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Synthetic method of perchloromethyl mercaptan

A technique for the synthesis of perchloromethanethiol and its synthesis method, which is applied in the synthesis of organic chemical raw material perchloromethylmercaptan, and in the field of synthesis of perchloromethylmercaptan, which can solve the problem of affecting personal health during operation, potential safety hazards of carbon disulfide, and increased production costs and other issues to achieve the effect of low cost, short response time and high safety

Active Publication Date: 2020-08-25
SHANDONG YANGGU HUATAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Now, the synthesis process of perchloromethanethiol generally adopts the method of passing chlorine gas into carbon disulfide, which has the problems of long reaction time, low product yield, carbon disulfide and chlorine gas can escape from the system during the reaction, and carbon disulfide There are certain safety hazards in the escape of chlorine gas. The escape of chlorine gas requires an exhaust gas absorption device, and at the same time it has a large odor, which affects the health of the operator and increases the production cost.

Method used

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  • Synthetic method of perchloromethyl mercaptan

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Add 154.10g of chloroform and 124.39g of triethylamine into a 1L reaction kettle, control the temperature at 10°C, start stirring, and slowly add 126.58g of sulfur dichloride into the system dropwise. After about 2 hours, sulfur dichloride drops After the addition is complete, keep stirring at this temperature for about 2h, and the reaction is complete. Suction filter the obtained reaction solution to remove the by-product triethylamine hydrochloride, then add about 100g of water for washing to remove a small amount of unreacted triethylamine, then raise the temperature of the collected lower layer to 65°C, and evaporate a small amount of Unreacted chloroform finally obtained 210.6g of yellow oily liquid, namely perchloromethanethiol, with a yield of 92.21% based on sulfur dichloride and a density of 1.69 after detection.

[0025] Use perchloromethanethiol as the raw material to carry out the synthesis experiment of anti-scorch agent E. The specific method is: control t...

Embodiment 2

[0027] Add 151g of chloroform and 116.34g of triethylamine into a 1L reaction kettle, control the temperature at 10°C, start stirring, slowly add 118.39g of sulfur dichloride into the system, and after about 2 hours, add sulfur dichloride dropwise Complete, keep the temperature and continue to stir for about 2h, the reaction is complete. Suction filter the obtained reaction solution to remove the by-product triethylamine hydrochloride, then add about 100g of water for washing to remove a small amount of unreacted triethylamine, then raise the temperature of the collected lower layer to 65°C, and evaporate a small amount of Unreacted chloroform finally obtained 199.2 g of yellow oily liquid, namely perchloromethanethiol, with a yield of 93.25% based on sulfur dichloride and a density of 1.69 after detection, meeting the requirements for use.

Embodiment 3

[0029] Add 167.28g of chloroform and 118.15g of triethylamine into a 1L reaction kettle, control the temperature at 0°C, start stirring, and slowly add 120.23g of sulfur dichloride into the system dropwise. After about 1 hour, sulfur dichloride drops After the addition was completed, the temperature was maintained and stirring was continued for about 1 h, and the reaction was completed. Suction filter the obtained reaction solution to remove the by-product triethylamine hydrochloride, then add about 100g of water for washing to remove a small amount of unreacted triethylamine, then raise the temperature of the collected lower layer to 65°C, and evaporate a small amount of Unreacted chloroform finally obtained 195.78g of yellow oily liquid, namely perchloromethanethiol, with a yield of 90.24% based on sulfur dichloride and a density of 1.69 after detection, meeting the requirements for use.

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Abstract

The invention discloses a synthetic method of perchloromethyl mercaptan. According to the synthetic method, trichloromethane and sulfur dichloride are used as reaction raw materials, and organic alkali is used as a catalyst and an acid-binding agent to prepare the perchloromethyl mercaptan. The method has the advantages of simple operation, strong operability, avoidance of the use of carbon disulfide and chlorine, effective solving of potential safety hazards caused by the use of carbon disulfide and chlorine and high safety; and the obtained perchloromethyl mercaptan appears to be yellow oilyliquid, has yield of 85% or above and density of 1.69 or above, meets use requirements, and presents industrial application value.

Description

technical field [0001] The present invention relates to a method for synthesizing perchloromethanemercaptan, an organic chemical raw material, in particular to a method for synthesizing perchloromethanemercaptan with simple and safe production process, less waste water, environmental protection and high product yield, which belongs to organic synthesis technology field. Background technique [0002] Perchloromethanethiol is an important chemical raw material for pesticide fungicides such as captan, folpet, and terendazim. In addition, perchloromethylmercaptan is also the key synthesis of anti-scorch agent V.E (also known as anti-scorch agent E) for rubber raw material. Anti-scorch agent V.E is a special anti-scorch agent developed by German Bayer company for light-colored rubber vulcanization. This product does not pollute, does not color, and does not foam when mixed at high temperature. Vulcanization system with Lamb type accelerators. Rubber is currently widely used in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/02C07C323/03
CPCC07C319/02C07C323/03
Inventor 王庆振吕寻伟马松马德龙
Owner SHANDONG YANGGU HUATAI CHEM
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