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A method for preparing high-purity sodium vc-2-monophosphate and the high-purity sodium vc-2-monophosphate product prepared therefrom

A technology of sodium monophosphate and monophosphate, which is applied in the field of vitamin C derivatives preparation, and can solve the problems of low ratio of Vc-2-monophosphate, high-cost technology for separating impurities, and difficult environmental protection treatment.

Active Publication Date: 2018-05-04
DSM JIANGSHAN PHARMACEUTICAL (JIANGSU) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there have been many patents for the product of Vc-2-monophosphate, but most of the products obtained from the patents have a relatively low ratio of Vc-2-monophosphate, or the process requires the use of environmentally-friendly treatment that is difficult additives, or the production of this product requires special equipment to meet the process conditions, or the high-cost technology of chromatographic separation is required for the separation and purification of impurities

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] The esterification reaction was carried out in a 2000 ml beaker. The beaker was placed in a constant temperature water bath with stirring. First, 560 ml of purified water was added to the beaker, and then 1112 g of crystalline Vc-Na was added after starting to stir. Stir evenly for later use; prepare 216 g of calcium hydroxide 33% water suspension, stir well and set aside. Weigh 520 g of sodium trimetaphosphate, slowly add it to the beaker, and slowly add calcium hydroxide, while raising the temperature of the reaction system to 45 ° C, the speed of adding sodium trimetaphosphate is first fast and then slow, and add 2 / 3 of the first half hour , add the remaining part one hour later, and gradually increase the temperature of the reaction system to 60°C, add calcium hydroxide 33% aqueous suspension to control the pH of the reaction system at 9.0-10.5, and continue the reaction for three hours after the addition of calcium hydroxide , to end the reaction, to obtain the fin...

Embodiment 2

[0047] The esterification reaction is carried out in a 2000ml beaker. The beaker is placed in a constant temperature water bath with stirring. First add 560ml of purified water to the beaker, then start stirring and then add 1132g of crystallized Vc-Na, stir well and set aside; prepare 216g of calcium hydroxide 33% water suspension liquid, stir well and set aside. Weigh 520g of sodium trimetaphosphate, slowly add it to the beaker, and slowly add calcium hydroxide, while raising the temperature of the reaction system to 45°C, the speed of adding sodium trimetaphosphate is first fast and then slow, add 2 / 3 in the first half hour, Add the remaining part one hour later, and at the same time gradually increase the temperature of the reaction system to 60°C, add calcium hydroxide 33% aqueous suspension to control the pH of the reaction system at 9.0-10.5, and continue the reaction for three hours after the calcium hydroxide is added. Finish the reaction to obtain the end solution of...

Embodiment 3

[0050] The esterification reaction is carried out in a 2000ml beaker. The beaker is placed in a constant temperature water bath with stirring. First add 560ml of purified water to the beaker, then start stirring and then add 1162g of crystallized Vc-Na, stir well and set aside; prepare 216g of calcium hydroxide 33% water suspension liquid, stir well and set aside. Weigh 520g of sodium trimetaphosphate, slowly add it to the beaker, and slowly add calcium hydroxide, while raising the temperature of the reaction system to 45°C, the speed of adding sodium trimetaphosphate is first fast and then slow, add 2 / 3 in the first half hour, Add the remaining part one hour later, and at the same time gradually increase the temperature of the reaction system to 60°C, add calcium hydroxide 33% aqueous suspension to control the pH of the reaction system at 9.0-10.5, and continue the reaction for three hours after the calcium hydroxide is added. Finish the reaction to obtain the end solution of...

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Abstract

The invention relates to a highly pure Vc-2-sodium monophosphate preparation method and a highly pure Vc-2-sodium monophosphate product prepared through the method. The method comprises the following steps: carrying out an esterification reaction on an excess amount of sodium ascorbate and sodium trimetaphosphate (a molar ratio of sodium ascorbate to phosphate groups of sodium trimetaphosphate is 1.1-1.15:1) at a controlled reaction temperature under a calcium hydroxide controlled reaction system pH value to obtain a high-Vc-2-monophosphate, low-Vc-2-diphosphate and Vc-2-triphosphate esterification liquid; and allowing the esterification liquid to go through strong acid cation resin to remove metal ions, neutralizing the obtained liquid by using a concentrated sodium hydroxide solution to obtain an aqueous solution with high-sodium Vc-2-monophosphate, concentrating the aqueous solution, carrying out methanol precipitation, carrying out mother liquor separation, and re-crystallizing the obtained material to obtain the finished sodium Vc-2-monophosphate with the purity of 97-99.5%.

Description

technical field [0001] The present invention relates to the field of preparation of vitamin C derivatives. Specifically, the present invention is a preparation method of sodium Vc-2-monophosphate. The invention adopts excess vitamin C salt to react with metaphosphate, and prepares high-purity vitamin C-2-sodium monophosphate product through ion exchange, precipitation, dissolution and re-precipitation. Background technique [0002] Sodium Vc-2-monophosphate is a derivative that protects the stability of the 2-position C on the carbon chain of vitamin C molecule. It was created to improve the stability of vitamin C, while also increasing its hydrophilic properties. It can slowly degrade in nature to release vitamin C. At the same time, its amorphous product has strong hygroscopicity. Therefore, it becomes a stable vitamin C enhancer, cosmetic heat preservation agent, whitening agent, and has a wide range of applications. [0003] At present, there have been many patents ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/655
CPCC07F9/65515
Inventor 黄加洪田学国袁琪曹云峰
Owner DSM JIANGSHAN PHARMACEUTICAL (JIANGSU) CO LTD
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