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Preparation method of ordered mesoporous non-noble-metal-nitrogen-graphitized carbon material

A non-precious metal and graphitized carbon technology, applied in chemical instruments and methods, chemical/physical processes, physical/chemical process catalysts, etc., can solve problems such as reducing the optimal amount of metal used, reducing the nitrogen density of materials, etc., to achieve superior catalysis Effects of stability and methanol resistance, good electrical conductivity, and good dispersibility

Inactive Publication Date: 2013-08-21
EAST CHINA NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although these methods can increase the specific surface area of ​​the material, the presence of the carrier inevitably confines the metal-nitrogen-carbon material to the surface of the material, limits the loading of the metal-nitrogen-carbon material with catalytic activity, reduces the overall nitrogen density of the material, and reduces The optimal amount of metal used (the optimal amount is generally only 2-5%)

Method used

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  • Preparation method of ordered mesoporous non-noble-metal-nitrogen-graphitized carbon material
  • Preparation method of ordered mesoporous non-noble-metal-nitrogen-graphitized carbon material
  • Preparation method of ordered mesoporous non-noble-metal-nitrogen-graphitized carbon material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] a. Synthesis of Metalloporphyrins

[0034] Add 4 g of tetrapyridyl porphyrin and 1.54 g of cobalt chloride into 150 mL of absolute ethanol, reflux at 50° C. for 6 h, and ethanol recrystallize.

[0035] b. Synthesis of filling materials

[0036] Add 1g of cobalt porphyrin to a mixed solution of 10mL of glacial acetic acid and 10mL of deionized water, stir to dissolve, add 1g of two-dimensional mesoporous silica SBA-15, and keep stirring until dry at room temperature; then, keep the temperature at 60°C After drying, the metal complex is filled into the mesoporous channel material.

[0037] c. High temperature roasting of filling materials

[0038] The obtained filling material was placed in a quartz tube, heated at 600°C in a 40ml / min pure nitrogen atmosphere, and kept for 3 hours to carbonize the filling material to obtain a black powder.

[0039] d. Removal of hard template mesoporous silica

[0040] The black powder prepared above was stirred with 25% hydrofluoric ...

Embodiment 2

[0042] a. Synthesis of Metalloporphyrins

[0043] Add 4g of tetrapyridyl porphyrin and 1.05g of anhydrous ferric chloride into 150mL of absolute ethanol, reflux at 55°C for 6h, and recrystallize the ethanol.

[0044] b. Synthesis of filling materials

[0045] Add 1g of iron porphyrin to 10mL of glacial acetic acid and 20mL of deionized water mixed solution, stir to dissolve, add 0.5g of two-dimensional mesoporous silica SBA-15, and keep stirring until dry at room temperature; then, keep the temperature at 60°C After drying, the metal complex is filled into the mesoporous channels.

[0046] c. High temperature roasting of filling materials

[0047] The obtained filling material was placed in a quartz tube, heated at 700° C. in a 40 ml / min pure nitrogen atmosphere, and kept for 3 hours to carbonize the filling material to obtain a black powder.

[0048] d. Removal of hard template mesoporous silica

[0049] The black powder prepared above was stirred with 25% hydrofluoric ac...

Embodiment 3

[0051] a. Synthesis of Metalloporphyrins

[0052] Add 4g of tetrapyridyl porphyrin and 1.02g of chromium chloride into 150mL of absolute ethanol, reflux at 55°C for 7h, and recrystallize from ethanol.

[0053] b. Synthesis of filling materials

[0054] Add 1g of chromium porphyrin to a mixed solution of 10mL of glacial acetic acid and 30mL of deionized water, stir to dissolve, add 0.35g of two-dimensional mesoporous silica SBA-15, and keep stirring until dry at room temperature; then, at 60°C Dry at constant temperature to obtain metal complexes to fill the mesoporous channels.

[0055] c. High temperature roasting of filling materials

[0056] The obtained filling material was placed in a quartz tube, heated at 700°C in a 40ml / min pure nitrogen atmosphere, and kept for 4 hours to carbonize the filling material to obtain a black powder.

[0057] d. Removal of hard template mesoporous silica

[0058] Stir the 25% hydrofluoric acid solution for the black powder prepared ab...

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Abstract

The invention discloses a preparation method of an ordered mesoporous non-noble-metal-nitrogen-graphitized carbon material. According to the method, mesoporous silicon oxide is used as a hard template, metalloporphyrin is used as a precursor, and then the ordered mesoporous non-noble-metal-nitrogen-graphitized carbon material is prepared through nano-pouring and high temperature roasting of the hard template. High specific surface area and good dispersibility are maintained while the material prepared by the invention has high nitrogen density; and the aperture size is adjustable, and regular pore passage structures are beneficial to material transfer inside electrodes, so that the catalytic active site density is greatly improved. Compared with traditional cathode materials of a fuel cell, the ordered mesoporous non-noble-metal-nitrogen-graphitized carbon material prepared by the invention has the advantages of good catalytic performance, low cost and good stability, a cross effect of a direct methanol fuel cell is prevented, and the preparation method has a good business prospect.

Description

technical field [0001] The invention relates to the synthesis technology of mesoporous materials prepared by a hard template method and the field of fuel cell electrocatalysts, in particular to a method for preparing ordered mesoporous non-noble metal-nitrogen-graphitized carbon materials; High electrocatalytic activity, mainly used in the cathode part of the fuel cell. Background technique [0002] With the progress of society and the development of human civilization, the consumption of energy in today's world has increased sharply, making the fossil energy that serves as the driving force of today's society frequently run out, and the price continues to rise, while human demand for resources continues to increase. Originally, the use of nuclear energy can relieve the pressure on fossil energy, but frequent nuclear accidents make people fearful. However, a fuel cell is a renewable and clean energy that continuously converts chemical energy into electrical energy. It can p...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J35/10H01M4/90
CPCY02E60/50
Inventor 单永奎孔爱国朱小方孔莹莹邢芳严莉丽
Owner EAST CHINA NORMAL UNIVERSITY
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