field of preparation of vitamin C derivatives, can solve the problems of difficult product separation and purification, complex synthesis process, and low total product yield, and achieve high impurity removal efficiency, simple process, and shortened reaction the effect of time

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 trad

Method used

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  • Preparation method of sodium ascorbyl phosphate
  • Preparation method of sodium ascorbyl phosphate

Examples

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Embodiment 1

[0016] Embodiment one: a kind of preparation method of vitamin C phosphate sodium, comprises the following processing steps:

[0017] (1) Adding 100Kg vitamin C, 6Kg anhydrous calcium chloride, and 100Kg deionized water into a 500L reaction kettle at -10°C, stirred for 1 hour, then added dropwise an aqueous sodium hydroxide solution with a concentration of 30%, and adjusted the pH to 6. Then add 50Kg of sodium trimetaphosphate, keep the temperature at 25°C, and react for 3 hours, and the obtained reactant is vitamin C ester calcium;

[0018] (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 hydrochloric acid, and the reactant obtained is vitamin C phosphate;

[0019] (3) Carry out membrane filtration with vitamin C phosphate through the microtube type dynamic membrane filter, the temperature of the microtube type dynamic membrane filter inlet is 100 ℃, the temperature of the microtube type dynamic...

Embodiment 2

[0028] Embodiment two: a kind of preparation method of vitamin C phosphate sodium, comprises the following processing steps:

[0029] (1) 100Kg vitamin C, 30Kg anhydrous calcium chloride, and 700Kg deionized water are added into a 1000L reaction kettle at 20°C, stirred for 2 hours, then added dropwise with a 50% aqueous sodium hydroxide solution to adjust the pH to 11 , then add 150Kg of sodium trimetaphosphate, keep the temperature at 45°C, react for 5 hours, and the reactant obtained is vitamin C ester calcium;

[0030] (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 hydrochloric acid, and the reactant obtained is ascorbic acid phosphate;

[0031] (3) Carry out membrane filtration with vitamin C phosphate through the microtube type dynamic membrane filter, the temperature of the microtube type dynamic membrane filter inlet is 120 ℃, the temperature of the microtube type dynamic membrane filte...

Embodiment 3

[0036] Embodiment three: a kind of preparation method of vitamin C phosphate sodium, comprises the following processing steps:

[0037] (1) Adding 100Kg vitamin C, 20Kg anhydrous calcium chloride, and 600Kg deionized water into an 800L reaction kettle with a temperature of 10°C, stirred for 1.5 hours, then added dropwise an aqueous solution of sodium hydroxide with a concentration of 40%, and adjusted the pH to 9 , then add 100Kg of sodium trimetaphosphate, keep the temperature at 35°C, and react for 4 hours, and the obtained reactant is vitamin C ester calcium;

[0038](2) Ascorbic acid ester calcium is added in the 800L bucket cleaner and washed with water, then the pH is adjusted to be 2.5 with hydrochloric acid, and the reactant obtained is ascorbic acid phosphate;

[0039] (3) Carry out membrane filtration with vitamin C phosphate through the microtube type dynamic membrane filter, the temperature of the microtube type dynamic membrane filter inlet is 110 ℃, the temperatu...

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Abstract

The invention relates to a preparation method of sodium ascorbyl phosphate, which is characterized by comprising the following steps: (1) adding ascorbic acid, anhydrous calcium chloride and deionized water into a reaction kettle, adding a sodium hydroxide solution, and adding sodium trimetaphosphate to obtain calcium ascorbate; (2) adding the calcium ascorbate into a barrel, washing with water, and regulating the pH value with sulfuric acid to obtain ascorbate phosphate; (3) filtering the ascorbate phosphate through a microtubule-type dynamic membrane; (4) adding the filtrate into a reaction kettle, dropwisely adding a sodium hydroxide solution to regulate the pH value while controlling the reaction temperature and time, thereby obtaining the sodium ascorbyl phosphate; (5) filtering the sodium ascorbyl phosphate through a roll-type nanofiltration membrane filter; and (6) filtering the sodium ascorbyl phosphate through activated carbon, adding 95% ethanol, and carrying out spray drying to obtain the sodium ascorbyl phosphate finished product. The method does not use any organic solvent, and has the advantages of simple technique, short reaction time, environmental safety, high product purity and high stability.

Description

Technical field [0001] The present invention relates to the field of preparation of vitamin C derivatives, specifically a preparation method of sodium vitamin C phosphate. Background technique [0002] Sodium Vitamin C Phosphate is a vitamin C derivative. Derivating the 2-position hydroxyl group into a phosphate ester can improve the stability of vitamin C. The formed derivative can regenerate vitamin C after being hydrolyzed by phosphatase that is widely present in the body. Therefore, it has become the main component of feed additives, food fortifiers and high-end cosmetics whitening, and is a valuable fine chemical. [0003] So far, there are two main methods for esterification of L-ascorbic acid-2-phosphate: one is phosphorylation of phosphorus oxychloride (such as those described in European patents 388869 and 582924, U.S. patent 4179445, Japanese patent No. 60-69079, etc. ), using vitamin C as raw material, protect the hydroxyl groups on the 5th and 6th carbons before...

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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