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New process for synthesizing 3,4,5-trichlorobenzotrifluoride

A technology of trichlorotrifluorotoluene and dichlorotrifluorotoluene is applied in the field of new synthesis process of 3,4,5-trichlorotrifluorotoluene, which can solve the problem that the dual benefits of environment and economy cannot be satisfied, the target compound has no use value, Harsh process conditions and other problems, to achieve significant social benefits, low prices, and significant economic benefits

Inactive Publication Date: 2020-01-07
JIANGSU FENGHUA CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The above-mentioned methods have high reaction temperature, long time, harsh process conditions, and complicated steps, and the raw material 4-chloro-3,5-dinitrobenzotrifluoride used in the reaction uses sulfuric acid and nitric acid in large quantities as raw materials, which is corrosive to equipment. Large, polluting and harmful to the environment
Can not meet the dual benefits of environment and economy
In addition, 3,4-dichlorobenzotrifluoride is produced from p-chlorobenzotrifluoride, and the by-product is 3,4,5-trichlorobenzotrifluoride, but the general content is about 1.5%. For the target compound no use value

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Chlorination: Put 800g of p-chlorobenzotrifluoride into a 3L reaction kettle, raise the temperature to 95°C, add 40g of catalyst, and pass in a flow rate of 40-80 m 3 / h of dry chlorine, after 4 hours of reaction, the temperature was increased to 110°C, and chlorine was continued for 20 hours to the end of the reaction. Introduce dry air to discharge unreacted chlorine gas, hydrogen chloride gas and gas impurities generated in the reaction kettle to obtain a mixture of 3,4-dichlorobenzotrifluoride and 3,4,5-trichlorobenzotrifluoride;

[0030] (2) Rectification: Under the condition of reflux ratio of 5:2, the mixture obtained in the first step is rectified from 3,4-dichlorobenzotrifluoride to form a refined product containing 3,4,5-trichlorobenzotrifluoride Distill the residue, then repeat the rectification, collect the distillate with a gas phase temperature of 199-202°C at the top of the tower, and obtain the target compound after condensation. Generally, the firs...

Embodiment 2

[0033] (1) Chlorination: Put 800g of p-chlorobenzotrifluoride into a 3L reaction kettle, raise the temperature to 95°C, add 80g of catalyst, and pass in a flow rate of 40-80 m 3 After 4 hours of reaction, the temperature was increased to 115° C., and chlorine was continued for 16 hours to the end of the reaction. Introduce dry air to discharge unreacted chlorine gas, hydrogen chloride gas and gas impurities generated in the reaction kettle to obtain a mixture of 3,4-dichlorobenzotrifluoride and 3,4,5-trifluorobenzotrichloride;

[0034] (2) Rectification: Under the condition of reflux ratio of 3:1, after the mixture obtained in the first step is rectified from 3,4-dichlorobenzotrifluoride, a refined product containing 3,4,5-trichlorobenzotrifluoride is formed. Distill the residue, then repeat the rectification, collect the distillate with a gas phase temperature of 199-202°C at the top of the tower, and obtain the target compound after condensation. Generally, the first rectif...

Embodiment 3

[0037] (1) Chlorination: Put 800g of p-chlorobenzotrifluoride into a 3L reaction kettle, raise the temperature to 95°C, add 60g of catalyst, and pass in a flow rate of 40-80 m 3 / h of dry chlorine gas, control the temperature at 110-115°C, and continue to pass chlorine for 18 hours until the end of the reaction. Introduce dry air to discharge unreacted chlorine gas, hydrogen chloride gas and gas impurities generated in the reaction kettle to obtain a mixture of 3,4-dichlorobenzotrifluoride and 3,4,5-trifluorobenzotrichloride;

[0038] (2) Rectification: Under the condition of reflux ratio of 3:1, after the mixture obtained in the first step is rectified from 3,4-dichlorobenzotrifluoride, a refined product containing 3,4,5-trichlorobenzotrifluoride is formed. Distill the residue, then repeat the rectification, collect the distillate with a gas phase temperature of 199-202°C at the top of the tower, and obtain the target compound after condensation. Generally, the first rectifi...

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Abstract

The invention discloses a new process for synthesizing 3,4,5-trichlorobenzotrifluoride, wherein p-chlorobenzotrifluoride is used as a raw material, andchlorination, rectification and neutralization are performed to obtain the 3,4,5-trichlorobenzotrifluoride. Compared with the method in the prior art, the method of the invention has the following characteristics that the used raw materials avoid alarge amount of sulfuric acid and nitric acid, so that the corrosion to equipment is small, the pollution is greatly reduced, and the harm to the environment is reduced; the used raw material p-chlorobenzotrifluoride is wide in source and low in price, so that the production cost of the target compound can be reduced, and the economic benefit is improved; and by adjusting the reaction conditions,the content of the 3,4,5-trichlorobenzotrifluoride achieves 8-10%, and the 3,4-dichlorobenzotrifluoride is separated from the 3,4,5-trichlorobenzotrifluoride by rectification, such that the operationis simple and convenient.

Description

technical field [0001] The invention relates to a preparation method of pesticide chemical products, in particular to a new synthesis process of 3,4,5-trichlorobenzotrifluoride. This method is applicable to the occasion that 3,4,5-trichlorobenzotrifluoride is obtained through several steps of chlorination, rectification and neutralization by using p-chlorobenzotrifluoride as raw material. Background technique [0002] 3,4,5-Trichlorobenzotrifluoride is a colorless oily liquid. The boiling point is 200-202°C, the flash point is 98°C, the relative density is 1.600, and the refractive index is 1.5000. Fluorine-containing aromatic compounds are important intermediates of physiologically active compounds such as medicines and pesticides. Due to the small volume of fluorine atoms, large electronegativity, high electron cloud density, and the introduction of fluorine atoms or fluorine-containing groups, the compound has good thermal stability, anti-oxidation, enhanced efficacy, l...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/12C07C17/383C07C25/13
CPCC07C17/12C07C17/383C07C25/13
Inventor 郑龙生方东张亮李付香
Owner JIANGSU FENGHUA CHEM IND
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