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Superfine M-N-C non-noble metal carbon-based oxygen reduction catalyst, and preparation method and application thereof

A non-precious metal, catalyst technology, applied in electrical components, battery electrodes, circuits, etc., can solve the problems of difficult to control the size and morphology of oxygen reduction catalysts of MOF materials, easy aggregation of metal active sites, and reduction of catalyst active site density.

Active Publication Date: 2020-11-24
CHINA UNIV OF PETROLEUM (EAST CHINA)
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Problems solved by technology

[0009] In the above patent documents, different precursors are used as raw materials for the preparation of carbon-based oxygen reduction catalysts, but they all have the disadvantages of complicated process and easy aggregation of metal active sites
In particular, the aggregation of active sites will greatly reduce the active site density per unit area of ​​the catalyst, resulting in a decrease in catalyst activity.
[0010] Chinese patent document CN107887616A discloses a novel transition metal-modified redox catalyst and its preparation method, which only uses easily soluble transition metal salts and organic ligands For the reaction, it is difficult to control the rate of the MOF assembly process, which makes it difficult to control the size and shape of the final MOF material and the oxygen reduction catalyst obtained after carbonization, which limits its ORR catalytic performance.
[0012] (1) The prior art uses different precursors as raw materials for the preparation of carbon-based oxygen reduction catalysts, but all of them have the disadvantages of complex process and easy aggregation of metal active sites shortcoming
In particular, the aggregation of active sites will greatly reduce the active site density per unit area of ​​the catalyst, resulting in a decrease in catalyst activity.
[0013](2) The existing technology uses easily soluble transition metal salts and organic ligands to react, it is difficult to control the rate of the MOF assembly process, so that the final MOF material and carbonization The size and shape of the obtained oxygen reduction catalyst are difficult to control, which limits its ORR catalytic performance.
[0014]The difficulty of solving the above problems and defects is: in the current preparation process of M-N-C non-noble metal oxygen reduction catalyst, because the size of the precursor is difficult to control, it is difficult to Realize the precise regulation of the size of M-N-C non-noble metal oxygen reduction catalyst

Method used

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  • Superfine M-N-C non-noble metal carbon-based oxygen reduction catalyst, and preparation method and application thereof
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  • Superfine M-N-C non-noble metal carbon-based oxygen reduction catalyst, and preparation method and application thereof

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preparation example Construction

[0061] Such as figure 1 As shown, the preparation method of the ultrafine M-N-C non-noble metal carbon-based oxygen reduction catalyst provided by the invention comprises the following steps:

[0062] S101: Put transition metal salt and basic zinc acetate in a reaction bottle, add solvent a, stir at room temperature for 20-40 minutes, centrifuge, then wash and dry to obtain binary transition metal basic acetate;

[0063] S102: Place the binary transition metal basic acetate in step S101 in a polytetrafluoroethylene-lined reaction kettle, then add organic ligands, solvent b and additives to the reaction kettle, seal the reaction kettle, and set the temperature at room temperature Stir for 20 to 40 minutes to obtain a suspension of the reactant;

[0064] S103: Place the reactant suspension obtained in step S102 in an oven with temperature control function, react at 80-140°C for 6-72 hours, centrifuge, then filter, wash and dry to obtain transition metal-doped metal-organic fra...

Embodiment 1

[0082] The preparation method of the ultrafine M-N-C non-noble metal carbon-based oxygen reduction catalyst provided by the invention comprises the following steps:

[0083] (1) Put 20mL of cobalt nitrate aqueous solution (2M) and 100mg of basic zinc acetate in a reaction flask, add 1mL of ultrasonically dispersed ethanol, stir at room temperature for 30 minutes, and then centrifuge, wash with methanol, and place at 80°C Dry for 360min to obtain cobalt-doped basic zinc acetate;

[0084] (2) Place 30 mg of cobalt-doped basic zinc acetate in step (1) in a 20 mL polytetrafluoroethylene-lined reactor, and then add 100 mg of 2-methylimidazole, 5 mL of DMF, and 1 mL of Ionized water and 2mL triethylamine, seal the reaction kettle, stir at room temperature for 30 minutes to obtain a reactant suspension;

[0085] (3) Place the reactant suspension obtained in step (2) in an oven with temperature control function, react at 100°C for 12 hours, centrifuge, then filter, wash with ethanol,...

Embodiment 2

[0088] The preparation method of the ultrafine M-N-C non-noble metal carbon-based oxygen reduction catalyst provided by the invention comprises the following steps:

[0089] (1) Put 20mL of ferric nitrate aqueous solution (2M) and 100mg of basic zinc acetate into a reaction flask, add 1mL of ethanol after ultrasonic dispersion, stir at room temperature for 30 minutes, then centrifuge, wash with methanol, and place at 80°C Dry for 360min to obtain iron-doped basic zinc acetate;

[0090] (2) Place 30 mg of iron-doped basic zinc acetate in step (1) in a 20 mL polytetrafluoroethylene-lined reactor, and then add 100 mg of 2-methylimidazole, 5 mL of DMF, and 1 mL of Ionized water and 2mL triethylamine, seal the reaction kettle, stir at room temperature for 30 minutes to obtain a reactant suspension;

[0091] (3) Place the reactant suspension obtained in step (2) in an oven with temperature control function, react at 100°C for 12 hours, centrifuge, then filter, wash with ethanol, an...

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Abstract

The invention belongs to the technical field of carbon material chemistry. The invention discloses a superfine M-N-C non-noble metal carbon-based oxygen reduction catalyst, and a preparation method and application thereof. Transition metal basic acetate, N-heterocyclic or carboxylic acid organic ligands are adopted as reactants, a certain amount of solvent and regulator are added, reaction is performed at a certain temperature to obtain a superfine metal-organic framework material, and the superfine non-noble metal carbon-based catalyst is obtained through a one-step carbonization process. Thesuperfine non-noble metal carbon-based catalyst is used as a catalyst for hydrogen fuel cathode oxygen reduction reaction, excellent catalytic activity is obtained, and the activity of the catalyst is superior to that of a commercial platinum-carbon catalyst; and in addition, the stability and methanol poisoning resistance of the catalyst in the oxygen reduction reaction are superior to those ofan existing platinum-carbon catalyst. The superfine non-noble metal carbon-based catalyst can be applied to the fields of hydrogen fuel cells, metal-air batteries and the like.

Description

technical field [0001] The invention belongs to the technical field of carbon material chemistry, and in particular relates to an ultrafine M-N-C non-noble metal carbon-based oxygen reduction catalyst, a preparation method and an application. Background technique [0002] Oxygen reduction reaction (ORR) is a cathodic reaction in efficient energy conversion technologies such as hydrogen fuel cells and metal-air batteries. Compared with the hydrogen oxidation reaction at the anode, the reaction kinetics of the ORR reaction is slower, resulting in a higher overpotential of the hydrogen fuel cell, which hinders the performance of the hydrogen fuel cell. In order to promote the reaction kinetics of the ORR reaction, conventional hydrogen fuel cell devices have widely used the noble metal platinum as the active center catalyst. However, due to the high price of platinum and the low reserves of platinum on the earth, it cannot meet the needs of large-scale promotion and use of hyd...

Claims

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Application Information

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IPC IPC(8): H01M4/90H01M4/88
CPCH01M4/9083H01M4/9008H01M4/88Y02E60/50
Inventor 李良军叶涵刘丹丹顾鑫代鹏程赵学波
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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