Method for synthesizing nitrogen-carbon nonmetal reducing catalyst by utilizing concentrated sulfuric acid carbonization

A carbon sulfate, chemical synthesis technology, applied in physical/chemical process catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve the problem of nitrogen active site loss, difficult to activate nitrogen, affecting oxygen reduction catalytic activity and other problems , to avoid nitrogen loss and improve the catalytic activity of oxygen reduction

Inactive Publication Date: 2013-07-24
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, simply subjecting nitrogen and carbon sources to high-temperature graphitization heat treatment will cause a large number of nitrogen active sites to be lost, making it difficult for active nitrogen to exert its ultimate effect, which in turn affects the oxygen reduction catalytic activity of nitrogen-carbon composites.

Method used

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  • Method for synthesizing nitrogen-carbon nonmetal reducing catalyst by utilizing concentrated sulfuric acid carbonization
  • Method for synthesizing nitrogen-carbon nonmetal reducing catalyst by utilizing concentrated sulfuric acid carbonization
  • Method for synthesizing nitrogen-carbon nonmetal reducing catalyst by utilizing concentrated sulfuric acid carbonization

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Add 4g sucrose and 2g melamine into a 400 mL beaker, mix and stir evenly, then add 20 mL of concentrated sulfuric acid with a mass concentration of 98% dropwise; then put it into an autoclave, and carbonize at 120°C for 10 h at a time; wait until the reaction is complete Then filter with suction, wash and dry. The obtained product was carbonized at a high temperature of 600 °C for 2 h under the protection of nitrogen to obtain a nitrogen-carbon composite non-metallic oxygen reduction catalyst material.

[0026] It is found by oxygen reduction test that on the electrode of the composite carbon material prepared by the present invention, the onset potential and the half-wave potential of the oxygen reduction reaction are respectively positively shifted by 49 mV and 30 mV compared with the catalyst prepared by the traditional heat treatment method; The XC-72 toner is positively shifted by 110 mV and 68 mV.

Embodiment 2

[0028] Add 4g of sucrose and 2g of melamine into a 400 mL beaker, mix and stir evenly, then add 20 mL of concentrated sulfuric acid with a mass concentration of 98% dropwise; Suction filtration, washing, and drying; the obtained product was subjected to secondary carbonization treatment at 800° C. for 2 h under the protection of nitrogen to obtain a non-metallic oxygen reduction catalyst material.

[0029] It is found by oxygen reduction test that on the electrode of the composite carbon material prepared by the present invention, the onset potential and the half-wave potential of the oxygen reduction reaction are respectively positively shifted by 59 mV and 36 mV compared with the catalyst prepared by the traditional heat treatment method; The XC-72 toner is positively shifted by 128 mV and 81 mV.

Embodiment 3

[0031] Add 4 g of inositol and 1 g of melamine into a 400 mL beaker, mix and stir evenly, then add 20 mL of concentrated sulfuric acid with a mass concentration of 98% dropwise, then put it into an autoclave, and carbonize at 120°C for 10 h at a time. After completion, suction filtration, washing, and drying; the obtained product was further carbonized at a high temperature of 600 °C for 2 h under the protection of nitrogen to obtain a non-metallic oxygen reduction catalyst material.

[0032] It is found by oxygen reduction test that on the electrode of the composite carbon material prepared by the present invention, the onset potential and the half-wave potential of the oxygen reduction reaction are respectively positively shifted by 42 mV and 29 mV compared with the catalyst prepared by the traditional heat treatment method; The XC-72 toner is positively shifted by 92 mV and 43 mV.

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Abstract

The invention provides a method for synthesizing a nitrogen-carbon compound nonmetal reducing catalyst by utilizing concentrated sulfuric acid carbonization. The method utilizing an organic compound containing carbon, hydrogen and oxygen as a carbon source and utilizing melamine as a nitrogen source comprises the following steps of: preliminarily carbonizing the hydrogen and the oxygen in the organic compound containing the carbon, the hydrogen and the oxygen by utilizing dehydration characteristic of the concentrated sulfuric acid, so that the melamine enters a duct of the preliminary carbonizing product, and the nitrogen source is effectively fixed; carrying out high-temperature deep carbonization under the protection of the nitrogen gas to obtain a compound material which is effectively combined with the nitrogen and the carbon, so that the active nitrogen with the effect of promoting oxygen reduction catalysis has a good effect, and therefore, a nitrogen loss problem generated by the conventional high-temperature treatment method is avoided, and the oxygen reduction catalysis activity of the nitrogen-carbon composite material is effectively improved.

Description

technical field [0001] The invention belongs to the technical field of composite materials, and relates to a preparation method of a nitrogen-carbon composite non-metallic oxygen reduction catalyst, in particular to a method for synthesizing a nitrogen-carbon composite non-metallic oxygen reduction catalyst by carbonization of concentrated sulfuric acid. Background technique [0002] As an environmentally friendly energy utilization technology, fuel cells can directly convert chemical energy into electrical energy, and have been widely concerned. However, because it mainly uses platinum-containing catalysts, the cost is relatively high, which seriously restricts the development and commercialization of fuel cell technology. Therefore, the development of non-precious metal and non-metal catalysts has become the most important research topic in the field of fuel cells. [0003] Studies have found that carbon materials with high nitrogen content have good oxygen reduction cata...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24H01M4/90
CPCY02E60/50
Inventor 王荣方马妍姣王辉季山
Owner NORTHWEST NORMAL UNIVERSITY
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