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Method for preparing D-sodium pantothenate from D-calcium pantothenate mother liquor

A technology of calcium pantothenate and sodium pantothenate, which is applied in the chemical industry, can solve the problems of increased types of mixed solvents, troubles in the recovery of mixed solutions, cumbersome steps, etc., and achieve the effects of recyclable solvents, reduced costs and procedures, and simple steps

Inactive Publication Date: 2021-02-05
安徽泰格生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Regarding the synthesis of D-sodium pantothenate, most of them buy finished D-calcium pantothenate to prepare D-sodium pantothenate. The steps are cumbersome, and the final crystallization rate of D-sodium pantothenate is below 50%. Some patent documents mention the use of ethanol With acetone mixed solvent, the crystallization yield can reach 90%, but the recovery of the mixed solution will also cause troubles in the later stage, and acetone is a relatively dangerous solvent, and the increase in the types of mixed solvents also leads to increased costs, not to mention from the realization of industrialization After security considerations, it is also unwise to

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The present embodiment provides a kind of method for preparing D-sodium pantothenate by D-calcium pantothenate mother liquor, specifically:

[0023] Take 1000g D-calcium pantothenate mother liquor, reflux and concentrate at 50°C in vacuum, recover methanol until there is no liquid reflux in the condenser, add 150g water, continue atmospheric distillation to 100°C, add 11.5g sodium carbonate, and keep warm at 80°C-90°C for one After adding dilute sulfuric acid to the filtrate to adjust the pH to 6.96, add 0.5g of activated carbon, stir for 30 minutes and filter, then concentrate under reduced pressure at 66°C to the remaining feed liquid 60g (water content 5.5%), add 180g of 95% methanol and stir evenly Then continue to cool down, then slowly cool down to 10°C and then filter, and vacuum-dry the filtered crystals at 40-45°C to obtain 36 g of D-sodium pantothenate as a dry product with a purity of 99.3%.

Embodiment 2

[0025] The present embodiment provides a kind of method for preparing D-sodium pantothenate by D-calcium pantothenate mother liquor, specifically:

[0026] Take 1000g D-calcium pantothenate mother liquor, reflux and concentrate at 50°C in vacuum, recover methanol until there is no liquid reflux in the condenser, add 160g water, continue atmospheric distillation to 100°C, add 12.2g sodium carbonate, and keep warm at 80°C-90°C for one After adding dilute sulfuric acid to the filtrate to adjust the pH to 7.1, add 0.5g of activated carbon, stir for 30 minutes and filter, then concentrate under reduced pressure at 63°C to the remaining feed liquid 63g (water content 8.3%), add 210g of methanol and stir evenly and continue Cool down, then slowly cool down to 20°C and filter, and vacuum-dry the filtered crystals at 40°C to obtain 33 g of D-sodium pantothenate as a dry product with a purity of 99.6%.

Embodiment 3

[0028] The present embodiment provides a kind of method for preparing D-sodium pantothenate by D-calcium pantothenate mother liquor, specifically:

[0029] Take 1000g D-calcium pantothenate mother liquor, reflux and concentrate at 50°C in vacuum, recover methanol until there is no liquid reflux in the condenser, add 146g water, continue atmospheric distillation to 100°C, add 11.5g sodium carbonate, and keep warm at 80°C-90°C for one After adding dilute sulfuric acid to the filtrate to adjust the pH to 7.06, add 0.5g of activated carbon, stir for 30 minutes and filter, then concentrate under reduced pressure at 65°C to the remaining feed liquid 65g (water content 10.0%), add 230g of methanol and stir evenly before continuing Cool down, then slowly cool down to 11°C and then filter. The filtered crystals are vacuum-dried at 40°C to obtain 39 g of dry sodium D-pantothenate with a purity of 99.0%.

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Abstract

The invention discloses a method for preparing sodium D-pantothenate from calcium D-pantothenate mother liquor. The method comprises the following steps: carrying out reflux concentration on the calcium pantothenate mother liquor, adding water, stirring, adding sodium carbonate, reacting, filtering, adding dilute sulfuric acid into the filtrate to regulate the pH value, adding activated carbon, filtering, concentrating the filtrate, adding methanol, cooling, crystallizing, filtering, and drying to obtain sodium D-pantothenate. According to the invention, 10%-20% of calcium D-pantothenate stillremains in the crystallization mother liquor of calcium D-pantothenate to prepare sodium pantothenate. A solvent used in the reaction is low in price, a mother solution needing to be recycled is usedas a raw material to prepare a new product, the cost has huge advantages, the reaction is environmentally friendly, the safety is high, the reaction time is short, the solvent can be recycled, the steps are simple, and the purity of the obtained sodium D-pantothenate product is high.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a method for preparing sodium D-pantothenate from a mother liquor of calcium D-pantothenate. Background technique [0002] Sodium pantothenate, the English name is D-Pantothenic Acid Sodium Salt, alias D-pantothenic sodium, the chemical name is (R)-N-(2,4-dihydroxy-3,3-dimethyl-1-oxobutyl )-beta-alanine monosodium salt, which is the sodium salt form of pantothenic acid. Pantothenic acid, also known as pantothenic acid and vitamin B3, is a kind of vitamin B family. It can help cells form, maintain normal development and the development of the central nervous system, and maintain the normal function of the adrenal gland. It is indispensable when fat and sugar are converted into energy. It is also an essential substance for antibody synthesis and human body's utilization of aminobenzoic acid and choline. There are two forms of pantothenic acid, calcium salt and sodium ...

Claims

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Application Information

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IPC IPC(8): C07C231/12C07C231/24C07C235/12
CPCC07C231/12C07C231/24
Inventor 周多祥段小瑞宋以航徐帝汪洪湖
Owner 安徽泰格生物科技有限公司
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