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Production of 3,4-dichloroaniline catalyst with 3,4-mirbane oil dichloride hydrogenation

A technology of dichloronitrobenzene and dichloroaniline, which is applied in the field of palladium-carbon catalyst preparation, can solve the problems of complex preparation process, high price, and dependence on carbon nanotubes, and achieve the effect of simple preparation process

Inactive Publication Date: 2006-08-16
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this patented technology uses binary active components, and there is also a complicated preparation process; the recovery cost of precious metal Ru increases due to the use of aluminum oxide as a carrier.
Chinese patent [CN02148509.7] uses Pd / NCT and Pt / NCT as catalysts respectively, and the selectivity of 3,4-dichloroaniline is 99.2% and 99% respectively, but uses carbon nanotubes as carrier, and the price of carrier is expensive, etc. , the prospect of industrial application of this patented technology will depend on the cost of carbon nanotubes

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Weigh 10g of activated carbon, the specific surface area of ​​activated carbon is 1600m 2 / g, activated carbon was impregnated in 120 ml of KI solution with a concentration of 2.5 mol / l for 6 hours, filtered, and washed with deionized water until no iodide ion was detected. Then the treated activated carbon was formulated into a 100ml slurry at a temperature of 80°C, and 4ml of H 2 PdCl 4 solution (Pd content is 0.05g / ml), stirred for 6h, then adjusted the pH value of the solution to weakly alkaline (pH=8) with 10% NaOH solution, and lowered the temperature to room temperature, filtered, and washed with deionized water to medium sex. The unreduced catalyst was prepared into a 150 ml slurry at 30° C., and then 2 ml of 85% hydrazine hydrate solution was slowly added dropwise, and the stirring was continued for 2 hours. The reduced catalyst was filtered, washed with deionized water until neutral, and finally dried in the air at room temperature, and the wet sample was t...

Embodiment 2

[0023] Weigh 10g of activated carbon, the specific surface area of ​​activated carbon is 1600m 2 / g, activated carbon was impregnated in 120 ml of KI solution with a concentration of 2.5 mol / l for 6 hours, filtered, and washed with deionized water until no iodide ion was detected. Then the treated activated carbon was formulated into a 100ml slurry at a temperature of 80°C, and 2ml of H 2 PdCl 4 Solution (Pd content is 0.05g / ml), stirred for 6h, adjusted the pH value of the solution to weakly alkaline (pH=8) with 10% NaOH solution, and lowered the temperature to room temperature, filtered, and washed with deionized water until neutral . The unreduced catalyst was prepared into a 150ml slurry at 30°C, and then 2ml of 85% hydrazine hydrate solution was slowly added dropwise, and the stirring was continued for 2 hours. The reduced catalyst was filtered, washed with deionized water until neutral, and finally dried in the air at room temperature, and the wet sample was taken and...

Embodiment 3

[0025] Weigh 10g of activated carbon, the specific surface area of ​​activated carbon is 1600m 2 / g, activated carbon was impregnated in 120 ml of KI solution with a concentration of 2.5 mol / l for 6 hours, filtered, and washed with deionized water until no iodide ion was detected. Then the treated activated carbon was formulated into a 100ml slurry at a temperature of 80°C, and 6ml of H 2 PdCl 4 Solution (Pd content is 0.05g / ml), stirred for 6h, adjusted the pH value of the solution to weakly alkaline (pH=8) with 10% NaOH solution, and lowered the temperature to room temperature, filtered, and washed with deionized water until neutral . The unreduced catalyst was prepared into a 150ml slurry at 30°C, and then 2ml of 85% hydrazine hydrate solution was slowly added dropwise, and the stirring was continued for 2 hours. The reduced catalyst was filtered, washed with deionized water until neutral, and finally dried in the air at room temperature, and the wet sample was taken and...

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Abstract

A catalyst for preparing 3,4-dichlorophenylamine from 3,4-dichloronitrobenzene by hydrogenating is prepared through immersing activated carbon in the aqueous solution of potassium (or sodium) halide, washing until no halogen ions, immersing it in the aqueous solution of H2PdCl4, regulating pH value, filtering, washing filtered cake, reducing to obtain neutral product, and drying. It has high catalytic activity and selectivity.

Description

(1) Technical field [0001] The invention relates to a preparation method of a palladium carbon catalyst used for the catalytic hydrogenation of 3,4-dichloronitrobenzene to prepare 3,4-dichloroaniline, especially suitable for the catalytic hydrogenation of 3,4-dichloronitrobenzene Process for the preparation of palladium activated carbon catalysts for the preparation of 3,4-dichloroaniline. (2) Background technology [0002] 3,4-Dichloroaniline is an important intermediate of pesticides and dyes, widely used in the synthesis of herbicides such as propanil, riguron, diuron, benzopyr and azo dyes, and also in the production of bacteriostatic agents 3,4,4'-Raw material for trichlorocarbanilide. Usually, 3,4-dichloroaniline is prepared by reducing 3,4-dichloronitrobenzene by chemical reduction method, electrolytic reduction method and catalytic hydrogenation reduction method. The chemical reduction methods such as the iron powder reduction method under acidic conditions or the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J37/02B01J37/16B01J23/44C07C209/36C07C211/45
Inventor 李小年马磊卢春山厉嘉云刘化章
Owner ZHEJIANG UNIV OF TECH
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