Nitrogen-doped carbon-supported non-noble metal (M-N-C) oxygen reduction catalyst and preparation method thereof

A nitrogen-doped carbon, non-precious metal technology, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve the problems of unfavorable catalyst industrialization, complex catalyst preparation methods, and difficult to control the process conditions of the preparation process. and other problems, to achieve excellent stability and methanol resistance, good ORR catalytic activity, and the effect of facilitating diffusion and transfer.

Inactive Publication Date: 2015-12-23
XIANGTAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Most of the above-mentioned catalyst preparation methods are relatively complicated, and the process conditio

Method used

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  • Nitrogen-doped carbon-supported non-noble metal (M-N-C) oxygen reduction catalyst and preparation method thereof
  • Nitrogen-doped carbon-supported non-noble metal (M-N-C) oxygen reduction catalyst and preparation method thereof
  • Nitrogen-doped carbon-supported non-noble metal (M-N-C) oxygen reduction catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

preparation example

[0054] Synthesis of tripyrrole-[1,3,5]-triazine (TPT):

[0055] Add 6.78g (0.10mol) of pyrrole and 80mL of anhydrous tetrahydrofuran into a 250mL single-necked round-bottomed flask, add KOH (8.86g, 0.15mol) into the above system under ice-cooling, rise to room temperature for 3 hours, and divide Add 5.59g (0.03mol) of cyanuric chloride in batches, and continue stirring at room temperature for 18h. After the reaction was completed, the reaction system was poured into a 250mL ice-water bath to settle, filtered, washed with deionized water three times (200mL×3), and then dried in a vacuum oven at 80°C for 24h. The obtained crude product was recrystallized with 15 mL of acetone and ethanol mixed solvent (acetone: ethanol ratio of 4:1), filtered, washed with ethanol, and the obtained off-white solid was vacuum-dried at room temperature to constant weight, 4.64 g, yield 56%, melting point: 210 ° C .

Embodiment 1

[0057] (1) Synthesis (P(TPT+Py)): Dissolve 55g (0.2mol) tripyrrole-[1,3,5]-triazine (TPT), 40.6g (0.6mol) pyrrole (Py) in 2000mL nitric acid Add 18.26g (0.24mol) of dimethoxymethane and 32.28g (0.24mol) of anhydrous aluminum trichloride to benzene, stir at 45°C for 5h, then rise to 80°C and stir for 19h; after the reaction is complete, pour Sediment in 10L methanol, filter, wash with water (1000mL×2), and dry for later use; the infrared spectrum of polymer P (TPT+Py) is as follows figure 1 shown;

[0058] The partial structure (i.e. repeating unit) of the polymer is as follows:

[0059]

[0060] (2) Add 2.5g (P(TPT+Py)) and 0.7g ferric trichloride to 300mL ethanol, ultrasonically disperse the whole system for 180min, evaporate the ethanol to dryness, and dry in a vacuum oven at 80°C 4h;

[0061] (3) Gained 3.2g powdery solid in N 2 Heat treatment at 800°C for 1 h in the atmosphere to obtain 0.9 g of nitrogen-doped carbon material;

[0062] (4) The obtained nitrogen-dop...

Embodiment 2

[0071] (1) Synthesis (P(TPT+Py)): Dissolve 55g (0.2mol) tripyrrole-[1,3,5]-triazine (TPT), 40.6g (0.6mol) pyrrole (Py) in 2000mL nitric acid Add 24g (0.24mol) dichloroethane and 32.28g (0.24mol) anhydrous aluminum trichloride to benzene, stir at 45°C for 5h, then rise to 80°C and stir for 19h; after the reaction is complete, pour 10L methanol Settled in medium, filtered, washed with water (1000mL×2), and dried for later use; the infrared spectrum of polymer P (TPT+Py) is as follows figure 1 shown;

[0072] (2) Add 2.5g (P(TPT+Py)) and 0.7g ferric trichloride to 300mL ethanol, ultrasonically disperse the whole system for 180min, evaporate the ethanol to dryness, and dry in a vacuum oven at 80°C 4h, obtain primary mixture;

[0073] (3) Gained 3.2g powdery solid in N 2 Heat treatment at 800°C for 1 hour in the atmosphere to obtain 0.91g of nitrogen-doped carbon material;

[0074] (4) The obtained nitrogen-doped carbon material was washed with 2000mL of 0.5M dilute sulfuric ac...

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Abstract

The invention discloses an M-N-C oxygen reduction catalyst and a preparation method thereof, wherein the raw materials of the catalyst comprise a copolymer (P(TPT+Py)) of tripyrrole-[1,3,5]-triazine (TPT) and pyrrole (Py) and a non-noble metal salt. The preparation method comprises: (1) using a Friedel-Crafts reaction to synthesize a copolymer (P(TPT+Py)) of tripyrrole-[1,3,5]-triazine (TPT) and pyrrole (Py); (2) adding (P(TPT+Py)) and a non-noble metal salt to ethanol, placing into an ultrasonic dispersion device, carrying out an ultrasonic treatment to make the whole system be uniformly dispersed, evaporating the ethanol, placing into a vacuum oven, and drying for 4 h at a temperature of 80 DEG C; (3) carrying out a first heat treatment to obtain a nitrogen-doped carbon material; (4) completely washing the obtained nitrogen-doped carbon material with a diluted acid; and (5) carrying out a second heat treatment so as to obtain the M-N-C oxygen reduction catalyst.

Description

technical field [0001] The invention relates to an oxygen reduction catalyst and a preparation method thereof, specifically an M-N-C oxygen reduction catalyst and a preparation method thereof, belonging to the field of fuel cell science and technology. Background technique [0002] Oxygen reduction reaction (ORR) is one of the most important electrocatalytic reactions and is a very critical process in devices such as fuel cells and metal-air batteries. Platinum and platinum-based catalysts are currently the most active and most commonly used ORR catalysts, but they are expensive, limited resources, and poor stability in long-term operation, which seriously hinder the development of fuel cells and other related fields. Therefore, the research and development of non-precious metal catalysts with high activity and high stability is of great significance for reducing the cost of fuel cells and accelerating their commercialization. [0003] It is undoubtedly promising to replace...

Claims

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Application Information

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IPC IPC(8): B01J27/24H01M4/90
CPCY02E60/50
Inventor 黎华明阳梅陈红飙高勇杨端光
Owner XIANGTAN UNIV
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