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New synthesis process of m-chlorobenzotrifluoride

A technology for m-chlorotrifluorotoluene and chlorotrifluorotoluene is applied in the new synthesis process field of m-chlorotrifluorotoluene, which can solve the problems of difficult separation and purification, large environmental protection pressure, generation of a large amount of waste hydrochloric acid, etc., and achieves abundant sources and high prices. The effect of low, low product cost

Active Publication Date: 2020-10-30
上海嘉化科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008]This method produces iron sludge, waste water and a large amount of waste hydrochloric acid, which has great environmental pressure
However, the content of chlorobenzotrifluoride is only 90%, because it contains 10% o-chlorobenzotrifluoride, and the subsequent separation and purification are extremely difficult.

Method used

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  • New synthesis process of m-chlorobenzotrifluoride
  • New synthesis process of m-chlorobenzotrifluoride
  • New synthesis process of m-chlorobenzotrifluoride

Examples

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Embodiment example 1

[0031] The invention provides a technical scheme: a new synthesis process of m-chlorobenzotrifluoride, comprising the following steps:

[0032] S1. Weigh each component: Weigh 300g of 3,4-dichlorobenzotrifluoride, 300g of cyclohexane, 280g of triethylamine, 280g of water, and 20g of Raney nickel in sequence, and put the above components into 2L in the autoclave;

[0033] S2. Replacement treatment: nitrogen replacement, hydrogen replacement;

[0034] S3. Temperature control: Slowly raise the temperature to 80°C, and control the temperature between 80~85°C;

[0035] S4, sampling analysis experimental data: the hydrogen pressure is 2.0MPa, after 4 hours of reaction, sampling analysis, the content is 92% for m-chlorobenzotrifluoride, 0.7% for p-chlorobenzotrifluoride, and 7.3% for benzotrifluoride, control p-Chlorotrifluorotoluene not more than 1%;

[0036] S5, static layering: static layering, the lower layer is an aqueous solution of triethylamine hydrochloride, adjusted to P...

Embodiment example 2

[0040] The invention provides a technical scheme: a new synthesis process of m-chlorobenzotrifluoride, comprising the following steps:

[0041] S1. Weigh each component: Weigh 300g of 3,4-dichlorobenzotrifluoride, 300g of ethanol, 117g of potassium hydroxide, and 10g of ruthenium carbon successively, and put the above-mentioned components into a 2L autoclave successively, wherein , the ruthenium content of ruthenium carbon 10g is 5%, and the dry weight is 40%;

[0042] S2. Replacement treatment: nitrogen replacement, hydrogen replacement;

[0043] S3. Temperature control: Slowly raise the temperature to 60°C, and keep the temperature between 60°C and 63°C;

[0044] S4, sampling analysis experimental data: the hydrogen pressure is 1.0MPa, after 4 hours of reaction, sampling analysis, the content is 94% for m-chlorobenzotrifluoride, 0.5% for p-chlorobenzotrifluoride, and 5.5% for benzotrifluoride, control p-Chlorotrifluorotoluene not more than 1%;

[0045] S5, stand and strat...

Embodiment example 3

[0049]The invention provides a technical scheme: a new synthesis process of m-chlorobenzotrifluoride, comprising the following steps:

[0050] S1. Weigh each component: Weigh 300 g of 3,4-dichlorobenzotrifluoride, 300 g of ethanol, 280 g of triethylamine, and 20 g of Raney nickel in sequence, and put the above components into a 2L autoclave in sequence;

[0051] S2. Replacement treatment: nitrogen replacement, hydrogen replacement;

[0052] S3. Temperature control: Slowly raise the temperature to 70°C, and control the temperature between 70~75°C;

[0053] S4, sampling analysis experimental data: the hydrogen pressure is 1.5MPa, after 3.5 hours of reaction, the sampling analysis shows that the content is 88% for m-chlorobenzotrifluoride, 0.8% for p-chlorobenzotrifluoride, and 11.2% for benzotrifluoride. p-Chlorotrifluorotoluene not more than 1%;

[0054] S5, standing and stratifying: standing and filtering to remove the catalyst, ethanol is obtained through desolventization, ...

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Abstract

The invention discloses a new synthesis process of m-chlorobenzotrifluoride, and relates to the technical field of synthesis of m-chlorobenzotrifluoride, in particular to the new synthesis process ofm-chlorobenzotrifluoride. The process comprises the following steps of: S1, weighing each component; S2, conducting replacement treatment; S3, performing temperature control; S4, conducting sampling and analyzing experimental data; S5, performing standing for layering; S6, conducting rectification; and S7, repeating the experiment. According to the invention, 3, 4-dichlorobenzotrifluoride is usedas a raw material, and due to the fact that trifluoromethyl has different influences on chlorine at different positions on a benzene ring, in the presence of an efficient catalyst, during hydrogenation, high selectivity can be achieved; cyclohexane, ethanol and trifluorotoluene are used as the solvent, triethylamine and potassium hydroxide are taken as the acid-binding agent, raney nickel, ruthenium carbon and palladium carbon are taken as the catalyst, hydrogen is introduced under a pressure of 0.5-2.0MPa and at a temperature of 60-100DEG C, and after hydrodechlorination, the solvent is removed, and the m-chlorobenzotrifluoride content reaches 99% or above through rectification separation and purification.

Description

technical field [0001] The invention relates to the technical field of synthesis of m-chlorobenzotrifluoride, in particular to a new synthesis process of m-chlorobenzotrifluoride. Background technique [0002] m-Chlorotrifluorotoluene is an essential intermediate for the synthesis of high-efficiency, broad-spectrum and safe agricultural fungicide flufenazole, and is also an important intermediate for the synthesis of some fluorine-containing azo dyes. The existing process uses m-aminobenzotrifluoride as a raw material, and prepares m-chlorobenzotrifluoride through diazotization and chlorination. This method has a large amount of waste water, a large amount of waste acid and waste salt, and the pressure on environmental protection is great. Trifluorotoluene is also used as raw material for direct chlorination to prepare m-chlorobenzotrifluoride. In this method, 90% m-chlorobenzotrifluoride and 10% o-chlorobenzotrifluoride are difficult to further separate, and high-purity m-...

Claims

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Application Information

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IPC IPC(8): C07C17/23C07C17/383C07C17/38C07C25/13
CPCC07C17/23C07C17/383C07C17/38C07C25/13
Inventor 于鹏吕亚成蔡杰顾晓轩
Owner 上海嘉化科技有限公司
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