Preparation method for nitrogen-doped carbon oxygen reduction catalyst with hierarchical porous structure

A nitrogen-doped carbon and catalyst technology, applied in structural parts, electrical components, battery electrodes, etc., can solve the problem that non-precious metal catalyst activity is difficult to meet the commercialization requirements of fuel cells, achieve excellent oxygen reduction catalytic activity, and the method is simple and easy. The effect of the line, the production cost is low

Active Publication Date: 2015-12-23
重庆铈坦新材料技术研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a method for preparing a nitrogen-doped carbon-oxygen reduction catalyst with a hierarchical porous structure in view of the fact that the activity of the existing non-precious metal catalysts is difficult to meet the commercialization requirements of fuel cells

Method used

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  • Preparation method for nitrogen-doped carbon oxygen reduction catalyst with hierarchical porous structure
  • Preparation method for nitrogen-doped carbon oxygen reduction catalyst with hierarchical porous structure
  • Preparation method for nitrogen-doped carbon oxygen reduction catalyst with hierarchical porous structure

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Effect test

Embodiment 1

[0033] The specific method steps of a nitrogen-doped carbon-oxygen reduction catalyst with a hierarchical porous structure include:

[0034] (1) Preparation of deep eutectic salt template

[0035] Lithium chloride and sodium chloride are weighed according to the mass ratio of lithium chloride: sodium chloride is 1:0.1, dispersed with ultrapure water to form an aqueous solution with a mass concentration of 80g / L, then put into an ultra-low temperature refrigerator to freeze, and finally Freeze-dry in a freeze dryer to obtain a deep eutectic salt template.

[0036] (2) Solid phase polymerization

[0037] The eutectic salt prepared by step (1): aniline: ferric chloride: the mass ratio of ammonium persulfate is 1: 0.08: 0.25: 0.15 takes by weighing eutectic salt, aniline, ferric chloride and ammonium persulfate, and then With absolute ethanol as solvent, aniline, ferric chloride and ammonium persulfate were dissolved in absolute ethanol respectively to form aniline solution with...

Embodiment 2

[0045] The specific method steps of a nitrogen-doped carbon-oxygen reduction catalyst with a hierarchical porous structure include:

[0046] (1) Preparation of deep eutectic salt template

[0047] Lithium chloride: sodium chloride is weighed according to the mass ratio of lithium chloride: sodium chloride to be 1: 2.5, dispersed with ultrapure water to form an aqueous solution with a mass concentration of 30g / L, then put into an ultra-low temperature refrigerator to freeze, and finally Freeze-dry in a freeze dryer to obtain a deep eutectic salt template.

[0048] (2) Solid phase polymerization

[0049] The eutectic salt prepared by step (1): o-phenylenediamine: iron sulfate: the mass ratio of ammonium persulfate is 1: 0.05: 0.05: 0.1 Weigh the eutectic salt, o-phenylenediamine, iron sulfate and persulfate Ammonium sulfate, then with dehydrated alcohol as solvent, o-phenylenediamine, ferric sulfate and ammonium persulfate are dissolved in dehydrated alcohol respectively to fo...

Embodiment 3

[0055] The specific method steps of a nitrogen-doped carbon-oxygen reduction catalyst with a hierarchical porous structure include:

[0056] (1) Preparation of deep eutectic salt template

[0057] The mass ratio of lithium chloride: sodium chloride is 1:5 to take lithium chloride: sodium chloride, disperse it with ultrapure water to form an aqueous solution with a mass concentration of 11g / L, then put it into an ultra-low temperature refrigerator to freeze, and finally Freeze-dry in a freeze dryer to obtain a deep eutectic salt template.

[0058] (2) Solid phase polymerization

[0059] The eutectic salt prepared by step (1): p-phenylenediamine: ferric nitrate: the mass ratio of ammonium persulfate is 1: 0.01: 0.01: 0.015. Weigh eutectic salt, p-phenylenediamine, ferric nitrate and persulfate Ammonium sulfate, then using absolute ethanol as a solvent, p-phenylenediamine, ferric nitrate and ammonium persulfate are dissolved in absolute ethanol respectively to form a p-phenylen...

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Abstract

The invention provides a preparation method for a nitrogen-doped carbon oxygen reduction catalyst with a hierarchical porous structure, belonging to the technical field of a fuel cell. The preparation method comprises the following steps of: firstly, preparing a eutectic molten salt having a three-dimensional macro-porous structure by a freeze drying method; secondly, using the eutectic molten salt as a template, doping a nitrogen-containing precursor, and leading the nitrogen-containing precursor to be oxidized and polymerized on the surface of the eutectic molten salt by a solid-phase polymerization method, wherein ammonium persulfate serves as an oxidizing agent, and a ferric salt serves as a promoter; and finally, carrying out high-temperature pyrolysis and removing the eutectic molten salt. With the adoption of the nitrogen-doped carbon oxygen reduction catalyst with the hierarchical porous structure, the nitrogen-containing precursor can be effectively prevented from pyrolysis loss, structural collapse and sintering during the high-temperature carbonation process, the catalyst yield and the nitrogen doping efficiency are improved, moreover, a large amount of micropores, mesoporous and macropores can be generated, and the mass transfer efficiency of oxygen and water is improved. The method is simple and practical, the production cost is low, and the prepared catalyst has excellent oxygen reduction catalytic activity and can substitute the traditional commercial Pt/C catalyst.

Description

Technical field: [0001] The invention belongs to the technical field of fuel cells, in particular to a preparation method of a nitrogen-doped carbon-oxygen reduction catalyst with a hierarchical porous structure. Background technique: [0002] Fuel cells have the advantages of high energy conversion efficiency, environmental friendliness, and rapid start-up at room temperature, and are considered to be the most promising chemical power sources for electric vehicles and other civilian applications in the future. In the process of fuel cell industrialization, its cost and life problems have always been the core issues that plague its development. At present, the main reason for the high cost of fuel cells is the extensive use of noble metal Pt. Due to the high price of Pt and the scarcity of resources, the development of low-cost and excellent performance low-temperature fuel cell cathode non-precious metal catalysts has become the focus of current research on fuel cell cataly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/88
CPCH01M4/8814H01M4/8842Y02E60/50
Inventor 魏子栋李佳陈四国吴睿丁炜李莉
Owner 重庆铈坦新材料技术研究院有限公司
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