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Preparation method of disulfide compound 3,3'-dithiodipropionic acid

A technology of dithiodipropionic acid and compounds, which is applied in the field of preparation of disulfide compound 3,3'-dithiodipropionic acid, can solve the problems of high production cost, low product yield, complicated process, etc. Achieve the effects of less environmental pollution, lower production costs, and guaranteed purity

Inactive Publication Date: 2015-11-25
SHANXI QIYOU BUILDING MATERIALS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem mainly solved by the present invention is to overcome the problems of complex process, serious personal injury and environmental pollution, low product yield and high production cost in the above preparation method, and provide a safe, green, environmentally friendly, simple process and low cost. The preparation method of disulfide compound 3,3'-dithiodipropionic acid, its structure is as follows:

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A preparation method of disulfide compound 3,3'-dithiodipropionic acid, comprising the following steps:

[0027] a) Dissolve 48.1g-70% sodium hydrosulfide in 43.5g of water. At 35°C, add 31g of acrylonitrile dropwise into the aqueous solution of sodium hydrosulfide for 1 hour. Keep warm at 35°C for 2 hours. After the heat preservation is over, add 125g -30% hydrochloric acid for acidification, after adjusting the pH value of the reaction solution to below 2.0, use lye 30% sodium hydroxide solution under negative pressure to carry out secondary absorption of hydrogen sulfide produced during acidification; then use 50g toluene Extracted twice, combined the organic phases, concentrated under reduced pressure, and distilled the raffinate under reduced pressure at 45~48°C / 3torr to obtain compound I, whose structural formula is as follows:

[0028] HSCH 2 CH 2 CN

[0029] The content of compound I was detected by gas chromatography, and the content was 98.5%.

[0030] b) ...

Embodiment 2

[0037] A preparation method of disulfide compound 3,3'-dithiodipropionic acid, comprising the following steps:

[0038] a) Dissolve 48.1g-70% sodium hydrosulfide in 43.5g of water. At 40°C, add 31g of acrylonitrile dropwise into the aqueous solution of sodium hydrosulfide for 1 hour, keep warm at 40°C for 2 hours, and add 125g after the heat preservation is completed. -30% hydrochloric acid for acidification, after adjusting the pH value of the reaction solution to below 2.0, use 30% sodium hydroxide solution under negative pressure to carry out secondary absorption of hydrogen sulfide generated during acidification. Then extract twice with 50g-30% hydrochloric acid, combine the organic phases, concentrate under reduced pressure, and distill the raffinate under reduced pressure at 45~48°C / 3torr to obtain compound I, whose structural formula is as follows:

[0039] HSCH 2 CH 2 CN

[0040] The content of compound I was detected by gas chromatography, and the content was 99.3%...

Embodiment 3

[0048] A kind of disulfide compound 3, the preparation method of 3'-dithiodipropionic acid comprises the following steps:

[0049] a) Dissolve 60.8g-70% sodium hydrosulfide in 43.5g of water. At 40°C, add 31g of acrylonitrile dropwise into the aqueous solution of sodium hydrosulfide for 1 hour, keep warm at 40°C for 2 hours, and add 142g after the heat preservation is completed. -30% hydrochloric acid for acidification, after adjusting the pH value of the reaction solution to below 2.0, use 30% sodium hydroxide solution under negative pressure to carry out secondary absorption of hydrogen sulfide generated during acidification. Then extract twice with 50 g of toluene, combine the organic phases, concentrate under reduced pressure, and distill the raffinate under reduced pressure at 45~48°C / 3torr to obtain compound I, whose structural formula is as follows:

[0050] HSCH 2 CH 2 CN

[0051] The content of compound I was detected by gas chromatography, and the content was 95.8...

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Abstract

A preparation method of a disulfide compound 3,3'-dithiodipropionic acid comprises the steps of: subjecting the raw materials of sodium hydrosulfide, acrylonitrile, iodine solution and acid to Michael addition, acidification, oxidation and hydrolysis; and recrystallizing and purifying to obtain the disulfide compound 3,3'-dithiodipropionic acid. Compared with the prior art, the method has the beneficial effects of safety, simpleness, green, environment-friendliness, simple technology, high yield and low production costs.

Description

technical field [0001] The invention relates to a preparation method of a disulfide compound 3,3'-dithiodipropionic acid. Background technique [0002] The disulfide compound 3,3'-dithiodipropionic acid is an important intermediate for the preparation of 3,3'-dithiodipropionic acid dimethyl ester, 3,3'-dithiodipropionic acid dimethyl ester It is an intermediate in the synthesis of isothiazolone industrial antifungal agents, and can also be used as a nickel plating brightener and a metal surface cleaner. [0003] Patent US20120040418A1 introduced a method to prepare 2-cyanoethanethiol from sodium hydrosulfide, acrylonitrile, sulfuric acid and chloroform; The crude product is purified by chromatography; finally, the preparation method of disulfide compound 3,3'-dithiodipropionic acid is obtained by hydrolyzing with cyanohydrolase. In this preparation method, the acidifying agent is sulfuric acid, and a large amount of sodium sulfate is generated in the reaction process. Beca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/52C07C319/22
Inventor 刘秀君吴林茂赵乐
Owner SHANXI QIYOU BUILDING MATERIALS TECH CO LTD
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