Novel synthesis method of chlorobenzotrifluoride

A technology of chlorinated benzotrifluoride and a synthetic method, which is applied in the field of preparation of pesticide chemical intermediate products, can solve the problems of low absorption utilization rate of chlorine gas, low reaction yield and other problems, and achieve convenient post-processing recovery, convenient operation, and reduction of The effect of pollutant emissions

Inactive Publication Date: 2020-01-07
JIANGSU FENGHUA CHEM IND
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  • Abstract
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  • Claims
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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 o-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%

Method used

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  • Novel synthesis method of chlorobenzotrifluoride

Examples

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Embodiment 1

[0024] (1) Chlorination step: put 630g of o-chlorotoluene into a dehydration kettle, heat to 80°C to remove water, and obtain 629g of o-chlorotoluene, put it into a 3L chlorination reaction kettle, heat up to 110°C, add 31.5g of chlorinated ethylene Copper catalyst (added in 4 batches, each batch 8-10g), start to pass dry chlorine gas, flow 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 o-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.

[0025] (2) Fluorination step: Press 4 moles of o-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 w...

Embodiment 2

[0030] (1) Chlorination step: put 470kg of o-chlorotoluene into a dehydration kettle, heat to 80°C to remove water to obtain dry o-chlorotoluene, put it into a 3000L chlorination reaction kettle, raise the temperature to 110°C, add 25kg of chlorinated Copper catalyst (added in 4 batches, each batch 6-7kg), start to pass 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 o-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.

[0031] (2) Fluorination step: pump 690kg of o-chlorotrichlorotoluene into the high level tank for metering and put it into the fluorination kettle, open the frozen brine system, and press 250kg of anhydrous hydrogen fluoride i...

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Abstract

The invention discloses a novel synthesis method of chlorobenzotrifluoride, wherein o-chlorotoluene is used as a raw material, copper chloride or cuprous chloride is used as a catalyst, and o-chlorobenzotrifluoride is synthesized through two steps of chlorination and fluorination. Compared with the method in the prior art, the method of the invention has the following characteristics that raw materials are subjected to heating dehydration treatment in the dehydration kettle, so that the chlorination side reactions are few, the product purity is high, the graded chlorination device does not need to be additionally arranged, the technological process is simple, and the operation is convenient. According to the chlorination process of the invention, the catalyst is added in batches to increase the efficiency of the catalyst, so that the by-product generated by thechlorination reaction and the emission of waste gas in the production are 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 o-chlorobenzotrifluoride. This method is applicable to the occasion of synthesizing o-chlorobenzotrifluoride through two steps of chlorination and fluorination by using o-chlorotoluene as raw material. Background technique [0002] O-Chlorotrifluorotoluene is a colorless transparent liquid at room temperature with the smell of halogenated benzene. The compound is insoluble in water, but miscible with benzene, toluene, ethanol, ether, halogenated hydrocarbons, etc. O-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, pesticides, and dyes. O-chlorotrifluorotoluene is used in the synthesis of fine organic chemical products such as medicines and pesticides, and it is...

Claims

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Application Information

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