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Method for continuously synthesizing perchloromethyl mercaptan by using reaction tower

A technology of perchloromethane mercaptan and reaction tower, which is applied in mercaptan preparation, organic chemistry and other directions, can solve the problems of back-mixing and by-products, low raw material utilization rate and production efficiency, low safety, etc., so as to improve reaction safety. Controllability and controllability, improve the low utilization rate of raw materials, and improve the effect of production efficiency

Active Publication Date: 2021-10-08
内蒙古立威生物科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The invention provides a method for continuously synthesizing perchloromethanethiol by using a reaction tower, which is used to solve the problems of back-mixing and by-products in a single-pot full-mixing reaction, low raw material utilization rate and production efficiency, and low safety; continuous Production can reduce production equipment, improve reaction conversion rate and selectivity, improve raw material utilization, thereby improve production efficiency and output, reduce production costs, and improve production safety

Method used

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  • Method for continuously synthesizing perchloromethyl mercaptan by using reaction tower
  • Method for continuously synthesizing perchloromethyl mercaptan by using reaction tower
  • Method for continuously synthesizing perchloromethyl mercaptan by using reaction tower

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Embodiment 1

[0047] Utilize the method for continuous synthesis of perchloromethanethiol in reaction tower, may further comprise the steps:

[0048] 1) Put carbon disulfide and water with a mass ratio of 1:1.05 into the blending kettle in proportion, after stirring and mixing, cool down to 10°C; the amount of material in the blending kettle is 82.5wt% of the total amount of carbon disulfide and water;

[0049] 2) Mix the remaining carbon disulfide and water evenly at a mass ratio of 1:1.05. After cooling down to 10°C, send the mixed solution to the mixing tank at the bottom of the reaction tower, and use a quantitative pump to feed the mixed solution at a rate of 0.8 L / min. The material flow rate is pumped into the feed inlet of the first layer of the reaction tower, the mixed liquid is dispersed through the distributor, and then chlorine gas is introduced at a flow rate of 5L / min, and the temperature in the reaction tower is controlled not to exceed 35°C, and the reacted reaction liquid is...

Embodiment 2

[0057] Utilize the method for continuous synthesis of perchloromethanethiol in reaction tower, may further comprise the steps:

[0058] 1) put carbon disulfide and water with a mass ratio of 1:1.1 into the blending kettle in proportion, after stirring and mixing, cool down to 10°C; the amount of material in the blending kettle is 85wt% of the total amount of carbon disulfide and water;

[0059] 2) Mix the remaining carbon disulfide and water evenly at a mass ratio of 1:1.1. After cooling down to 10°C, send the mixed solution to the mixing tank at the bottom of the reaction tower, and use a quantitative pump to feed the mixed solution at a rate of 1.0L / min. The material flow rate is pumped into the feed inlet of the first layer of the reaction tower, the mixed liquid is dispersed through the distributor, and then chlorine gas is introduced at a flow rate of 6L / min, and the temperature in the reaction tower is controlled not to exceed 35°C. After the reaction, the reaction liquid...

Embodiment 3

[0067] Utilize the method for continuous synthesis of perchloromethanethiol in reaction tower, may further comprise the steps:

[0068] 1) Put carbon disulfide and water with a mass ratio of 1:1 into the blending kettle in proportion, after stirring and mixing, cool down to 10°C; the amount of material in the blending kettle is 80wt% of the total amount of carbon disulfide and water;

[0069] 2) Mix the remaining carbon disulfide and water evenly at a mass ratio of 1:1. After cooling down to 10°C, send the mixed solution to the mixing tank at the bottom of the reaction tower, and use a quantitative pump to feed the mixed solution at a rate of 1.2L / min. The material flow rate is pumped into the feed inlet of the first layer of the reaction tower, the mixed liquid is dispersed through the distributor, and then chlorine gas is introduced at a flow rate of 7L / min, and the temperature in the reaction tower is controlled not to exceed 35°C. The reacted reaction liquid is sent into th...

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Abstract

The invention provides a method for continuously synthesizing perchloromethyl mercaptan by using a reaction tower, which comprises the following steps of: preparing a mixed solution from carbon disulfide and water, and continuously feeding the mixed solution and chlorine into a reaction tower respectively for reaction to synthesize the perchloromethyl mercaptan. The reaction tower is a three-layer feeding tower type reactor. The reaction temperature in the reaction tower is not higher than 35 DEG C. The method provided by the invention can solve the problems of many backmixing and byproducts, low raw material utilization rate, low production efficiency and low safety of single-kettle complete mixing reaction. The continuous production can reduce production equipment, improve the reaction conversion rate and selectivity and improve the utilization rate of raw materials, so that the production efficiency and yield are improved, the production cost is reduced, and the production safety is also improved. Reaction byproducts can be sold as industrial products after being absorbed and recovered, and the comprehensive utilization value of the raw materials is improved.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for continuously synthesizing perchloromethanethiol using a reaction tower. Background technique [0002] Perchloromethanethiol, foreign name Perchloromethyl Mercaptan, CAS No. 594-42-3, molecular formula CCl 3 SCl, molecular weight 185. This product is an important intermediate in organic synthesis such as synthetic dyes and pesticides. For example: perchloromethanethiol is synthesized with 1,2,3,6-tetrahydrophthalimide and phthalimide respectively, and the pesticide fungicides captan and folpet can be prepared, and at the same time It is also an important intermediate in the synthesis of cloxazone. Although this type of pesticide is old, its annual sales volume in the international market is tens of thousands of tons, which is difficult to be replaced by modern new agricultural fungicides. For this reason, it is urgent to develop the intermediate of this ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C381/00C07C319/02C07C323/03
CPCC07C381/00C07C319/02C07C323/03
Inventor 毛志建何小虎郭时贵曾关景
Owner 内蒙古立威生物科技有限公司
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