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Nitrogen-doped mesoporous carbon supported metal catalyst as well as preparation method and application thereof

A metal-loaded, nitrogen-mesoporous technology, which is applied in the preparation of amino compounds, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of unfavorable industrial production, aggregation of metal particles, and difficult operation, and achieve uniform dispersion. , High reactivity, high catalytic activity

Active Publication Date: 2020-07-14
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the method of preparing mesoporous carbon materials is generally cumbersome and difficult to operate, which is not conducive to industrial production, and the catalyst obtained by directly impregnating the mesoporous carbon carrier may easily cause the aggregation and loss of metal particles.

Method used

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  • Nitrogen-doped mesoporous carbon supported metal catalyst as well as preparation method and application thereof
  • Nitrogen-doped mesoporous carbon supported metal catalyst as well as preparation method and application thereof
  • Nitrogen-doped mesoporous carbon supported metal catalyst as well as preparation method and application thereof

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preparation example Construction

[0028] The invention provides a method for preparing a nitrogen-doped mesoporous carbon-supported metal catalyst, comprising the following steps:

[0029] 1) dissolving citric acid and magnesium nitrate in water to obtain a mixed solution, and evaporating the obtained mixed solution to obtain a transparent sol;

[0030] 2) foaming the transparent sol to obtain a xerogel foam;

[0031] 3) performing roasting treatment after refining the dry gel foam to obtain a roasted material;

[0032] 4) The obtained calcined material is acid-washed to remove magnesium to obtain a mesoporous carbon material;

[0033] 5) mixing nitrogen source, mesoporous carbon material and solvent, evaporating to dryness and roasting to obtain nitrogen-doped mesoporous carbon material;

[0034] 6) Mixing the nitrogen-doped mesoporous carbon material with metal particles, performing metal loading treatment, and further performing reduction treatment to obtain a nitrogen-doped mesoporous carbon-supported me...

Embodiment 1

[0058] 1) Dissolve citric acid monohydrate and magnesium nitrate hexahydrate in water to obtain a mixed solution, in which the concentrations of citric acid and magnesium nitrate are both 5mol / L, place the mixed solution in a water bath at 90°C for 3 hours, stir and evaporate to obtain a transparent Sol;

[0059] 2) Put the transparent sol in an oven at 140°C for foaming treatment for 4 hours to obtain dry gel foam;

[0060] 3) Grind the dry gel foam in a mortar, put it into a tube furnace, and carry out roasting treatment under a nitrogen atmosphere at a temperature of 800°C (heating rate of 2°C / min) for 2 hours to obtain a roasted material;

[0061] 4) Stir and reflux the obtained calcined material with 3 mol / L hydrochloric acid solution in a water bath at 65°C for 6 hours to remove MgO in the mixture, filter the product, wash with excess deionized water until neutral, and finally put it in an oven for Dry to obtain mesoporous carbon material;

[0062] 5) Take 8-hydroxyqu...

Embodiment 2

[0068] 1) Dissolve citric acid monohydrate and magnesium nitrate hexahydrate in water to obtain a mixed solution, in which the concentrations of citric acid and magnesium nitrate are both 5mol / L, place the mixed solution in a water bath at 90°C for 3 hours, stir and evaporate to obtain a transparent Sol;

[0069] 2) Put the transparent sol in an oven at 140°C for foaming treatment for 4 hours to obtain dry gel foam;

[0070] 3) Grind the dry gel foam in a mortar, put it into a tube furnace, and carry out roasting treatment under a nitrogen atmosphere at a temperature of 700°C (heating rate of 2°C / min) for 2 hours to obtain a roasted material;

[0071] 4) Stir and reflux the obtained calcined material with 3 mol / L hydrochloric acid solution in a water bath at 65°C for 6 hours to remove MgO in the mixture, filter the product, wash with excess deionized water until neutral, and finally put it in an oven for Dry to obtain mesoporous carbon material;

[0072] 5) Take 8-hydroxyqu...

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Abstract

The invention relates to the technical field of catalyst preparation, in particular to a nitrogen-doped mesoporous carbon supported metal catalyst as well as a preparation method and application thereof. Citric acid and magnesium nitrate are dissolved in water and evaporated, dry gel foam is obtained after foaming treatment, and the dry gel foam is sequentially subjected to roasting and acid pickling magnesium removal to obtain the mesoporous carbon material. A nitrogen source, a mesoporous carbon material and a solvent are mixed, evaporated to dryness, subjected to secondary roasting and thensubjected to metal loading and reduction treatment in sequence, and the nitrogen-doped mesoporous carbon loaded metal catalyst is obtained. The preparation method of the nitrogen-doped mesoporous carbon supported metal catalyst provided by the invention is simple, the nitrogen-doped mesoporous carbon supported metal catalyst is applied to selective reduction reaction of nitro compounds, the catalytic activity is high, the selectivity of amine preparation by reduction reaches up to 99%, and the catalytic effect is excellent.

Description

technical field [0001] The invention relates to the technical field of catalyst preparation, in particular to a nitrogen-doped mesoporous carbon-supported metal catalyst and a preparation method and application thereof. Background technique [0002] Halogenated arylamine is an important intermediate in organic synthesis, and it is the main raw material for chemical reagents, dyes, pigments and other chemical products, as well as medicine, pesticide and photographic medicine. The main preparation method of aromatic amines is obtained by reducing the corresponding aromatic nitro compounds. At present, the methods for producing aromatic amines by reducing nitro groups include iron powder reduction method, alkali sulfide reduction method, catalytic hydrogenation method, and hydrogen transfer reduction method. law etc. [0003] Iron powder reduction method and alkali sulfide reduction method tend to produce a large amount of waste water and toxic sludge during the reduction proc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J35/10C07C209/36C07C211/52
CPCB01J27/24C07C209/365B01J35/391B01J35/618B01J35/638B01J35/647C07C211/52
Inventor 尚兴付邢志康汪学广邹秀晶程功林丁伟中
Owner SHANGHAI UNIV