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Method for preparing 3-mercaptopropionic acid

A technology of mercaptopropionic acid and acrylic acid, which is applied in the field of preparation of 3-mercaptopropionic acid, can solve the problems such as difficult disposal of reactant residue and by-products, and achieves the effects of easy extraction, few by-products and high content

Inactive Publication Date: 2011-11-02
YUANPING TONGLI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to solve the problem that the reactant raffinate and by-products in the existing 3-mercaptopropionic acid preparation method are difficult to handle, and to provide a preparation method of 3-mercaptopropionic acid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Stir 1mol thiourea and 1.0mol hydrochloric acid at 40°C for 0.5 hours; add 1.1mol of acrylic acid dropwise at 60°C for 0.5 hours, maintain the reaction temperature at 80°C, and maintain the reaction time for 1 hour; add 2.1mol The reaction temperature after sodium hydroxide is 90°C, and the reaction time is 0.5 hours; add 1.2 hydrochloric acid to acidify the temperature at 20°C, and the acidification time is 0.2 hours to obtain a solution of 3-mercaptopropionic acid; finally extract with benzene and distill under reduced pressure The product 3-mercaptopropionic acid is evaporated.

Embodiment 2

[0022] Stir 1mol thiourea and 1.5mol hydrochloric acid at 90°C for 2.0 hours; add 1.5mol of acrylic acid dropwise at 90°C for 2.0 hours, maintain the reaction temperature at 90°C, and maintain the reaction time for 7 hours; add 3.0mol The reaction temperature after sodium hydroxide is 110°C, and the reaction time is 3 hours; the acidification temperature is 60°C with 1.5mol hydrochloric acid, and the acidification time is 1 hour to obtain a solution of 3-mercaptopropionic acid; finally, it is extracted with benzene and xylene , Vacuum distillation to steam out the product 3-mercaptopropionic acid.

Embodiment 3

[0024] 1mol thiourea and 1.2mol hydrochloric acid were stirred at 70°C for 1.2 hours; 1.3mol of acrylic acid was added dropwise at a temperature of 75°C for 1.5 hours, and the reaction temperature was maintained at 85°C for 4 hours; 2.5mol The reaction temperature after sodium hydroxide is 100°C, and the reaction time is 1.5 hours; the acidification temperature after adding 1.3mol hydrochloric acid is 20-60°C, and the acidification time is 0.6 hours to obtain a solution of 3-mercaptopropionic acid; finally, use ethyl acetate Extraction, vacuum distillation to steam out the product 3-mercaptopropionic acid.

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Abstract

The invention discloses a method for preparing 3-mercaptopropionic acid, comprising the following steps of: (1), after mixing thiourea and hydrochloric acid, stirring; (2), dropping acrylic acid; keeping temperature at 80-90 degrees centigrade; and keeping the reaction for 1-7 h; (3), adding sodium hydroxide solution; hydrolyzing; generating sulphur sodium propionate and urea; and (4), acidizing by adding hydrochloric acid; preparing solution containing 3-mercaptopropionic acid; and, after extracting through an organic solvent, decompressing and distilling to obtain the 3-mercaptopropionic acid. Reaction liquid contains a few by-products. The extraction process is easily carried out. The product is good in colour and high in content. After being extracted, waste liquid can be separated and recycled by simply distilling and filtering. Residual liquid can be added to new waste liquid to be further treated. The zero emission of the three wastes (waste gas, waste water and industrial residue) can be basically realized.

Description

technical field [0001] The invention relates to a method for preparing 3-mercaptopropionic acid, in particular to a method for preparing 3-mercaptopropionic acid with acrylic acid. Background technique [0002] 3-Mercaptopropionic acid is an intermediate of pharmaceutical fennarol, and it is also used as a stabilizer of polyvinyl chloride, antioxidant, catalyst and biochemical reagent. There are three main methods for synthesizing 3-mercaptopropionic acid: acrylonitrile-thiourea method, acrylonitrile-sodium hydrosulfide or sodium thiosulfate method, acrylic acid-hydrogen sulfide high-pressure synthesis method. [0003] The acrylonitrile-thiourea method is to stir and react thiourea and hydrochloric acid, then cool, add acrylonitrile dropwise, and keep warm at 100-115°C for 3 hours. Then cool to below 40°C, add liquid sodium hydroxide dropwise, and reheat to 100-115°C to react for 4 hours. After exhausting ammonia and cooling, acidify with hydrochloric acid to obtain an aqu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/52C07C319/12C07C275/00C07C273/02
Inventor 薄宪明贺芬霞张婧
Owner YUANPING TONGLI CHEM
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