A kind of method that solvent-free catalytic hydrogenation prepares o-chloroaniline

A technology for catalytic hydrogenation and o-chloroaniline, which is applied in the preparation of amino compounds, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of increased production costs, low catalyst selectivity, etc., and achieves cost savings and is conducive to industrialization. Promotion and application, the effect of low cost recovery

Active Publication Date: 2016-01-20
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of CN102050746A and CN101774931A are that the selectivity of the catalyst is not high, and a dechlorination inhibitor needs to be added, which increases the production cost. At the same time, there are problems of dechlorination inhibitor treatment and alcohol solvent recovery
The disadvantage is that it needs to add a variety of additives to inhibit dechlorination, which increases the production cost, and there are problems in the treatment of dechlorination inhibitors and the recovery of alcohol solvents

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 60g o-nitrochlorobenzene and 0.36g3%Pt / C (59.98% water content) catalyst into a 100ml stainless steel autoclave, seal the autoclave, replace the air in the autoclave with nitrogen three times, and then replace it with hydrogen Nitrogen in the kettle for three times and maintain a certain pressure in the kettle. Under stirring, heat up to 95°C, maintain the reaction pressure of 2.25MPa, and react for 120 minutes. After the reaction is over, close the hydrogen valve, let the gas out after cooling, and open the autoclave to discharge the material. Filter out the catalyst. The filtrate is analyzed by high performance liquid chromatography. The conversion rate of benzene is 100%, the selectivity of o-chloroaniline is 99.3%, and the dechlorination rate is 0.09%.

Embodiment 2

[0026] Add 60g of o-nitrochlorobenzene and 0.36g of 1%Pt / C (59.78% water content) catalyst into a 100ml stainless steel autoclave, seal the autoclave, replace the air in the autoclave with nitrogen three times, and then replace it with hydrogen Nitrogen in the kettle for three times and maintain a certain pressure in the kettle. Under stirring, heat up to 95°C, maintain the reaction pressure of 2.25MPa, and react for 120 minutes. After the reaction is over, close the hydrogen valve, let the gas out after cooling, and open the autoclave to discharge the material. Filter out the catalyst. The filtrate is analyzed by high performance liquid chromatography. The conversion rate of benzene is 96%, the selectivity of o-chloroaniline is 99.5%, and the dechlorination rate is 0.06%.

Embodiment 3

[0028] Add 60g of o-nitrochlorobenzene and 0.36g of 5%Pt / C (60.12% water content) catalyst into a 100ml stainless steel autoclave, seal the autoclave, replace the air in the autoclave with nitrogen three times, and then replace it with hydrogen Nitrogen in the kettle for three times and maintain a certain pressure in the kettle. Under stirring, heat up to 95°C, maintain the reaction pressure of 2.25MPa, and react for 120 minutes. After the reaction is over, close the hydrogen valve, let the gas out after cooling, and open the autoclave to discharge the material. Filter out the catalyst. The filtrate is analyzed by high performance liquid chromatography. The conversion rate of benzene is 100%, the selectivity of o-chloroaniline is 98.9%, and the dechlorination rate is 0.39%.

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Abstract

The invention belongs to the technical field of fine chemicals and relates to a method for preparing o-chloroaniline by solvent-free catalytic hydrogenation of o-nitrochlorobenzene. Using o-nitrochlorobenzene as a raw material, in the presence of a catalyst, react with hydrogen at 70°C to 120°C and a pressure of 0.5MPa to 5.0MPa, and process to obtain o-chloroaniline after the reaction. The method of the present invention does not add a solvent, overcomes the defect of adding a solvent, avoids the problems of solvent pollution to the environment and solvent recovery, reduces equipment investment, and reduces production costs. The method of the present invention can make ortho-nitrochlorinated benzene The conversion rate reaches 100%, the selectivity of o-chloroaniline is greater than 99.2%, and the dechlorination rate is less than 0.09%.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and relates to a new preparation method of o-chloroaniline, in particular to a method for preparing o-chloroaniline by solvent-free catalytic hydrogenation of o-nitrochlorinated benzene. Background technique [0002] O-Chloroaniline is an important intermediate in the industries of pesticides, medicines, spices, dyes, and polyurethane. The preparation of o-chloroaniline in industrial production uses o-nitrochlorobenzene as a raw material, and undergoes a reduction reaction to obtain o-chloroaniline. Due to the serious pollution problems of the iron powder reduction method, alkali sulfide reduction method, and hydrazine hydrate reduction method, they have been eliminated. At present, the commonly used process for the production of o-chloroaniline is to use skeletal nickel as a catalyst, methanol or ethanol as a solvent, and catalytic hydrogenation to reduce o-chloroaniline. Nitrochlorinate...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/52C07C209/36
Inventor 吴其建杜建国周亚苓
Owner CHINA PETROLEUM & CHEM CORP
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