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Catalyst for preparing dichloroaniline through hydrogenization for dichloronitrobenzene, and preparation method

A technology of dichloronitrobenzene and dichloroaniline, which is applied in the preparation of amino compounds, chemical instruments and methods, catalysts for physical/chemical processes, etc., can solve the problems of few times of applying catalysts, adding dehalogenation inhibitors, and high content of precious metals , to achieve the effect of many times of application, inhibition of dechlorination phenomenon, and simple preparation process

Inactive Publication Date: 2007-10-10
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0021] Although the above-mentioned existing patented technologies have their own characteristics, they also have their own shortcomings, for example, the reaction pressure is too high, dehalogenation inhibitors need to be added, the content of precious metals is too high, and the number of times the catalyst is applied is low, etc.

Method used

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  • Catalyst for preparing dichloroaniline through hydrogenization for dichloronitrobenzene, and preparation method
  • Catalyst for preparing dichloroaniline through hydrogenization for dichloronitrobenzene, and preparation method
  • Catalyst for preparing dichloroaniline through hydrogenization for dichloronitrobenzene, and preparation method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Grind the activated carbon into powder in a ball mill, screen 80-120 mesh activated carbon in 2mol.L -1 HNO 3 Soak in water for 24 hours, then filter out the activated carbon, wash it repeatedly with water until neutral, add water to make a slurry with a concentration of 5ml water / g activated carbon;

[0039] 0.083ml concentration is the PdCl of 80g / L 2 Aqueous solution, with a concentration of 10g / L Na 2 CO 3 The aqueous solution was adjusted to pH 5.

[0040] Add the above PdCl dropwise to 6g of activated carbon slurry 2 The aqueous solution was magnetically stirred in a water bath at 70°C for 3 hours, then filtered, and the filter cake was dried in an oven at 110°C for 3 hours to obtain a Pd / activated carbon catalyst with a loading capacity of 0.4%.

Embodiment 2～6

[0042] Adopt the same preparation method as Example 1, wherein, PdCl 2 The addition amount of aqueous solution is 0.125, 0.167, 0.208, 0.250, 0.375ml respectively, can obtain the Pd / activated carbon catalyst of loading capacity as 0.6%, 0.8%, 1.0%, 1.2%, 1.8%.

Embodiment 7

[0044] 3g 3,4-dichloronitrobenzene, 25ml methanol solvent and the 0.6%Pd / activated carbon catalyst prepared in 0.05g embodiment 1 were added in a stainless steel autoclave, the autoclave was closed, and the air in the autoclave was replaced with nitrogen for 3 times , and then replace the nitrogen in the kettle with hydrogen for 3 times and maintain a certain pressure in the kettle. Under stirring, raise the temperature of the autoclave to 60°C, maintain the reaction pressure at 0.4 MPa, and react at a constant temperature until the pressure in the autoclave remains constant, unload the autoclave, discharge the material, filter out the catalyst, and analyze the filtrate with a capillary gas chromatograph, 3,4 - The conversion rate of dichloronitrobenzene is 100.0%, and the selectivity of 3,4-dichloroaniline is 97.1%.

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Abstract

A catalyst for preparing dichlorophenylamine by hydrogenating dichloronitrobenzene is composed of the activated carbon as carrier and the Pd as active component (0.2-2.0 Wt%) carried by said activated carbon. Its preparing process includes such steps as cyclically immersing activated carbon in diluted nitric acid, water washing until it becomes neutral, immersing in the aqueous solution of PdCl2, filtering, and baking the filtered cake. It has high catalytic performance and long cyclic service life.

Description

technical field [0001] The invention relates to a catalyst for preparing dichloroaniline by hydrogenation of dichloronitrobenzene and a preparation method thereof. Background technique [0002] Dichloroaniline is an important class of fine chemical intermediates, widely used in the fields of medicine, pesticides, dyes and daily chemicals. 3,4-Dichloroaniline is an important pesticide and dye intermediate, mainly used in the production of propanil, diuron, rituron and other herbicides and as a dye intermediate to synthesize disperse Scarlet G-S, and can also be used in the synthesis of Dichlorophenylthiourea, isocyanate, polymer monomer, etc. 2,4-Dichloroaniline is an important pharmaceutical and pesticide intermediate, mainly used in the synthesis of ciprofloxacin anti-cold medicine, agricultural fungicides, herbicides, etc. [0003] Common production processes for preparing dichloroaniline by hydrogenation of dichloronitrobenzene include iron powder reduction method, alka...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J21/18C07C211/52C07C209/36
Inventor 郭杨龙卢冠忠王义君郭耘王筠松刘晓晖王艳芹张志刚
Owner EAST CHINA UNIV OF SCI & TECH
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