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Preparation method of supported catalyst for synthesizing chloroaniline through catalytic hydrogenation of chloronitrobenzene

A technology that catalyzes chloronitrobenzene and catalyzes chloronitrobenzene with high efficiency. It is applied in the direction of amino compound preparation, organic compound preparation, catalyst activation/preparation, etc. It can solve the problems of increasing the residual volume of the kettle and affecting the purity of the product. Achieve the effect of improving catalytic activity, low price, and not easy to lose

Inactive Publication Date: 2019-06-28
JIANGSU YANGNONG CHEM GROUP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods need to continuously add dechlorination inhibitors. Although the dechlorination amount decreases, it also increases the residual amount of the kettle and affects the product purity.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1.1 Activated carbon pretreatment

[0024] Add 50 g of activated carbon and 1000 g of 20 wt % hydrochloric acid solution to a 2000 mL three-necked flask in sequence, and stir at 60° C. for 3 h. After filtering, 300 g of 25 wt % nitric acid solution was added to the filter cake, and stirred at 80° C. for 5 h. Add ammonia water to adjust pH to neutrality, then wash twice to obtain activated carbon slurry, N 2 Dry under air and set aside.

[0025] 1.2 Preparation of catalyst

[0026] Get 20g polyacrylonitrile, 30g pretreated activated carbon, 0.4g chloroplatinic acid, 0.13g zinc chloride, ultrasonically disperse in N,N-dimethylformamide for 2h, then in N 2 Under drying treatment, a yellow-brown slurry was obtained. Put the slurry in the pass with N 2 、H 2 The Pt / Zn bimetallic catalyst supported on nitrogen-doped activated carbon was obtained by calcination at a high temperature of 900 °C in a muffle furnace with mixed gas for 2 h. The Pt content is 0.30wt% and the Z...

Embodiment 2

[0030] 2.1 Activated carbon pretreatment

[0031] Add 50 g of activated carbon and 1000 g of 20 wt % hydrochloric acid solution to a 2000 mL three-necked flask in sequence, and stir at 60° C. for 3 h. After filtering, 300 g of 25 wt % nitric acid solution was added to the filter cake, and stirred at 80° C. for 5 h. Add ammonia water to adjust pH to neutrality, then wash twice to obtain activated carbon slurry, N 2 Dry under air and set aside.

[0032] 2.2 Preparation of catalyst

[0033] Take 20g polyacrylonitrile, 30g pretreated activated carbon, 0.60g chloroplatinic acid, 0.15g zinc chloride, ultrasonically disperse in N,N-dimethylformamide for 2h, and then in N 2 Under drying treatment, a yellow-brown slurry was obtained. Put the slurry in the pass with N 2 、H 2 The mixed gas was calcined in a muffle furnace at 900°C for 2 hours to obtain a Pt / Zn bimetallic catalyst supported on nitrogen-doped activated carbon. The Pt content is 0.45wt% and the Zn content is 0.16wt% ...

Embodiment 3

[0037] 3.1 Activated carbon pretreatment

[0038] Add 50 g of activated carbon and 1000 g of 20 wt % hydrochloric acid solution to a 2000 mL three-necked flask in sequence, and stir at 60° C. for 3 h. After filtering, 300 g of 25 wt % nitric acid solution was added to the filter cake, and stirred at 80° C. for 5 h. Add ammonia water to adjust pH to neutrality, then wash twice to obtain activated carbon slurry, N 2 Air dry, set aside.

[0039] 3.2 Preparation of catalyst

[0040] Take 20g polyacrylonitrile, 30g pretreated activated carbon, 0.80g chloroplatinic acid, 0.30g zinc chloride, ultrasonically disperse in N,N-dimethylformamide for 2h, then in N 2 Under drying treatment, a yellow-brown slurry was obtained. Put the slurry in the pass with N 2 、H 2 The mixed gas was calcined in a muffle furnace at 900°C for 2 hours to obtain a Pt / Zn bimetallic catalyst supported on nitrogen-doped activated carbon. The ICP spectrometer was used to measure and calculate the Pt content...

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Abstract

The invention relates to a preparation method of a supported catalyst for synthesizing chloroaniline through catalytic hydrogenation of chloronitrobenzene and particularly relates to a preparation method of a nitrogen-doped carbon material supported noble metal catalyst applied to the synthesis of chloroaniline through catalytic hydrogenation. The catalyst has the advantages of high catalytic activity, dechloridation inhibition capacity, long service life and the like, and the prepared chloroaniline product is high in purity.

Description

technical field [0001] The invention relates to a preparation method of a catalyst for synthesizing chloroaniline. Specifically, it relates to a preparation method of a nitrogen-doped carbon material supported noble metal catalyst, which is applied to the synthesis of chloroaniline by catalytic hydrogenation. Background technique [0002] Chloroaniline is a class of important organic synthesis intermediates, which can be widely used in the production of fine chemicals such as medicines, pesticides, and dyes. The industrialization methods of chloroaniline at home and abroad mainly include iron powder reduction method, alkali sulfide reduction method and catalytic hydrogenation method. The iron powder reduction method and the alkali sulfide reduction method have problems such as high cost, low yield, and large environmental pollution caused by the three wastes produced, and have basically been eliminated. The catalytic hydrogenation method has the advantages of short reactio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J37/34B01J37/08C07C209/36C07C211/52
Inventor 寇书培丁克鸿徐林郑亚清张寅马庆炎王敏娟陆仁标
Owner JIANGSU YANGNONG CHEM GROUP
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