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Preparation method of Mn monatomic-loaded N-doped carbon polyhedral catalyst

A carbon polyhedron and catalyst technology, which is applied in the field of preparation of N-doped carbon polyhedron catalysts, can solve the problems of low metal single atom loading, easy agglomeration of carbon supports, and reduced mass transfer efficiency, so as to improve ORR stability and activity, The effect of optimizing the reaction path and simple synthesis process

Active Publication Date: 2021-12-03
CENT SOUTH UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above method has the following technical defects: (1) During the preparation process of carbon-supported SACs, the carbon support is easy to agglomerate, causing pore blockage and reducing the mass transfer efficiency; (2) The directly synthesized metal single-atom loading is low

Method used

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  • Preparation method of Mn monatomic-loaded N-doped carbon polyhedral catalyst
  • Preparation method of Mn monatomic-loaded N-doped carbon polyhedral catalyst
  • Preparation method of Mn monatomic-loaded N-doped carbon polyhedral catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0057] (1) Dissolve 10.0 mg manganese carbonyl and 1190 mg zinc nitrate in 30 mL of methanol solution at room temperature and stir for 10 minutes to obtain solution A. Dissolve 1380 mg of dimethylimidazole in 30 mL of methanol solution at room temperature and stir for 10 minutes , to obtain solution B, and then mix solution A and solution B at room temperature for 2 hours, then leave it to age for 12 hours at room temperature, centrifuge, filter and wash the precipitate with methanol solution for 3 times, and the white precipitate is stored at -25°C , freeze-dried for 48 hours to obtain precursor powder;

[0058] (2) The precursor powder obtained in step (1) was subjected to a heat treatment at 900°C for 3 hours under the protection of a high-purity nitrogen atmosphere to obtain a black powder;

[0059] (3) Disperse 100 mg of the black powder obtained in step (2) in 10 mL of 0.1 mol / L manganese carbonyl solution, stir at 25°C for 2 hours, and freeze-dry at -25°C for 36 hours t...

Embodiment 2

[0082] (1) Dissolve 20.0 mg of manganese acetate and 1190 mg of zinc nitrate in 40 mL of methanol solution at room temperature and stir for 20 minutes to obtain solution A. Dissolve 1450 mg of dimethylimidazole in 40 mL of methanol solution at room temperature and stir for 20 minutes , to obtain solution B, and then mix solution A and solution B at 60°C for 3 hours, then stand and age at 60°C for 16 hours, centrifuge, filter and wash the precipitate with methanol solution 3 times, the white precipitate is at -30 ℃, freeze-dried for 36 hours to obtain the precursor powder;

[0083] (2) Under the protection of a high-purity argon atmosphere, the precursor powder obtained in step (1) is subjected to a heat treatment at 800°C for 2 hours to obtain a black powder;

[0084] (3) Disperse 100 mg of the black powder obtained in step (2) in 5 mL of 0.2 mol / L manganese acetate solution, stir at 30°C for 1 hour, and freeze-dry at -30°C for 48 hours to obtain the sample powder;

[0085] (...

Embodiment 3

[0100] (1) Dissolve 30.0 mg of manganese acetylacetonate and 1190 mg of zinc nitrate in 50 mL of deionized water at room temperature and stir for 30 minutes to obtain solution A. Dissolve 1300 mg of dimethylimidazole in 50 mL of deionized water at room temperature and stir for 30 minutes In water, solution B was obtained, and then solution A and solution B were stirred and mixed for 1 hour at 80°C, then aged at 80°C for 8 hours, centrifuged, and the precipitate was filtered and washed 4 times with deionized water, and the white precipitate was in Freeze-drying at -20°C for 24 hours to obtain precursor powder;

[0101] (2) Mix the precursor powder obtained in step (1) with a volume fraction of 5% H 2 / 95%N 2 Under the protection of mixed gas atmosphere, heat treatment at 1000°C for 1 hour to obtain black powder;

[0102] (3) Disperse 100 mg of the black powder obtained in step (2) in 8 mL of 0.3 mol / L manganese acetylacetonate solution, stir at 20°C for 1.5h, and freeze-dry a...

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Abstract

The invention relates to a preparation method of an Mn monatomic-loaded N-doped carbon polyhedral catalyst, which comprises the following steps: (1) stirring and dissolving manganese salt and zinc nitrate in a solvent to obtain a solution A, stirring and dissolving an N-containing organic ligand in the solvent to obtain a solution B, stirring and mixing the solution A and the solution B, standing and aging, centrifuging, filtering and washing, and freeze-drying; (2) carrying out primary heat treatment under the protection of inert atmosphere; (3) dispersing in a manganese salt solution, stirring, and freeze-drying; and (4) carrying out secondary heat treatment under the protection of an inert atmosphere to obtain the Mn monatomic-loaded N-doped carbon polyhedral catalyst. The catalyst obtained through the method is good in dispersion, the metal Mn is dispersed in an atomic scale, Mn, N and C elements are evenly distributed, the electro-catalytic oxygen reduction performance is good, the rate performance is superior to that of a commercial Pt / C catalyst, and the catalyst is simple in synthesis process, efficient, low in cost, high in universality and suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of a catalyst, in particular to a preparation method of an N-doped carbon polyhedron catalyst supporting Mn single atoms. Background technique [0002] Single-atom catalysts (SACs) are a frontier of catalytic science in recent years. Reducing active species from particles to single atoms is an effective strategy to improve catalytic performance. Exposure increases the number of active sites; on the other hand, the intrinsic activity of active sites can be improved by utilizing effects such as enhanced interaction and charge transfer between single atoms and supports. However, due to the high specific surface energy, single metal atoms easily migrate and aggregate into nanoparticles at higher temperatures. Therefore, the controllable synthesis of highly stable and highly active SACs is still a big challenge. At present, the strategies for synthesizing SACs mainly include: defect engineering, spatial confin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/90H01M4/88
CPCH01M4/9083H01M4/9041H01M4/8825Y02E60/50
Inventor 雷永鹏王启晨
Owner CENT SOUTH UNIV
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