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Preparation method of 3-mercaptopropionic acid

A technology of mercaptopropionic acid and sodium acrylate, which is applied in the fields of mercaptan preparation, thioether preparation, organic chemistry, etc., can solve the problems of difficult acquisition of 3-chloropropionic acid, difficult treatment of waste water or waste liquid, and high equipment requirements, and achieves high yield The efficiency and cracking efficiency are improved, the yield and purity are improved, and the effect of high purity

Active Publication Date: 2019-10-25
HEBEI HOFMANN NEW MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But these methods usually have the following problems: the raw materials used are poisonous or difficult to obtain, such as acrylonitrile is highly toxic, and 3-chloropropionic acid is difficult to obtain; the reaction requires high equipment, such as acrylic acid is corrosive to high-pressure vessels; waste water Or waste liquid is difficult to handle, etc.

Method used

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  • Preparation method of 3-mercaptopropionic acid
  • Preparation method of 3-mercaptopropionic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0054] Add 1mol sodium acrylate and 0.8mol sodium sulfide to a 500mL four-necked bottle, add water and stir to dissolve, react at 50°C for 1h, and the reaction pressure is 0.2MPa;

[0055] Add 0.6mol of sodium sulfide and 0.02mol of sulfur powder, raise the temperature to 100°C, and the reaction pressure is 0.2MPa, and continue to react for 1h;

[0056] After the reaction is completed, cool, crystallize, add 1mol sulfuric acid to the crystals after suction filtration, and acidify the crystals. The acidification temperature is 60°C, and the acidification time is 1.5h to obtain a solution of 3-mercaptopropionic acid; After washing the crystals, dry them to obtain sodium sulfate crystals, which can be used as industrial products;

[0057] Add chlorobenzene to the solution of the obtained 3-mercaptopropionic acid for extraction, reclaim the organic phase, and carry out vacuum distillation to the organic phase; the former fraction is the reclaimed solvent which can be extracted and...

Embodiment 2

[0060] Add 1mol sodium acrylate and 0.2mol sodium hydrosulfide to a 500mL four-necked flask, add water and stir to dissolve, react at 50°C for 1 hour, and the reaction pressure is 0.15MPa;

[0061] Add 1.2mol of sodium sulfide and 0.01mol of sulfur powder, raise the temperature to 110°C, and the reaction pressure is 0.15MPa, and continue to react for 1h;

[0062] After the reaction is completed, cool and crystallize, add 1 mol of sulfuric acid to the crystals for acidification after suction filtration, the acidification temperature is 60°C, and the acidification time is 1h to obtain a solution of 3-mercaptopropionic acid;

[0063] Add toluene to the solution of the obtained 3-mercaptopropionic acid for extraction, reclaim the organic phase, and carry out vacuum distillation to the organic phase to obtain a colorless liquid, i.e. 3-mercaptopropionic acid; its purity is 99.5%, and its refractive index is 1.492; its infrared spectrum is shown in figure 1 , you can know by compa...

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Abstract

The embodiment of the invention relates to the field of synthesis of sulfhydryl compounds, in particular to a preparation method of 3-mercaptopropionic acid. The preparation method includes the stepsthat sodium acrylate and sodium bisulfide or sodium sulfide are mixed and have a reaction; the sodium sulfide is added (or the sodium sulfide and powdered sulfur are added), and the reaction is continued; crystallization and acidification by adding acid are conducted, and a 3-mercaptopropionic acid solution is obtained. According to the preparation method, the costs of raw materials are low, the yield of the 3-mercaptopropionic is high, the purity of the 3-mercaptopropionic is high, solid waste and a solvent can be separated and recycled, a sodium salt is used as an industrial product after crystallization, the solvent is distilled, recycled and reused, and three wastes are easy to process.

Description

technical field [0001] The invention relates to the field of synthesis of mercapto compounds, in particular to a preparation method of 3-mercaptopropionic acid. Background technique [0002] 3-mercaptopropionic acid is an important chemical raw material and intermediate, which can be used in medicine, additives and catalysts. It is an intermediate of the medicine Fennarol (Clomezadone); it can be used as a stabilizing agent for polyvinyl chloride; it can be used as a curing agent in the field of coatings; it can be used to prepare polycarboxylate water reducers. [0003] At present, the preparation process routes of 3-mercaptopropionic acid at home and abroad mainly include the following: acrylonitrile-sodium hydrosulfide or sodium thiosulfate method; acrylonitrile-thiourea method; acrylic acid-hydrogen sulfide method; 3-chloropropionic acid- Sodium thiosulfate method, etc. But these methods usually have the following problems: the raw materials used are poisonous or diffi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/06C07C319/14C07C323/52
CPCC07C319/06C07C319/14C07C323/52C07B2200/13C07C319/28
Inventor 王新夫张小博杨遵华夏媛媛
Owner HEBEI HOFMANN NEW MATERIAL TECH CO LTD
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