A kind of preparation method of n-doped carbon polyhedron catalyst supporting mn single atom

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: 2022-02-15
CENT SOUTH UNIV
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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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  • A kind of preparation method of n-doped carbon polyhedron catalyst supporting mn single atom
  • A kind of preparation method of n-doped carbon polyhedron catalyst supporting mn single atom
  • A kind of preparation method of n-doped carbon polyhedron catalyst supporting mn single atom

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] (1) First, 10.0 mg of carbonyl manganese and 1190 mg of zinc nitrate were dissolved in 30 mL of methanol solution at room temperature with stirring for 10 min to obtain solution A, and 1380 mg of dimethylimidazole was dissolved in 30 mL of methanol solution at room temperature with stirring for 10 min , get solution B, and then mix solution A and solution B at room temperature for 2 hours, then at room temperature, let stand for aging for 12 hours, centrifuge, filter and wash the precipitate with methanol solution 3 times, the white precipitate is at -25 ℃ , freeze-dried for 48h to obtain precursor powder;

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

[0059] (3) Disperse 100 mg of black powder obtained in step (2) in 10 mL of 0.1 mol / L manganese carbonyl solution, stir at 25 °C for 2 h, and freeze-dry it at -25 °C for 36 h 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 with stirring for 20 min to obtain solution A, and dissolve 1450 mg of dimethylimidazole in 40 mL of methanol solution at room temperature with stirring for 20 min , get solution B, and then mix solution A and solution B at 60 ℃ for 3 hours, then at 60 ℃, let stand for aging for 16 hours, centrifuge, filter and wash the precipitate with methanol solution 3 times, the white precipitate is at -30 At ℃, freeze-drying was carried out for 36h to obtain the precursor powder;

[0083] (2) Under the protection of 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 black powder;

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

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 for 30 minutes to obtain solution A. Dissolve 1300 mg of dimethylimidazole in 50 mL of deionized water at room temperature for 30 minutes with stirring In water, solution B was obtained, and then solution A and solution B were stirred and mixed at 80 °C for 1 hour, then left to age at 80 °C for 8 hours, centrifuged, and the precipitate was filtered and washed with deionized water for 4 times. Freeze-drying for 24h at -20°C to obtain precursor powder;

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

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

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Abstract

A preparation method of an N-doped carbon polyhedral catalyst supporting Mn single atoms, comprising the following steps: (1) Stirring and dissolving manganese salt and zinc nitrate in a solvent to obtain solution A, stirring and dissolving an N-containing organic ligand in In the solvent, get solution B, then stir and mix solution A and solution B, let it stand for aging, centrifuge, filter and wash, freeze-dry; (2) conduct a heat treatment under the protection of an inert atmosphere; (3) disperse in manganese salt solution, stirred, and freeze-dried; (4) Under the protection of an inert atmosphere, a second heat treatment is performed to obtain an N-doped carbon polyhedral catalyst supporting Mn single atoms. The catalyst obtained by the method of the present invention is well dispersed and metal Mn is dispersed at the atomic level, Mn, N, and C elements are evenly distributed, the electrocatalytic oxygen reduction performance is good, the rate performance is better than that of commercial Pt / C catalysts, and the synthesis process is simple, efficient, and low in cost. The utility model has strong versatility and is suitable for industrialized 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 loaded with Mn single atoms. Background technique [0002] Single-atom catalysts (SACs) are a frontier of catalysis science in recent years. The reduction of active species from particles to single atoms is an effective strategy to improve catalytic performance. exposure, increasing the number of active sites; on the other hand, it is possible to utilize effects such as enhanced interaction and charge transfer between single atoms and carriers to enhance the intrinsic activity of active sites. 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 active SACs remains a great challenge. At present, strategies for synthesizing SACs mainly include defect engineering, spatia...

Claims

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Application Information

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Patent Type & Authority Patents(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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