Method for continuously synthesizing perchloromethyl mercaptan

A technology for perchloromethane mercaptan and chloromethyl mercaptan is applied in the field of continuous synthesis of perchloromethane mercaptan, which can solve the problems of workers' health hazards, increase labor costs, reduce selectivity and the like, and achieves improved reaction safety and efficiency. Controllability, reducing the liquid chlorine gasification process, and improving the effect of reaction selectivity

Active Publication Date: 2020-06-05
NINGXIA G R FINE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This type of synthetic method mainly has the following disadvantages: (1) the reaction time is long, and it takes up to 22 hours to complete the reaction; the longer reaction time increases labor costs and reduces the output per unit time
(2) The product perchlorine and chlorine will further undergo series side reactions. Using a tank reactor, back mixing will cause an increase in series side reactions and reduce selectivity
(3) Most of the synthesis reaction devices are batch kettles, and the amount of reaction materials is large
Carbon disulfide is extremely flammable, chlorine gas is highly toxic, and has a high risk of reaction. It is easy to run,

Method used

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  • Method for continuously synthesizing perchloromethyl mercaptan
  • Method for continuously synthesizing perchloromethyl mercaptan
  • Method for continuously synthesizing perchloromethyl mercaptan

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Using liquid chlorine, carbon disulfide, and dilute hydrochloric acid (12%) as raw materials, use a high-pressure pump to pump them into the microchannel reactor under pressure, wherein the flow rate of liquid chlorine is 0.620L / h (12.5mol / h), and the flow rate of carbon disulfide is 0.150L / h (2.5mol / h), the hydrochloric acid flow rate is 0.536L / h, the reaction temperature is controlled at 15±1°C, the reaction pressure is 1Mpa, and the residence time is 1.5min. The raw materials enter the pressure storage tank after the microchannel reaction is completed, and the content of carbon disulfide in the oil phase is less than 3% after sampling and measurement, and the reaction is considered to be completed. After 1 hour of continuous production, 457.8g of the product was obtained, the content of perchloromethanethiol was 99.7%, and the yield was 98.4%, CS 2 The conversion rate is 99.4%, and the selectivity is 99.0%.

[0045] product testing:

[0046] (1) Carry out infrared ...

Embodiment 2

[0057] Using liquid chlorine, carbon disulfide, and dilute hydrochloric acid (12%) as raw materials, use a high-pressure pump to pump them into the microchannel reactor under pressure, wherein the flow rate of liquid chlorine is 0.595L / h (12.0mol / h), and the flow rate of carbon disulfide is 0.150L / h (2.5mol / h), the hydrochloric acid flow rate is 0.536L / h, the reaction temperature is controlled at 15±1°C, the reaction pressure is 1Mpa, and the residence time is 1.5min. The raw material enters the pressure storage tank after the microchannel reaction is completed, and the content of carbon disulfide in the oil phase is less than 3% after sampling and is considered as the completion of the reaction. 447.4g of the product was obtained by continuous production in one hour. According to the detection method of Example 1, the effects such as content and yield of the product were tested, and the results are shown in Table 2.

Embodiment 3

[0059] Using liquid chlorine, carbon disulfide, and dilute hydrochloric acid (12%) as raw materials, use a high-pressure pump to pump them into the microchannel reactor under pressure, wherein the flow rate of liquid chlorine is 0.657L / h (13.2mol / h), and the flow rate of carbon disulfide is 0.150L / h (2.5mol / h), the hydrochloric acid flow rate is 0.536L / h, the reaction temperature is controlled at 15±1°C, the reaction pressure is 1Mpa, and the residence time is 1.5min. The raw material enters the pressure storage tank after the microchannel reaction is completed, and the content of carbon disulfide in the oil phase is less than 3% after sampling and is considered as the completion of the reaction. 458.2 g of the product was obtained by continuous production in one hour. According to the detection method of Example 1, the effects such as content and yield of the product were tested, and the results are shown in Table 2.

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Abstract

The invention provides a method for continuously synthesizing perchloromethyl mercaptan. Liquid chlorine, carbon disulfide and a hydrochloric acid solution are adopted as raw materials and react in the continuous flow reactor under certain temperature and pressure conditions through a full-liquid-phase reaction among the materials, so that the reaction efficiency is greatly improved; meanwhile, back mixing can be effectively avoided by adopting continuous flow reaction, further reaction of total chlorine, chlorine and other byproducts is reduced, and the reaction selectivity is improved. Besides, compared with the prior art, the method has the advantages that the liquid chlorine gasification procedure is omitted, so that the problem of dissolution heat release during chlorine reaction isavoided, the total heat release in the reaction process is reduced, and the production energy consumption is reduced; moreover, high-toxicity chlorine and extremely flammable carbon disulfide need tobe used for synthesizing total chlorine, while the continuous reactor is used in the invention, so that the material amount in a reaction system can be greatly reduced, the reaction safety and controllability are improved, and the harm to the health of workers or other dangers caused by running, emitting, dripping, leaking and the like can be effectively avoided.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for continuously synthesizing perchloromethanethiol. Background technique [0002] Perchloromethanethiol is an intermediate in organic synthesis of synthetic dyes and pesticides, such as the pesticide fungicides folpet and captan. Therefore, the synthesis of perchloromethanethiol is of great significance. [0003] At present, the synthesis method of perchloromethanethiol mostly adopts intermittent gas-liquid kettle synthesis, using carbon disulfide and hydrochloric acid as raw materials, passing chlorine gas at a temperature of 10-30°C for a period of time to complete the reaction, and then separating liquids to obtain perchloromethanethiol. For example, in the Chinese patent application with the publication number CN103360295A, two reactors are used, carbon disulfide and hydrochloric acid are added to the two reactors, and then chlorine is synthesized, and pe...

Claims

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Application Information

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IPC IPC(8): C07C319/02C07C323/03
CPCC07C319/02C07C323/03
Inventor 李涛张学举高技峰张恒李江王进步杨海鹏陈淑娇
Owner NINGXIA G R FINE CHEM CO LTD
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