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Non-precious metal-nitrogen-carbon type oxygen reduction catalyst and preparation method thereof

A non-precious metal and catalyst technology, which is applied in the direction of electrical components, battery electrodes, circuits, etc., can solve the problems of difficult control of the process conditions in the preparation process, complex catalyst preparation methods, unfavorable catalyst industrialization, etc., and achieve excellent stability and methanol resistance. , good ORR catalytic activity, beneficial to the effect of diffusion transfer

Inactive Publication Date: 2017-07-04
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Most of the above-mentioned catalyst preparation methods are relatively complicated, and the process conditions in the preparation process are not easy to control, which is not conducive to the industrialization of catalysts.

Method used

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  • Non-precious metal-nitrogen-carbon type oxygen reduction catalyst and preparation method thereof
  • Non-precious metal-nitrogen-carbon type oxygen reduction catalyst and preparation method thereof
  • Non-precious metal-nitrogen-carbon type oxygen reduction catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

preparation example

[0066] Synthesis of tripyrrole-[1,3,5]-triazine (TPT):

[0067] 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

[0069] (1) Synthesis of P(TPT): Dissolve 110g (0.4mol) tripyrrole-[1,3,5]-triazine (TPT) in 2000mL nitrobenzene, then add 18.26g (0.24mol) dimethoxy Methyl methane and 32.28g (0.24mol) of anhydrous aluminum trichloride, stirred at 45°C for 5h, then raised to 80°C and stirred for 19h; after the reaction was completed, poured into 10L methanol for sedimentation, filtered, washed with water (1000mL×2), and dried Standby; The infrared spectrogram of polymer P (TPT) is shown as figure 1 shown;

[0070] The partial structure (i.e. repeating unit) of the polymer is as follows:

[0071] where n=1;

[0072] (2) Add 2.5g of P(TPT) and 0.7g of ferric nitrate (or ferric chloride) into 300mL of ethanol, ultrasonically disperse the whole system for 180min, then evaporate the ethanol to dryness, place in a vacuum oven at 80°C Dry for 4 hours;

[0073] (3) Gained 3.2g powdery solid in N 2 Heat treatment at 800°C for 1 hour in the atmosphere to obtain 0.97g of nitrogen-doped carbon mate...

Embodiment 2

[0083] (1) Synthesis of P(TPT): Dissolve 110g (0.4mol) tripyrrole-[1,3,5]-triazine (TPT) in 2000mL nitrobenzene, then add 24g (0.24mol) dichloroethane and 32.28g (0.24mol) of anhydrous aluminum trichloride, stirred at 45°C for 5h, then raised to 80°C and stirred for 19h; after the reaction was completed, poured into 10L of methanol for settling, filtered, washed with water (1000mL×2), and dried for later use; The infrared spectrum of polymer P(TPT) is as follows figure 1 shown;

[0084] (2) Add 2.5g of P(TPT) and 0.7g of ferric chloride to 300mL of ethanol, ultrasonically disperse the whole system for 180min, then evaporate the ethanol to dryness, place it in a vacuum oven and dry at 80°C for 4h to obtain primary mixture;

[0085] (3) Gained 3.2g powdery solid in N 2 Heat treatment at 800°C for 1 hour in the atmosphere to obtain 0.98g of nitrogen-doped carbon material;

[0086] (4) The obtained nitrogen-doped carbon material was washed with 2000mL 0.5M dilute sulfuric acid...

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Abstract

The invention discloses an M-N-C oxygen reduction catalyst and a preparation method thereof. The catalyst comprises the following raw materials: a polymer P(TPT) of tripyrrole-[1,3,5]-triazine (TPT) and a non-noble metal salt; and the preparation method comprises the following steps: (1) synthesizing the polymer P(TPT) of tripyrrole-[1,3,5]-triazine (TPT) through a Friedel-Crafts reaction; (2) adding the P(TPT) and the non-noble metal salt to ethanol, putting the mixture in an ultrasonic dispersion instrument and carrying out ultrasonic treatment to make the whole system uniform in dispersion, evaporating the ethanol to dryness, and drying in a vacuum drying oven at 80 DEG C for 4 hours; (3) carrying out first heat treatment to obtain a nitrogen-doped carbon material; (4) fully washing the obtained nitrogen-doped carbon material with dilute acid; and (5) carrying out 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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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/90
CPCH01M4/90Y02E60/50
Inventor 黎华明阳梅陈红飙高勇杨端光
Owner XIANGTAN UNIV
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