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Preparation method for catalyst used for preparation of chlorinated arylamines through catalytic hydrogenation

A technology for chlorinated aromatic amines and catalytic hydrogenation, which is applied in the preparation of organic compounds, catalysts for physical/chemical processes, and preparation of amino compounds. Hydrogen absorption and storage capacity, avoiding direct reduction, uniform distribution inhibition effect

Active Publication Date: 2018-05-01
JIANGSU RUIXIANG CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The above-mentioned existing patented technologies for the hydrogenation of chloronitrobenzene have their own characteristics, but there are also shortcomings: ①The cost of the catalyst is too high, such as carbon nanotubes, which have little industrial application value; ②The use of Pt or Pd with several other metals Compounding, the catalyst preparation process is complicated; ③ During the preparation of chloroaniline, one or more additives need to be continuously added to inhibit dechlorination, affecting product quality or increasing the residual amount of the kettle; ④ Using methanol or ethanol as a solvent increases costs and reduces production ability

Method used

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  • Preparation method for catalyst used for preparation of chlorinated arylamines through catalytic hydrogenation

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Coconut shell carbon with a particle size of 75 μm is used as the activated carbon carrier, and its specific surface area is 1500m 2 / g, the ash content is 1.5%. Weigh 50g of the above activated carbon, add 1000mL of 10wt% hydrochloric acid to it, stir at 60°C for 4h, filter to obtain a filter cake (activated carbon wet basis); add 400mL of 20wt% nitric acid to the activated carbon wet basis, heat and stir at 80°C for 4h, filter Obtain filter cake, wash with deionized water to neutrality, add 200mL deionized water to filter cake and be mixed with charcoal slurry.

[0026] Weigh 2.50g palladium chloride and dissolve it in 50mL of 20wt% dilute hydrochloric acid, add it to the carbon slurry, stir at 30°C for 2h, add 10wt% sodium hydroxide to adjust the pH=9.5, and continue to keep warm for 4h; Into H 2 6.5h, add 0.35g of ammonia water with a concentration of 10wt%, stir at 30°C for 6h, filter, wash the catalyst repeatedly with deionized water until the pH of the catalys...

Embodiment 2

[0028] Apricot shell charcoal with a particle size of 75 μm is used as the activated carbon carrier, and its specific surface area is 1200m 2 / g, the ash content is 2.0%. Weigh 50g of the above-mentioned activated carbon, add 800mL of 20wt% hydrochloric acid to it, stir at 60°C for 4h, and filter to obtain a filter cake (activated carbon wet basis); add 400mL of 30wt% nitric acid to the activated carbon wet basis, stir at 80°C for 4h, and obtain The filter cake was washed with deionized water until neutral, and 200 mL of deionized water was added to the filter cake to prepare a carbon slurry.

[0029] Weigh 1.83g of palladium nitrate and dissolve it in 50mL of 20wt% dilute hydrochloric acid, add it to the carbon slurry, stir at 30°C for 2h, add 10wt% sodium hydroxide to adjust the pH=9.5, and continue to keep warm for 4h; Access to H 2After 6.5 hours, continue to flow 0.11g of ammonia gas, stir at 30°C for 6 hours, filter, and wash the catalyst repeatedly with deionized wate...

Embodiment 3

[0031] Coconut shell carbon with a particle size of 75 μm is used as the activated carbon carrier, and its specific surface area is 1500m 2 / g, the ash content is 1.5%. Weigh 50g of the above-mentioned activated carbon, add 800mL of 15wt% hydrochloric acid to it, heat and stir at 60°C for 4h, filter to obtain a filter cake (activated carbon wet basis); add 800mL of 10wt% nitric acid to the activated carbon wet basis, heat and stir at 80°C for 4h, filter The obtained filter cake was washed with deionized water to neutrality, and 200 mL of deionized water was added to the filter cake to prepare carbon slurry.

[0032] Weigh 5.25g of chloroplatinic acid and dissolve it in 50mL of 20wt% dilute hydrochloric acid, add it to the carbon slurry, stir at 30°C for 2h, add 10wt% sodium hydroxide to adjust pH=10, and continue to keep warm for 4h; Into H 2 After 2h, add 0.86g of ammonium sulfate, stir at 30°C for 6h, filter, and wash the catalyst repeatedly with deionized water until the...

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Abstract

The invention relates to a preparation method for a catalyst used for preparation of chlorinated arylamines through catalytic hydrogenation, and specifically to a preparation method for a supported noble metal complex catalyst and an application of the supported noble metal complex catalyst in preparation of the chlorinated arylamines like o-chloroaniline, 3,4-dichloroaniline and 2,5-dichloroaniline through catalytic hydrogenation. The invention provides a preparation method for a carbon-supported catalyst (Pt-N / C or Pd-N / C for short, wherein N represents one or more selected from the group consisting of inorganic ammonium compounds) which is obtained through an action of noble metal and an inorganic ammonium compound; and the catalyst is used for preparation of the chlorinated arylaminesthrough catalytic hydrogenation of chloronitrobenzene. The preparation processes for the catalyst and the chlorinated arylamines have the following main advantages: 1, little difference is generated between preparation processes of the catalyst and ordinary noble metal carbon-supported catalysts, and the preparation processes are simple; 2, continuous addition of an auxiliary agent is not needed in the process of preparation of the chlorinated arylamines through catalytic hydrogenation of chloronitrobenzene by utilizing the catalyst; 3, the catalyst has stable activity and low dechlorination amount in the process of hydrogenation; and 4, no solvent is used in the process of hydrogenation, and production capacity is improved.

Description

technical field [0001] The present invention relates to a method for preparing a catalyst for preparing chlorinated arylamine by catalytic hydrogenation; in particular, it relates to a method for preparing a supported noble metal complex catalyst and its application in preparing chloroaniline by catalytic hydrogenation , such as o-chloroaniline, 3,4-dichloroaniline and 2,5-dichloroaniline. Background technique [0002] Chloroaniline is a class of important organic intermediates of pesticides and medicines, and is widely used in the synthesis of fine chemical products such as medicines, dyes and pigments. Among them, o-chloroaniline can be applied to the color base of dyes, as a diazo component of azo dyes and as an intermediate for the manufacture of medicines and pesticides; 3,4-dichloroaniline and 2,5-dichloroaniline are important pesticides and dyes Intermediates are widely used in the synthesis of herbicides and azo dyes, and some of them are used in the synthesis of me...

Claims

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Application Information

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IPC IPC(8): B01J27/24C07C209/36C07C211/52
CPCB01J27/24C07C209/365C07C211/52
Inventor 周颖华徐林黄杰军丁克鸿
Owner JIANGSU RUIXIANG CHEM
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