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Method for preparing o-chloroaniline

A technology for o-chloroaniline and o-chloronitrobenzene is applied in the field of liquid-phase catalytic hydrogenation of o-chloronitrobenzene to produce o-chloroaniline, and can solve the problems of lowering product quality, increasing production cost, serious dechlorination, etc. Low, dehydrogenation inhibition, high yield effect

Inactive Publication Date: 2008-11-26
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Increase production costs, and dechlorination is still relatively serious, reducing product quality

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] In a 100ml stainless steel high-pressure reactor, add 2g of o-chloronitrobenzene, 0.45g of Ru / C catalyst, 30ml of ethanol solution with a mass percentage of 95%, close the reactor, replace the air with nitrogen for 3 times, start stirring, and heat up to 210 ℃, reacted for 6 hours, stopped the reaction, took out the reaction solution, filtered out the catalyst, and the filtrate was analyzed by gas chromatography for the content of each component. The results showed that the conversion rate of o-chloronitrobenzene was 91.6%, and the selectivity of o-chloroaniline was 88.7%. %.

Embodiment 2

[0014] In a 100ml stainless steel high-pressure reactor, add 2g o-chloronitrobenzene, 0.45g Ru / C catalyst, 30ml mass percentage is 95% ethanol solution, close the reactor, replace the air with nitrogen for 3 times, start stirring, and heat up to 180°C , reacted for 6 hours, stopped the reaction, took out the reaction solution, filtered out the catalyst, and the filtrate was analyzed by gas chromatography for the content of each component. The results showed that the conversion rate of o-chloronitrobenzene was 26.2%, and the selectivity of o-chloroaniline was 97.4%. .

Embodiment 3

[0016] In a 100ml stainless steel high-pressure reactor, add 2g o-chloronitrobenzene, 0.45g NiB amorphous catalyst, 30ml mass percent as 95% ethanol solution, close the reactor, replace the air with nitrogen for 3 times, start stirring, and heat up to 210 DEG C, reacted for 6 hours, stopped the reaction, took out the reaction solution, filtered out the catalyst, and the filtrate was analyzed by gas chromatography for the content of each component. The results showed that the conversion rate of o-chloronitrobenzene was 22.1%, and the selectivity of o-chloroaniline was 89.7%.

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Abstract

A process for preparing O-chlorophenylamine from O-chloronitrobenzene features that under existance of alcohol and the catalyst chosen from Ru / C, non-crystalline NiB, Ni-Fe-B and Ni-Co-B, the O-chloronitrobenzene takes part in catalytic hydrogenation reaction at 150-250 deg.C and then is post-treated to obtain said product. It has high output rate.

Description

(1) Technical field [0001] The invention relates to a preparation method of o-chloroaniline, in particular to a method for preparing o-chloroaniline by liquid-phase catalytic hydrogenation of o-chloronitrobenzene. (2) Background technology [0002] O-Chloroaniline is an important chemical intermediate of medicine, pesticide, dyestuff, fragrance, etc., and has a wide range of uses. The synthesis methods of o-chloroaniline usually include iron powder reduction method, alkali sulfide reduction method and catalytic hydrogenation method. The first two synthesis methods seriously pollute the environment. The main problem of catalytic hydrogenation method is that hydrogen must be used. Because hydrogen is Flammable gas is very dangerous in production, and it is difficult to store and transport, and most small and medium-sized enterprises have no hydrogen source, which directly affects the popularization and application of catalytic hydrogenation, an advanced production process. Th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/36C07C211/52
Inventor 严新焕李小年罗雄军孙军庆徐振元
Owner ZHEJIANG UNIV OF TECH