Catalyst for preparing chlorinated aromatic amine and preparation method thereof

A catalyst and aromatic amine technology, applied in the field of catalysis, can solve the problems of excessive dechlorination by-products and insignificant inhibition of dechlorination side reactions, and achieve the effects of avoiding the accumulation of hydroxylamine, good activity and selectivity, and not easy to be poisoned

Active Publication Date: 2016-06-22
中国中化股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Li Xiaonian et al. [CN102285891A] disclosed a method for preparing aromatic amines by catalytic hydrogenation of nitro compounds. In the presence of inhibitor ammonium compounds (such as ammonium chloride, ammonium acetate, etc.), the generation of azo compounds can be significantly reduced , but the inhibition effect of this process on the side reaction of dechlorination is not significant
Using this method, when 2-chloronitrobenzene is catalytically hydrogenated with Pt / C catalyst, the selectivity of 2-chloroaniline is 97.62%, and more dechlorination by-products are produced

Method used

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  • Catalyst for preparing chlorinated aromatic amine and preparation method thereof
  • Catalyst for preparing chlorinated aromatic amine and preparation method thereof
  • Catalyst for preparing chlorinated aromatic amine and preparation method thereof

Examples

Experimental program
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preparation example Construction

[0028] The preparation method of the catalyst: impregnating the carrier with a vanadium compound solution, washing, and drying; then impregnating the carrier impregnated with the vanadium compound solution in an aqueous solution of a palladium compound and a copper compound, and adjusting the pH value of the solution to alkaline with an alkali solution, and Use reducing agent to reduce treatment, filter and wash, and dry to obtain the catalyst.

[0029] The catalyst is used for the catalytic hydrogenation of chlorinated aromatic nitro compounds to prepare chlorinated aromatic amines, wherein the structural formula of the chlorinated aromatic nitro compounds is shown in formula I:

[0030]

[0031] In the formula I, X=Cl; R 1 =H, R, NH 2 etc., wherein R is a C1-C8 alkane group; s, r, t represent numbers 1, 2 or 3, wherein s+r+t is less than or equal to 6.

Embodiment 1

[0033] Preparation of Pd-Cu-V / C Catalyst with 5% Pd Loading

[0034] Weigh 10.0g activated carbon (the specific surface area is 1000m 2 / g), added to 120mL distilled water stirred at a speed of 300 rpm. Add 50mL of vanadyl acetylacetonate in ethanol (containing 0.12gV) to the above suspension, keep it for 5h, filter and wash with water. Add the above treated activated carbon into 150mL of distilled water stirred at a speed of 300 rpm, slowly add 10mL of H 2 PdCl 4 solution (containing 0.5gPd), then slowly dropwise add 10mL copper acetate solution (containing 0.15gCu), stir for 6h, slowly add dropwise a sodium hydroxide solution with a mass content of 10% to adjust the pH to weakly alkaline (pH=8), and stir After 1h, the temperature was lowered to room temperature, filtered, and washed with water until neutral. After washing to neutrality, make a 150ml slurry at 30°C, then slowly add 2mL of 85% hydrazine hydrate solution dropwise, continue to stir for 2h, filter, wash with ...

Embodiment 2

[0036] Pd-Cu-V / C catalyst with 3% Pd loading

[0037] Weigh 10.0g activated carbon (the specific surface area is 1000m 2 / g), added to 120mL distilled water stirred at a speed of 300 rpm. Add 50ml of vanadyl acetylacetonate ethanol solution (containing 0.072gV) to the above suspension, keep it for 5h, filter and wash with water. Add the above treated activated carbon into 150 mL of distilled water stirred at 300 rpm, slowly add 6 mL of H 2 PdCl 4 solution (containing 0.3gPd), then slowly dropwise added 6mL copper acetate solution (containing 0.09gCu), stirred for 6h, slowly added dropwise a sodium hydroxide solution with a mass content of 10% to adjust the pH to weakly alkaline (pH=8), and stirred 1h, the temperature is lowered to room temperature, filtered, washed with water until neutral; after washing to neutral, make 150mL slurry at 30°C, then slowly add 2mL of 85% hydrazine hydrate solution dropwise, continue to stir for 2h, filter, wash with water , and dried to obta...

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Abstract

The invention belongs to the field of catalysis, and particularly relates to a catalyst for preparation of a chlorinated aromatic amine through catalytic hydrogenation of a chlorinated aromatic nitro compound and a preparation method thereof. The catalyst is a carrier activated carbon, an active component is palladium, and auxiliary agent components are copper and vanadium, wherein the weight of palladium accounts for 0.1-10% of the weight of the carrier, the molar ratio of palladium to copper is 1:2-10:1, and the molar ratio of palladium to vanadium is 1:2-10:1. The catalyst is used for selective catalytic hydrogenation of the chlorinated aromatic nitro compound, not only has quite good catalytic activity and selectivity, but also has good stability, is easy to prepare, and has a good application prospect.

Description

technical field [0001] The invention belongs to the field of catalysis, and specifically relates to a catalyst used for catalytic hydrogenation of chlorinated aromatic nitro compounds to prepare chlorinated aromatic amines and a preparation method thereof. Background technique [0002] Chlorinated aromatic amines are important fine chemical intermediates, widely used in medicine, pesticides, dyes, pigments, rubber additives, resins, photosensitive materials and other fields. They are prepared by catalytic hydrogenation of the corresponding chlorinated aromatic nitro compounds. The catalytic hydrogenation is usually carried out in the liquid phase. The typical catalytic hydrogenation conditions are: the reaction temperature is 25-250 °C, and the hydrogen pressure is 0.1- 35MPa, the reaction conditions are well known to those skilled in the art. [0003] The advantages of catalytic hydrogenation, such as atom economy, environmental friendliness, and continuous large-scale dev...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/89C07C209/36C07C211/52
Inventor 李付刚孙兵
Owner 中国中化股份有限公司
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