Preparation of sulfur-doped activated carbon catalyst loaded with noble metal and application of sulfur-doped activated carbon catalyst loaded with noble metal in halogenated aromatic nitro-compound hydrogenation reaction

A noble metal catalyst and aromatic nitro group technology, which is applied in the direction of catalyst activation/preparation, metal/metal oxide/metal hydroxide catalyst, amino compound preparation, etc. It can solve the problems of poor stability, poor selectivity, easy loss, etc. , to achieve the effect of many application times, low cost, and not easy to reunite and lose

Active Publication Date: 2019-02-12
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 sulfur-doped activated carbon catalyst loaded with noble metal and application of sulfur-doped activated carbon catalyst loaded with noble metal in halogenated aromatic nitro-compound hydrogenation reaction
  • Preparation of sulfur-doped activated carbon catalyst loaded with noble metal and application of sulfur-doped activated carbon catalyst loaded with noble metal in halogenated aromatic nitro-compound hydrogenation reaction
  • Preparation of sulfur-doped activated carbon catalyst loaded with noble metal and application of sulfur-doped activated carbon catalyst loaded with noble metal in halogenated aromatic nitro-compound hydrogenation reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 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

[0033] 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

[0035] 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 preparation of a sulfur-doped activated carbon catalyst loaded with noble metal and application of the sulfur-doped activated carbon catalyst loaded with the noble metal in halogenated aromatic nitro-compound hydrogenation reaction. A preparation method is carried out according to the following steps that 1, a hydrothermal method is adopted for preparing sulfur-doped activated carbon; 2, the sulfur-doped activated carbon is taken, deionized water is added to prepare slurry, under stirring, a soluble noble metal compound solution is added dropwise, the noble metal is Pdor Pt, stirring is conducted, then a sodium acetate solution is added, stirring is conducted, an alkaline solution is added dropwise to adjust a pH to be 7-9, stirring is continued, and then a formaldehyde solution is added dropwise for reduction, so that the sulfur-doped activated carbon catalyst loaded with the noble metal is obtained. The catalyst is simple in preparation method operation, lowin cost, small in generated pollution and beneficial for industrial application. The catalyst is applied to halogenated aromatic nitro-compound liquid phase catalytic hydrogenation to prepare halogenated arylamine, the conversion rate and the selectivity are high, and the catalyst is good in stability, and can be recovered and reused for multiple 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. (2) Technical background [0002] 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 often occur,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/42B01J23/44B01J35/00B01J37/02B01J37/10B01J37/16B01J37/20C07C209/36C07C211/52
CPCC07C209/365B01J23/42B01J23/44B01J35/0046B01J35/006B01J37/0207B01J37/10B01J37/16B01J37/20C07C211/52
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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