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Refining method for recovering beta-aminopropionic acid

A kind of technology of GAPA and refining method, which is applied in the field of refining β-GAPA, which can solve the problems of low content in β-GAPA recovery process and sodium sulfate cannot be excluded, and achieve control of purification cost and recrystallization efficiency High, easy-to-operate effect

Pending Publication Date: 2020-09-15
CHIFENG PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a refining method for reclaiming β-alanine, mainly to solve the problem that the existing β-alanine recovery process has low content and cannot be eliminated by sodium sulfate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1: Throwing 65% crude β-alanine into the reactor, adding 3 times the mass of 50% aqueous methanol solution; controlling the reaction temperature at 50°C, stirring and dissolving for 25 minutes; centrifuging to remove sodium sulfate in the methanol solution , the mother liquor is concentrated under reduced pressure to distill methanol, and the remaining mass is 18% of the total input solution, and the distillation raffinate is stirred to a slurry state, cooled to about 15°C, β-alanine crystals are precipitated, and centrifuged to obtain β-alanine Wet product, dried to get β-alanine finished product. According to empirical tests, the β-alanine content is 79.4%.

Embodiment 2

[0020] Example 2: Throwing 72% crude β-alanine into the reactor, adding 5 times the mass of 52% aqueous methanol solution; controlling the reaction temperature at 45°C, stirring and dissolving for 28 minutes; centrifuging to remove sodium sulfate in the methanol solution , the mother liquor is concentrated under reduced pressure to distill methanol, and the remaining mass is 19% of the total input solution, and the distillation raffinate is stirred to a slurry state, cooled to about 25°C, β-alanine crystals are precipitated, and centrifuged to obtain β-alanine Wet product, dried to get β-alanine finished product. According to experience, the β-alanine content is 81.3%.

Embodiment 3

[0021] Example 3: Throwing 75% crude β-alanine into the reactor, adding 3.6 times the mass of 58% aqueous methanol solution; controlling the reaction temperature at 52°C, stirring and dissolving for 30 minutes; centrifuging to remove sodium sulfate in the methanol solution , the mother liquor is concentrated under reduced pressure to distill methanol, and the residual mass of the distillation raffinate, which is 20% of the total input solution, is stirred to a slurry state, cooled to about 20°C, β-alanine crystals are precipitated, and centrifuged to obtain β-alanine Wet product, dried to get β-alanine finished product. According to empirical tests, the β-alanine content is 91.7%.

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PUM

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Abstract

The invention discloses a refining method for recovering beta-aminopropionic acid. The refining method comprises the following steps: (1) dissolving: putting crude beta-aminopropionic acid into a reaction kettle, adding a 50-58% methanol aqueous solution of which the mass is 3-5 times that of the crude beta-aminopropionic acid, controlling the reaction temperature to be 45-55 DEG C, and stirring and dissolving for 25-35 minutes; (2) concentrating and crystallizing: centrifuging to remove sodium sulfate in the methanol solution, collecting the obtained mother liquor, carrying out reduced pressure concentration and distillation on methanol, stirring distillation raffinate until the distillation raffinate is pasty, cooling to 15-25 DEG C, and separating out beta-aminopropionic acid crystals;and (3) performing centrifugal drying: centrifuging to obtain a beta-aminopropionic acid wet product, and drying the beta-aminopropionic acid wet product to obtain refined beta-aminopropionic acid. The method is simple to operate, high in recrystallization efficiency and low in cost, and an efficient method is provided for purification of beta-aminopropionic acid.

Description

technical field [0001] The invention belongs to the technical field of chemical pharmacy, in particular to a refining method for recovering β-alanine. Background technique [0002] Calcium D-pantothenate (vitamin B5) is mainly used in medicine, food additives and feed additives, and is an indispensable trace substance for human and animals to maintain normal physiology. β-alanine is an important raw material for the synthesis of calcium D-pantothenate, and during the production process, the mother liquor of calcium D-pantothenate is recycled to obtain recovered β-alanine. [0003] Because sulfuric acid and sodium hydroxide are added in the recovery process of D-calcium pantothenate mother liquor, cause the crude β-alanine of recovery to contain a large amount of sodium sulfates. Therefore, it is necessary to further refine the crude β-alanine to remove sodium sulfate. Contents of the invention [0004] The purpose of the present invention is to provide a refining method ...

Claims

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Application Information

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IPC IPC(8): C07C227/40C07C229/08
CPCC07C227/40C07C229/08
Inventor 王兵王淑霞王丽敏米红杰朱庆林史宇浩
Owner CHIFENG PHARMA CO LTD