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Synthesis method of 4-chlorobenzotrifluoride

A technology of chlorotrifluorotoluene and a synthesis method, applied in chemical instruments and methods, organic chemistry, halogenated hydrocarbon preparation, etc., can solve the problems of low absorption utilization rate of chlorine gas, low reaction yield and the like, and achieve economic benefits and social benefits. Significant benefits, easy operation, and the effect of reducing pollutant emissions

Inactive Publication Date: 2019-11-22
JIANGSU DAHUA CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] (1) During the chlorination reaction, due to the failure to strictly control the occurrence of side reactions, the content of 4-chlorobenzotrifluoride in the chlorination reaction can only reach about 90%, and the reaction yield is low;
[0005] (2) In the chlorination production process of this synthesis process, since the single-pot chlorination form is adopted, the absorption and utilization rate of chlorine gas in the chlorination process 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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  • Synthesis method of 4-chlorobenzotrifluoride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Chlorination: put 630g of p-chlorotoluene into a dehydration kettle, heat to 80°C to remove water to obtain 629g of 4-chlorobenzotrifluoride, put it into a 3L chlorination reaction kettle, heat up to 110°C, add 40g of catalyst (minutes Add in 4 batches, each batch is 10g), and start to feed dry chlorine gas with a flow rate of 40-80 m 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 0.2M...

Embodiment 2

[0034] (1) Chlorination: put 630g of p-chlorotoluene into a dehydration kettle, heat to 80°C to remove water, and obtain 629g of 4-chlorobenzotrifluoride, put it into a 3L chlorination reaction kettle, heat up to 110°C, add 80g of catalyst (minutes Add 4 batches, each batch is 20g), start to feed dry chlorine gas, the flow rate is 40-80 m 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 0.2MPa comp...

Embodiment 3

[0039] (1) Chlorination: put 630g of p-chlorotoluene into a dehydration kettle, heat to 80°C to remove water to obtain 629g of 4-chlorobenzotrifluoride, put it into a 3L chlorination reaction kettle, heat up to 110°C, add 60g of catalyst (minutes Add in 4 batches, each batch is 15g), and start to feed dry chlorine gas with a flow rate of 40-80 m 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 with 0.2M...

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Abstract

The invention discloses a synthetic method of 4-chlorobenzotrifluoride. P-chlorotoluene is used as a raw material, and 4-chlorobenzotrifluoride is synthesized through two steps of chlorination and fluorination. Compared with the prior art, the raw materials are subjected to heating dehydration treatment in the dehydration kettle, chlorination side reactions are few, the product purity is high, a graded chlorination device does not need to be added, the technological process is simple, and operation is convenient; according to the chlorination process, a mode of adding the catalyst in batches is adopted, so that the use efficiency of the catalyst is improved, the emission of byproducts and waste gas generated by chlorination reaction in production is greatly reduced, and the emission of pollutants in the production process is reduced.

Description

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

Claims

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Application Information

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IPC IPC(8): C07C17/20C07C17/383C07C25/13
CPCC07C17/14C07C17/206C07C17/383C07C25/02C07C25/13
Inventor 郑龙洲方东张亮李付香
Owner JIANGSU DAHUA CHEM IND
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