P-chlorobenzotrifluoride synthesizing method

A technology of p-chlorobenzotrifluoride and p-chlorobenzotrichloride, which is applied in the field of preparation of pesticide chemical intermediate products, can solve the problems of low absorption and utilization rate of chlorine gas, low reaction yield, etc., and achieve remarkable economic and social benefits , easy operation, reduction of by-products and exhaust emissions

Inactive Publication Date: 2014-05-14
JIANGSU DAHUA CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] (1) In the chlorination reaction process, due to failure to strictly control the occurrence of side reactions, the p-chlorobenzotrifluoride content can only reach about 90% in the chlorination reaction, and the reaction yield is low;
[0005] (2) This synthesis process is in the chlorination production process, owing to adopting is the single kettle chlorination form, in the chlorination process, the absorption utilization rate of chlorine is too low, only about 75%
This method needs to increase the raw material processing device, and the graded chlorination device

Method used

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  • P-chlorobenzotrifluoride synthesizing method
  • P-chlorobenzotrifluoride synthesizing method

Examples

Experimental program
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Effect test

Embodiment 1

[0029] (1) Chlorination: 630g p-chlorotoluene is put into dehydration kettle, after being heated to 80 ℃ to remove moisture content, obtain 629g p-chlorobenzotrifluoride, put into 3L chlorination reaction kettle, heat up to 110 ℃, add 40g catalyst (minutes) Add 4 batches, each batch 10g), start to feed dry chlorine gas, the flow rate is 40-80m 3 / h, then add the catalyst every 30 minutes, control the temperature at 110-112°C, and the reaction time is 24 hours. After sampling and analyzing the chlorinated material as qualified, stop the chlorine flow. The p-chlorotrichlorotoluene produced by chlorination is pumped into the chlorination tank for use, and the tail gas generated by the reaction is sent to the tail gas absorption device.

[0030] (2) Fluorination: Press 4 moles of p-chlorotrichlorotoluene and 12 moles of anhydrous hydrogen fluoride into a 3L fluorination reaction kettle, open the frozen brine system, press hydrogen fluoride into the fluorination kettle with 0.2MPa...

Embodiment 2

[0034] (1) Chlorination: 630g p-chlorotoluene is put into dehydration kettle, after being heated to 80 ℃ to remove moisture content, obtain 629g p-chlorobenzotrifluoride, put into 3L chlorination reactor, heat up to 110 ℃, add 80g catalyst (minutes) Add in 4 batches, each batch is 20g), and start to feed dry chlorine gas with a flow rate of 40-80m 3 / h, then add the catalyst every 30 minutes, control the temperature at 110-112°C, and the reaction time is 20 hours. After sampling and analyzing the chlorinated material as qualified, stop the chlorine flow. The p-chlorotrichlorotoluene produced by chlorination is pumped into the chlorination tank for use, and the tail gas generated by the reaction is sent to the tail gas absorption device.

[0035] (2) Fluorination: Press 4 moles of p-chlorotrichlorotoluene and 14 moles of anhydrous hydrogen fluoride into a 3L fluorination reaction kettle, open the frozen brine system, press hydrogen fluoride into the fluorination kettle with 0....

Embodiment 3

[0039] (1) Chlorination: 630g p-chlorotoluene is put into dehydration kettle, is heated to 80 ℃ to remove moisture content and obtains 629g p-chlorobenzotrifluoride, puts into 3L chlorination reaction kettle, heats up to 110 ℃, adds 60g catalyst (minutes) Add in 4 batches, each batch is 15g), and start to feed dry chlorine gas with a flow rate of 40-80m 3 / h, then add the catalyst every 30 minutes, control the temperature at 110-112°C, and the reaction time is 22 hours. After sampling and analyzing the chlorinated material as qualified, stop the chlorine flow. The p-chlorotrichlorotoluene produced by chlorination is pumped into the chlorination tank for use, and the tail gas generated by the reaction is sent to the tail gas absorption device.

[0040] (2) Fluorination: Press 4 moles of p-chlorotrichlorotoluene and 13 moles of anhydrous hydrogen fluoride into a 3L fluorination reaction kettle, open the frozen brine system, press hydrogen fluoride into the fluorination kettle w...

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Abstract

The invention discloses a p-chlorobenzotrifluoride synthesizing method. P-chlorotoluene is used as a raw material, and p-chlorobenzotrifluoride is synthesized through chlorination and fluorination. Compared with the prior art, in the method, a dehydration kettle is used for performing thermal dehydration processing on the raw material, side reactions of chlorination are few, the product is high in purity, no grading chlorination device needs to be added, and the technological process is simple and convenient to operate; according to the method, in the chlorination process, the mode that catalysts are added in batches is adopted, so that the use efficiency of the catalysts is improved, therefore, emission of by-products and exhaust gas generated by chlorination in production is reduced significantly, and therefore emission of pollutants in the production process is reduced.

Description

a technical field [0001] The invention relates to a method for preparing a pesticide chemical intermediate product, in particular to a method for synthesizing p-chlorobenzotrifluoride. This method is applicable to the occasion of synthesizing p-chlorobenzotrifluoride through two steps of chlorination and fluorination by using p-chlorotoluene as raw material. Two background technology [0002] 4-Chlorobenzotrifluorotoluene (4-chlorobenzotrifluoride) is a colorless transparent liquid with an odor of halogenated benzene. The compound is insoluble in water, but miscible with benzene, toluene, ethanol, ether, halogenated hydrocarbons, etc. p-Chlorotrifluorotoluene is an important intermediate in organic synthesis, and the fluorine atom it contains endows it with special activity. It is widely used in fine organic synthesis fields such as medicine, pesticide, and dyestuff. p-Chlorobenzotrifluoride is a key intermediate in the synthesis of various fluorine-containing insecticides...

Claims

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Application Information

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IPC IPC(8): C07C25/13C07C17/20
Inventor 郑龙洲方东李付香
Owner JIANGSU DAHUA CHEM IND
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