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A kind of preparation method of copper-manganese bimetallic catalyst for hydrogenation of p-nitrophenol

A bimetallic catalyst and catalyst technology, applied in the field of nanomaterials, can solve the problems of difficulty in industrialized production of cost resources, inability to meet industrial requirements, and reduce conversion rate, so as to improve production conditions, improve activity and stability, and prolong service life. Effect

Active Publication Date: 2021-08-10
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, Raney-Ni not only catalyzes the hydrogenation of nitro groups but also catalyzes the hydrogenation of benzene rings, resulting in the generation of by-products and reducing the conversion rate
Although noble metal catalysts have good catalytic activity, they are difficult to be used in industrial production due to high cost and scarce resources, and cannot meet industrial requirements.

Method used

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  • A kind of preparation method of copper-manganese bimetallic catalyst for hydrogenation of p-nitrophenol
  • A kind of preparation method of copper-manganese bimetallic catalyst for hydrogenation of p-nitrophenol
  • A kind of preparation method of copper-manganese bimetallic catalyst for hydrogenation of p-nitrophenol

Examples

Experimental program
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Effect test

Embodiment 1

[0029] (1) Weigh 0.2664g copper chloride, 0.36g manganese chloride and 0.2g Al2O3 into a beaker, add 30mL of ethanol and deionized water mixed liquid, dissolve at room temperature and stir for 12h.

[0030] (2) Stir the impregnated solution at 80° C. until evaporated to dryness.

[0031] (3) Dry the obtained solid under vacuum at 60° C. for 24 h.

[0032] (3) After complete drying, the obtained solid is ground, and calcined under the protection of nitrogen after grinding. The calcination temperature is 400°C, the calcination time is 2h, the heating rate is 5°C / min, and the gas flow rate is maintained at about one bubble per second. Cooling after reaction, the obtained copper-manganese bimetallic catalyst particles for p-nitrophenol hydrogenation reaction.

[0033] Add 1 mg of catalyst to 2 mL of deionized water, 0.1 mL of 5 mM p-nitrophenol solution, and 1 mL of 0.02 M sodium borohydride solution, and test the reaction with a UV spectrophotometer.

[0034] figure 1 It is t...

Embodiment 2

[0038] (1) Weigh 0.2664g copper chloride, 0.36g manganese chloride and 0.2g Al2O3 into a beaker, add 30mL of ethanol and deionized water mixed liquid, dissolve at room temperature and stir for 12h.

[0039] (2) Stir the impregnated solution at 80° C. until evaporated to dryness.

[0040] (3) Dry the obtained solid under vacuum at 60° C. for 24 h.

[0041] (4) After complete drying, the obtained solid is ground, and calcined under the protection of nitrogen after grinding. The calcination temperature is 600°C, the calcination time is 2 hours, the heating rate is 5°C / min, and the gas flow rate is maintained at about one bubble per second. Cooling after reaction, the obtained copper-manganese bimetallic catalyst particles for p-nitrophenol hydrogenation reaction.

Embodiment 3

[0043] (1) Weigh 0.1903g copper chloride, 0.0514g manganese chloride and 0.2g Al2O3 into a beaker, add 30mL of ethanol and deionized water mixed liquid, dissolve at room temperature and stir for 12h.

[0044] (2) Stir the impregnated solution at 80° C. until evaporated to dryness.

[0045] (3) Dry the obtained solid under vacuum at 60° C. for 24 h.

[0046] (4) After complete drying, the obtained solid is ground, and calcined under the protection of nitrogen after grinding. The calcination temperature is 400°C, the calcination time is 2h, the heating rate is 5°C / min, and the gas flow rate is maintained at about one bubble per second. Cooling after reaction, the obtained copper-manganese bimetallic catalyst particles for p-nitrophenol hydrogenation reaction.

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Abstract

The invention discloses a method for preparing a copper-manganese bimetallic catalyst for hydrogenation of p-nitrophenol, which belongs to the field of nanometer materials. Catalyst preparation follows the following steps: 1) Mix copper source, manganese source, carrier Al2O3 and solvent to obtain mixed solution A; 2) Stir and impregnate the mixed solution at room temperature for 12h-24h, and then mix it at 80°C-110°C Evaporate to dryness to obtain solid B; 3) Dry solid B, and calcinate the dried solid at 200°C-600°C under the protection of an inert gas. The catalyst prepared by the method does not use additional reducing agents, surface active agents and organic solvents, has low cost, is environmentally friendly, saves resources, and has high activity and stability. The preparation method is simple and is suitable for industrialization.

Description

technical field [0001] The invention relates to a copper-manganese bimetallic catalyst and its application in hydrogenation of p-nitrophenol, belonging to the field of nanometer materials. Background technique [0002] P-Aminophenol (PAP) is an intermediate of fine chemical industry, especially synthetic medicine, dyestuff and organic synthesis. In my country, it is mostly used in medicine, especially the important intermediates for the synthesis of paracetamol, parametremol and clofibrate, among which paracetamol is the most important application. There are several production methods of p-nitroaminophenol, such as p-nitrophenol reduction method, pressurized hydrolysis and acidification of p-nitrochlorinated benzene under alkaline conditions, hydrolysis of p-phenylenediamine, and hydrogenation rearrangement of p-nitrophenol Wait. Among them, the hydrogenation rearrangement of p-nitrophenol has attracted attention due to its low cost and low environmental pollution. [000...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/889C07C215/76C07C213/02
Inventor 程道建栾晓旭吴登峰
Owner BEIJING UNIV OF CHEM TECH