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Preparation of a sulfur-doped activated carbon-supported noble metal catalyst and its application in hydrogenation of halogenated aromatic nitro compounds

A precious metal catalyst, hydrogenation reaction technology, applied in catalyst activation/preparation, metal/metal oxide/metal hydroxide catalyst, preparation of amino compounds, etc., can solve the problems of poor stability, poor selectivity and high activity, Achieve the effect of delayed life, low cost and low consumption

Active Publication Date: 2022-03-18
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Traditional commercial Pd / C catalysts have problems such as poor selectivity and poor stability in the selective hydrogenation of halogenated aromatic nitro compounds to prepare halogenated aromatic amines
Therefore, solving the problems of high activity, poor selectivity, easy loss or agglomeration of Pd / C catalyst is of great significance for the industrial production of halogenated aromatic amines

Method used

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  • Preparation of a sulfur-doped activated carbon-supported noble metal catalyst and its application in hydrogenation of halogenated aromatic nitro compounds
  • Preparation of a sulfur-doped activated carbon-supported noble metal catalyst and its application in hydrogenation of halogenated aromatic nitro compounds
  • Preparation of a sulfur-doped activated carbon-supported noble metal catalyst and its application in hydrogenation of halogenated aromatic nitro compounds

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Weigh Na 2 S·9H 2 O 1.4981g, add deionized water to make 50mL solution, mix well with 10g activated carbon, hydrothermally treat in a high-pressure hydrothermal reactor at 180°C for 10h; filter after cooling to room temperature, wash with a large amount of deionized water until the filtrate is neutral , The resulting filter cake was vacuum-dried at 110°C for 12 hours to obtain sulfur-doped activated carbon. Then 2.5g of the above-mentioned sulfur-doped activated carbon was made into a slurry with deionized water at a ratio of 1:3, and 0.5mL of H 2 PdCl 4 solution (Pd content is 0.05g / mL), stirred for 30min; then added 0.5mL sodium acetate solution (0.1g / mL), stirred for 30min; adjusted the pH value of the solution to 7-9 with 0.1g / mL NaOH solution, and continued to stir 30min; slowly add 0.5mL formaldehyde solution (37%-40%) dropwise, and continue to stir for 30min; filter, wash the filter cake with deionized water, and vacuum dry the filter cake at 110°C for 12h to ...

Embodiment 2

[0034] Weigh Na 2 S·9H 2 O 3.8216g, add 50mL deionized water to make a solution, mix with 10g activated carbon evenly, and hydrothermally treat in a high-pressure hydrothermal reactor at 200°C for 24h; filter after cooling to room temperature, wash with a large amount of deionized water until the filtrate is neutral , The resulting filter cake was vacuum-dried at 110°C for 12 hours to obtain sulfur-doped activated carbon. Then 2.5 g of the above-mentioned sulfur-doped activated carbon was made into a slurry with deionized water at a ratio of 1:5, and 1 mL of H 2 PdCl 4 Solution (Pd content is 0.05g / mL), stir for 100min; then add 1.5mL sodium acetate solution (0.1g / mL), stir for 100min; use 0.1g / mL KOH solution to adjust the pH value of the solution to 7-9, continue to stir 100 min; slowly add 1 mL of formaldehyde solution dropwise, and continue to stir for 100 min; filter, wash the filter cake with deionized water, and vacuum dry the filter cake at 110°C for 12 h to obtain ...

Embodiment 3

[0036] Weigh Na 2 S·9H 2O 7.4934g, add 100mL of deionized water to make a solution, mix well with 10g of activated carbon, hydrothermally treat in a high-pressure hydrothermal reactor at 250°C for 36h; filter after cooling to room temperature, wash with a large amount of deionized water until the filtrate is neutral , The resulting filter cake was vacuum-dried at 110°C for 12 hours to obtain sulfur-doped activated carbon. Then 2.5g of the above-mentioned sulfur-doped activated carbon was made into a slurry with deionized water at a ratio of 1:10, and 2.5mL of H 2 PdCl 4 Solution (Pd content is 0.05g / mL), stir for 60min; then add 2.5mL sodium acetate solution (0.1g / mL), stir for 60min; use 0.1g / mL NaOH solution to adjust the pH value of the solution to 7-9, continue to stir 60min; slowly add 0.6mL formaldehyde solution (37%-40%) dropwise, and continue to stir for 60min; filter, wash the filter cake with deionized water, and vacuum dry the filter cake at 80°C for 24h to obtai...

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Abstract

The invention discloses the preparation of a sulfur-doped activated carbon-supported noble metal catalyst and its application in the hydrogenation reaction of halogenated aromatic nitro compounds. The preparation method is carried out according to the following steps: (1) The sulfur-doped Miscellaneous activated carbon; (2) Take sulfur-doped activated carbon and add deionized water to form a slurry, add dropwise a soluble noble metal compound solution under stirring, the noble metal is Pd or Pt, stir; then add sodium acetate solution, stir; add alkali dropwise The pH of the solution is adjusted to 7-9, and the stirring is continued; then formaldehyde solution is added dropwise for reduction to obtain a sulfur-doped activated carbon-supported noble metal catalyst. The preparation method of the catalyst of the invention is simple in operation, low in cost, produces little pollution, and is favorable for industrial application. The catalyst is applied to the liquid-phase catalytic hydrogenation of halogenated aromatic nitro compounds to prepare halogenated aromatic amines, has high conversion rate and selectivity, good catalyst stability, and can be recycled and reused many times.

Description

(1) Technical field [0001] The invention relates to a preparation method of a sulfur-doped activated carbon supported noble metal catalyst and its application in the selective hydrogenation of halogenated aromatic nitro compounds to prepare halogenated aromatic amines. [0002] (2) Technical background [0003] Heterogeneous catalysts loaded with noble metals on different types of carriers have the advantages of high activity, easy separation and recovery, and reusability, and are widely used in various organic synthesis reactions. Carbon materials stand out among many support materials due to their unique pore structure, mechanical properties, and electrochemical properties. Pd / C catalysts have been commercialized and have broad application prospects in various heterogeneous catalytic reactions. However, due to its high activity, when catalyzing the selective hydrogenation reaction of substances with multiple reducing functional groups, excessive hydrogenation reactions ofte...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/42B01J23/44B01J35/00B01J37/02B01J37/10B01J37/16B01J37/20C07C209/36C07C211/52
CPCC07C209/365B01J23/42B01J23/44B01J37/0207B01J37/10B01J37/16B01J37/20B01J35/391B01J35/393C07C211/52
Inventor 张群峰周媛马磊卢春山丰枫李小年
Owner ZHEJIANG UNIV OF TECH
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