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Synthesis method of 3-mercaptopropionic acid

A technology of mercaptopropionic acid and its synthesis method, which is applied in the direction of organic chemistry, can solve the problems of large production investment and high equipment requirements, and achieve the effects of good environmental protection, high safety, and mild operating conditions

Active Publication Date: 2017-12-22
SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method requires an autoclave as a reaction vessel, which requires high equipment and large production investment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Pass acrylic acid with a content of 99.5% into the gasification chamber, control the temperature of the gasification chamber at 200°C, and pass hydrogen sulfide and vaporized acrylic acid into a mixer at a temperature of 220°C in a molar ratio of 8:1 well mixed;

[0033] (2), fill 30ml of 8wt% zinc oxide / alumina catalyst in a dielectric barrier plasma reactor, control the reaction temperature at 220°C and feed the mixed gas, turn on the power, adjust the input power of the power supply to 35W, and stabilize the plasma reactor Work;

[0034] (3) Set the flow rate of the mixed gas at 40ml / min and feed it into the reactor. Under the synergistic action of the plasma and the catalyst, the mixed gas stays for 25s to complete the reaction and collect the product at the outlet of the reactor.

[0035] The reaction product was rectified under reduced pressure to obtain 3-mercaptopropionic acid; the calculated yield was 80.12%, and the product purity was 99.1%.

Embodiment 2

[0037] (1) Pass acrylic acid with a content of 99.0% into the gasification chamber, control the temperature of the gasification chamber at 220°C, and pass hydrogen sulfide and vaporized acrylic acid into a mixer at a temperature of 240°C in a molar ratio of 8:1 well mixed;

[0038] (2), 4wt% magnesia / silicon dioxide catalyst 30ml are filled in the radio frequency discharge plasma reactor, control reaction temperature 240 ℃ and feed mixed gas, turn on the power supply, adjust the power supply input power 55W, make the plasma reactor stable job;

[0039] (3) Set the flow rate of the mixed gas to 60ml / min and feed it into the reactor. Under the synergistic action of the plasma and the catalyst, the mixed gas stays for 21s to complete the reaction and collect the product at the outlet of the reactor.

[0040] The reaction product was rectified under reduced pressure to obtain 3-mercaptopropionic acid; the calculated yield was: 79.68%, and the product purity was 99.3%.

Embodiment 3

[0042] (1) Pass acrylic acid with a content of 99.5% into the gasification chamber, control the temperature of the gasification chamber at 240°C, and pass hydrogen sulfide and vaporized acrylic acid into a mixer at a temperature of 250°C in a molar ratio of 10:1 well mixed;

[0043] (2) Fill 30ml of 12wt% zirconia / molecular sieve catalyst in a dielectric barrier plasma reactor, control the reaction temperature to 250°C and feed the mixed gas, turn on the power, adjust the input power of the power supply to 70W, and make the plasma reactor work stably ;

[0044] (3) Set the flow rate of the mixed gas to 80ml / min and feed it into the reactor. Under the synergistic action of the plasma and the catalyst, the mixed gas has a residence time of 18s, completes the reaction, and collects the product at the outlet of the reactor.

[0045] The reaction product was rectified under reduced pressure to obtain 3-mercaptopropionic acid; the calculated yield was 78.09%, and the product purity...

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PUM

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Abstract

The invention belongs to the field of synthesis of sulfhydryl compounds and in particular relates to a synthesis method of 3-mercaptopropionic acid. The method comprises the following steps: (1) adding acrylic acid into a gasification chamber according to a pre-set flow; introducing hydrogen sulfide and acrylic acid into a mixer according to a certain mol ratio and uniformly mixing; (2) starting a plasma reactor filled with a catalyst and introducing mixed gas into the plasma reactor to react; controlling reaction temperature and pressure; (3) after reaction is finished, cooling and rectifying to obtain the 3-mercaptopropionic acid. The method provided by the invention can be used for effectively synthesizing the 3-mercaptopropionic acid; a whole synthesis process is carried out under -0.05MPa to 0.1MPa; a technology is simple and can realize continuous operation. An experiment result shows that the average yield of the method provided by the invention on the 3-mercaptopropionic acid is 78.77 percent.

Description

technical field [0001] The invention belongs to the field of synthesizing mercapto compounds, in particular to a method for synthesizing 3-mercaptopropionic acid. Background technique [0002] 3-Mercaptopropionic acid is an important chemical raw material, and its main application fields are medicine, auxiliaries and water reducing agents. It can be used to prepare the medicine Fennarol (Clomezadone), which has the effect of sleeping and calming; it can be used to prepare pentaerythritol tetrakis (3-mercaptopropionic acid) ester, which is an intermediate used in organic synthesis, as a curing The agent can be used in the field of coatings; it can be used to prepare polycarboxylic acid-based high-efficiency water reducers, and to synthesize heat stabilizers such as organic tin and organic antimony. At present, its main process route at home and abroad is to use acrylonitrile and sodium hydrosulfide as raw materials for production. This process can be carried out under normal...

Claims

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Application Information

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IPC IPC(8): C07C321/04C07C323/52
CPCC07C321/04C07C323/52
Inventor 吴玉强马韵升杨姗易先君郭龙龙张建林韩立霞
Owner SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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