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Method for preparing 3, 5-dichloroaniline by means of catalytic hydrogenation

A technology for catalytic hydrogenation and dichloroaniline, which is applied in the preparation of amino compounds, chemical instruments and methods, preparation of organic compounds, etc., to achieve the effects of low recovery cost, reduced separation process, and reduced corrosion

Pending Publication Date: 2018-12-18
JIANGXI HEYI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The object of the present invention is aimed at the shortcoming of above-mentioned process method, and a kind of that proposes is to use 3,5-dichloronitrobenzene solution body as raw material, take Pt / c as catalyst hydrogenation reduction to prepare 3,5-dichloroaniline method, which can effectively solve the problems existing in the existing restoration process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043]With 400g3,5-dichloronitrobenzene and 6g1%Pt / c (water content is 66.67%) catalyzer joins in the 1L stainless steel autoclave, airtight autoclave, replaces the air in the autoclave with nitrogen three times, then with Hydrogen replaced the nitrogen in the kettle three times and kept a certain pressure in the kettle. Raise the temperature to 80°C under stirring, maintain the reaction pressure at 1.05Mpa, and keep the temperature at 90°C. After reacting for 100 minutes, close the hydrogen valve, release the pressure after cooling, and replace with nitrogen. The conversion rate of 3,5-dichloronitrobenzene is 100%, the selectivity of 3,5-dichloroaniline is 99.6%, and the dechlorination rate is 0.2%.

Embodiment 2

[0046] Increase the reaction temperature to investigate the effect of temperature on the hydrogenation reduction of 3,5-dichloronitrobenzene.

[0047] With 400g3,5-dichloronitrobenzene and 6g1%Pt / c (water content is 66.67%) catalyzer joins in the 1L stainless steel autoclave, airtight autoclave, replaces the air in the autoclave with nitrogen three times, then with Hydrogen replaced the nitrogen in the kettle three times and kept a certain pressure in the kettle. Raise the temperature to 80°C under stirring, maintain the reaction pressure at 1.05Mpa, and keep the constant temperature at 100°C. After reacting for 80 minutes, close the hydrogen valve, release the pressure after cooling, and replace with nitrogen. The conversion rate of 3,5-dichloronitrobenzene is 100%, the selectivity of 3,5-dichloroaniline is 99.5%, and the dechlorination rate is 0.22%.

Embodiment 3

[0049] Increase the reaction temperature to investigate the effect of temperature on the hydrogenation reduction of 3,5-dichloronitrobenzene.

[0050] With 400g3,5-dichloronitrobenzene and 6g1%Pt / c (water content is 66.67%) catalyzer joins in the 1L stainless steel autoclave, airtight autoclave, replaces the air in the autoclave with nitrogen three times, then with Hydrogen replaced the nitrogen in the kettle three times and kept a certain pressure in the kettle. Heat up to 80°C under stirring, maintain the reaction pressure at 1.05Mpa, and keep the constant temperature at 110°C. After reacting for 60 minutes, close the hydrogen valve, vent the gas after cooling, and replace with nitrogen. , the conversion rate of 5-dichloronitrobenzene is 100%, the selectivity of 3,4-dichloroaniline is 99.3%, and the dechlorination rate is 0.25%.

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PUM

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Abstract

The invention discloses a method for preparing 3, 5-dichloroaniline by means of catalytic hydrogenation. According to the method, 3, 5-dichloronitrobenzene is used as a raw material, and the 3, 5-dichloroaniline is prepared by taking the 3, 5-dichloronitrobenzene as body and carrying out a catalytic hydrogenation reduction reaction under the conditions of 0.8-1.2MPa and 90-120 DEG C in presence ofa Pt / c catalyst. The method uses the Pt / c catalyst, thus effectively solving the problems of hydrogenolysis and dechlorination in a hydrogenation reduction process of the 3, 5-dichloronitrobenzene; the dechlorination rate does not exceed 0.25%, so that the corrosion, caused by dechlorination, of reaction equipment is reduced, and equipment maintenance and care costs are lowered; the Pt / c catalystis simple in components, low in recovery costs, stable in activity, high in selectivity and long in continuous application time. In addition, the method does not use a dechlorination inhibitor, so that the separation process of the dechlorination inhibitor is omitted, and the influence of the dechlorination inhibitor on the quality of the finished product is fundamentally eliminated.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a method for preparing 3,5-dichloroaniline by catalytic hydrogenation. Background technique [0002] 3,5-Dichloroaniline is an important pesticide and dye intermediate, which is used as a raw material for agricultural pesticides, and it can be used to prepare sclerotin, sclerotin, iprodione and sclerotin; It can also be used to synthesize herbicides and plant growth regulators. The pharmaceutical industry is used to manufacture quinoline derivatives for the treatment of malaria. The dye industry is used in the manufacture of azo dyes and pigments. In industrial hygiene for the manufacture of insecticides and pest repellents. There are usually three production methods: iron powder reduction method, sodium persulfide reduction method and catalytic hydrogenation reduction method to reduce 3,5-dichloronitrobenzene to 3,5-dichloroaniline. [0003] Due to serious environment...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/36C07C211/52
CPCC07C209/365C07C211/52Y02P20/584
Inventor 高金平候云飞柴明根吴勇廖勇
Owner JIANGXI HEYI CHEM
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