Synthesis method for bis (2-mercaptoethyl) sulfide

A technology of dimercaptoethyl sulfide and its synthetic method, which is applied in the fields of sulfide preparation and organic chemistry, can solve the problems of low product purity, high processing cost, and large amount of three wastes, and achieve high product purity and environmental protection. The effect of being friendly and reducing the amount of three wastes

Active Publication Date: 2012-07-04
INSIGHT FINECHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But these methods have the following defects: the product purity is not high, the total yield is low, the amount of three wastes is difficult to handle and the cost is high

Method used

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  • Synthesis method for bis (2-mercaptoethyl) sulfide
  • Synthesis method for bis (2-mercaptoethyl) sulfide
  • Synthesis method for bis (2-mercaptoethyl) sulfide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Synthesis of isosulfuronium salts

[0023] In a 2L four-necked flask, add 334.4g (4.4mol) thiourea and 573.6g (4.4mol, 28%) industrial hydrochloric acid, when the temperature rises to 32 DEG C, the solid dissolves completely, and the heating is stopped, and 244.0g (2.0 mol) of thiodiethylene glycol, after the dropwise addition, add 25g of zinc chloride to the system, slowly raise the temperature to 90-100°C (about 40min), keep the temperature for 4 hours, stop heating, and cool the reaction solution to 30- 35°C, directly used in subsequent reactions.

[0024] Synthesis of Bismercaptosulfide

[0025] Add 17.3g of tetrabutylammonium bromide to the above-mentioned isosulfuronium salt solution, stir and mix well, add 740g of diammonium hydrogen phosphate / ammonium phosphate buffer solution (pH=11.0) dropwise, and finish dropping in about 30 minutes, pay attention to control the reaction The pH value of the system is ~10, and the temperature is raised to 60-65°C, and the re...

Embodiment 2

[0027] Synthesis of isosulfuronium salts

[0028] Add 334.4g (4.4mol) thiourea and 573.6g (4.4mol, 28%) industrial hydrochloric acid in a 2L four-necked flask, when the temperature rises to 32°C, the solid dissolves completely, stop heating, and add 244.0g (2.0mol) dropwise within 20min ) of thiodiethylene glycol, after the dropwise addition, 30g of ferric chloride was added to the system, the temperature was slowly raised to 90-100°C (about 40min), and the temperature was kept for 7.5 hours, then the heating was stopped, and the temperature of the reaction solution was lowered to 30-35 °C, used directly in subsequent reactions.

[0029] Synthesis of Dimercaptosulfide (DMDS)

[0030] Add 17.3g of tetrabutylammonium bromide to the above-mentioned isosulfuronium salt solution, stir and mix well, add 740g of diammonium hydrogen phosphate / ammonium phosphate buffer solution (pH=11.0) dropwise, and finish dropping in about 30 minutes, pay attention to control the reaction The pH o...

Embodiment 3

[0032] Synthesis of isosulfuronium salts

[0033] Add 334.4g (4.4mol) thiourea and 573.6g (4.4mol, 28%) industrial hydrochloric acid in a 2L four-necked flask, when the temperature rises to 32°C, the solid dissolves completely, stop heating, and add 244.0g (2.0mol) dropwise within 20min ) of thiodiethylene glycol, after the dropwise addition, add 30g of zinc chloride to the system, slowly raise the temperature to 70-80°C (about 25min), keep the temperature for 8h, stop heating, and cool the reaction solution to 30-35°C , used directly in subsequent reactions.

[0034] Synthesis of Dimercaptosulfide (DMDS)

[0035] Add 17.3g tetrabutylammonium bromide to the solution of above-mentioned isosulfuronium salt, stir and mix, dropwise add 712g ammonium carbonate aqueous solution (wt 50%), drip in about 30min, pay attention to controlling the exhaust rate in the early stage of reaction, control The pH of the reaction system is ~10, and the temperature is raised to 60-65°C, and the r...

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Abstract

The invention relates to a synthesis method and production technology for bis (2-mercaptoethyl) sulfide. The method uses thiodiglycol and thiourea as raw materials to synthesize target products after two reacting steps of substitute salifying and alkaline hydrolysis, product purity is larger than 99%, total yield of the two steps is improved to more than 98% on the basis of 80% in the existing technology. The synthesis method has the advantages of being free of rigor conditions in production, smooth and safe in operation, less in three wastes, high in product purity, low in production cost and the like and is suitable for being applied to industrial production.

Description

field of invention [0001] The present invention relates to the synthesis method and production process of important chemical raw material dimercaptoethyl sulfide. The method of the present invention uses thiodiglycol and thiourea as raw materials, and synthesizes the target product through two-step reactions of substitution into salt and alkaline hydrolysis, and the product purity is It is greater than 99%, and the two-step total yield is increased to more than 98% on the basis of 80% in the original process. The synthesis method of the invention has the characteristics of no harsh conditions for production, smooth and safe operation, less amount of three wastes, high product purity, low production cost, etc., and is suitable for industrial production. Background of the invention [0002] Dimercaptoethyl sulfide (DMDS) is a kind of organic compound with special unpleasant smell, which is often used as an intermediate product in the synthesis of other sulfur-containing organi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C321/14C07C319/20
Inventor 凌云吴清来汪泳三徐公达亓国秀殷巍
Owner INSIGHT FINECHEM
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