Production process of p-trifluoromethyl aniline

A technology of trifluoromethylaniline and p-chlorotrifluorotoluene is applied in the production field of p-trifluoromethylaniline, and can solve the problems of low single-pass conversion rate, large pollution and the like

Active Publication Date: 2007-11-21
江苏优普生物化学科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The existing production method of p-trifluoromethylaniline has a low conversion rate per pass, generally only within 40%, and the pollution is large

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] A kind of production method of p-trifluoromethylaniline: p-chlorobenzotrifluoride and liquefied ammonia are reacted in an autoclave in the presence of alcohol and catalyst, and the consumption of p-chlorobenzotrifluoride, liquid ammonia, alcohol and catalyst They are: 950kg of p-chlorobenzotrifluoride, 450kg of liquid ammonia, 800kg of alcohol, and 80kg of catalyst. The reaction temperature is 140-150°C, the pressure is 6-7.5MPa, and the reaction time is 9-13 hours. After the reaction is over, excess liquid ammonia is absorbed into ammonia water, and industrial alcohol is flashed out at the same time, and the catalyst is removed by filtration, and the catalyst is regenerated mechanically. The obtained p-trifluoromethylaniline crude product is rectified to obtain 560 kg of finished product, and 220 kg of raw materials are recovered, and single-pass conversion The yield is 66%, and the yield is 90%. Above-mentioned catalyst is made up of following weight components:

[0...

Embodiment 2

[0020] A kind of production method of p-trifluoromethylaniline: p-chlorobenzotrifluoride and liquefied ammonia are reacted in an autoclave in the presence of alcohol and catalyst, and the consumption of p-chlorobenzotrifluoride, liquid ammonia, alcohol and catalyst They are: p-chlorobenzotrifluoride 900kg, liquid ammonia 400kg, alcohol 700kg, catalyst 70kg, the reaction temperature is 140-150°C, the pressure is 6-7.5MPa, and the reaction time is 9-13 hours. After the reaction, the excessive liquid ammonia is absorbed into ammonia water, and industrial alcohol is flashed out simultaneously, and the catalyst is removed by filtration, and the catalyst regeneration is applied mechanically. The rate is about 90%. Above-mentioned catalyst is made up of following weight components:

[0021] Ferrocene 31%

[0022] Triphenylphosphine 50%

[0023] Potassium Fluoride 12%

[0024] Tetrabutylammonium bromide 7%.

Embodiment 3

[0026] A kind of production method of p-trifluoromethylaniline: p-chlorobenzotrifluoride and liquefied ammonia are reacted in an autoclave in the presence of alcohol and catalyst, and the consumption of p-chlorobenzotrifluoride, liquid ammonia, alcohol and catalyst They are: p-chlorobenzotrifluoride 1000kg, liquid ammonia 600kg, alcohol 900kg, catalyst 90kg, the reaction temperature is 140-150°C, the pressure is 6-7.5MPa, and the reaction time is 9-13 hours. After the reaction, the excessive liquid ammonia was absorbed into ammonia water, and industrial alcohol was flashed out simultaneously, and the catalyst was removed by filtration, and the catalyst regeneration was applied mechanically. The rate is about 90%. Above-mentioned catalyst is made up of following weight components:

[0027] Ferrocene 50%

[0028] Triphenylphosphine 31%

[0029] Potassium Fluoride 17%

[0030] Tetrabutylammonium bromide 2%.

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PUM

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Abstract

The present invention discloses the production process of p-trifluoromethyl aniline. P-trifluorotoluene and liquid ammonia are reacted in the presence of alcohol and catalyst to obtain p-trifluoromethyl aniline. The catalyst may consist of ferrocene, triphenyl phosphor, potassium fluoride, ammonium tetrabutyl bromide. The present invention has high efficient composite catalyst used, single pass conversion rate up to 66 % and yield up to 90 %. The organic solvent may be used circularly, the excessive liquid ammonia may be prepared into ammonia water, the catalyst may be regenerated and reused, and the process has no waste water exhausted.

Description

Technical field: [0001] The present invention relates to a kind of production method of p-trifluoromethylaniline. Background technique: [0002] In the existing production method of p-trifluoromethylaniline, the conversion rate per pass is low, generally only within 40%, and the pollution is large. Invention content: [0003] The object of the present invention is to provide a kind of single pass conversion rate height, the production method of the high p-trifluoromethylaniline of yield. [0004] Technical solution of the present invention is: [0005] P-chlorobenzotrifluoride and liquid ammonia are reacted to obtain p-trifluoromethylaniline in the presence of alcohol and a catalyzer, wherein the catalyzer is composed of the following weight components: [0006] Ferrocene 30~50% [0007] Triphenylphosphorus 30~50% [0008] Potassium fluoride 10-30% [0009] Tetrabutylammonium bromide 2-7%. [0010] The consumption ratio of p-chlorobenzotrifluoride, liquid ammonia, al...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/10C07C211/46B01J31/24B01J31/22
CPCY02P20/584
Inventor 李巍陶坤山徐国军秦建军于海军
Owner 江苏优普生物化学科技股份有限公司
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