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Nitrogen and sulfur co-doped carbon-loaded non-noble metal type oxygen reduction catalyst and preparation method thereof

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

Inactive Publication Date: 2015-10-28
XIANGTAN UNIV
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  • Summary
  • 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 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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  • Nitrogen and sulfur co-doped carbon-loaded non-noble metal type oxygen reduction catalyst and preparation method thereof
  • Nitrogen and sulfur co-doped carbon-loaded non-noble metal type oxygen reduction catalyst and preparation method thereof
  • Nitrogen and sulfur co-doped carbon-loaded non-noble metal type oxygen reduction catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

preparation example

[0064] Synthesis of tripyrrole-[1,3,5]-triazine (TPT):

[0065] 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

[0067] (1) Synthesis (P(TPT+Tp)): 55g (0.2mol) tripyrrole-[1,3,5]-triazine (TPT), 50.5g (0.6mol) thiophene (Tp) were dissolved 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 Settled in 10L methanol, filtered, washed with water (1000mL×2), and dried for later use; the infrared spectrum of polymer P (TPT+Tp) was as follows figure 1 shown.

[0068] The partial structure (i.e. repeating unit) of the polymer is as follows:

[0069] where n=1;

[0070] (2) Add 2.5g (P(TPT+Tp)) and 0.7g ferric chloride 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;

[0071] (3) Gained 3.2g powdery solid in N2 Heat treatment at 900°C for 1 h in the atmosphere to obtain 0.9 g of nitrogen-doped carbon material;

[0072] (4) The o...

Embodiment 2

[0081] (1) Synthesis (P(TPT+Tp)): 55g (0.2mol) tripyrrole-[1,3,5]-triazine (TPT), 50.5g (0.6mol) thiophene (Tp) were dissolved 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 Settling in medium, filtering, washing with water (1000mL×2), drying for later use; the infrared spectrum of polymer P (TPT+Tp) is as follows figure 1 shown;

[0082] (2) Add 2.5g (P(TPT+Tp)) and 0.7g ferric chloride into 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;

[0083] (3) Gained 3.2g powdery solid in N 2 Heat treatment at 800°C for 1 hour in the atmosphere to obtain 0.95g of nitrogen-doped carbon material;

[0084] (4) The obtained nitrogen-doped carbon material was washed with 2000mL 0.5M dilute sulfuri...

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Abstract

The invention discloses a nitrogen and sulfur co-doped carbon-loaded non-noble metal type oxygen reduction catalyst and a preparation method thereof and discloses a M-N-S-C oxygen reduction catalyst and a preparation method thereof. The raw materials of the catalyst comprise copolymer P (TPT+Tp) of tripyrrole-[1,3,5]-triazine (TPT) and thiophene (Tp) and non-noble metal salt. The preparation method of the catalyst includes the following steps that firstly, a Friedel-Crafts reaction is adopted for synthesizing the copolymer P (TPT+Tp) of the tripyrrole-[1,3,5]-triazine (TPT) and the thiophene (Tp); secondly, the P (TPT+Tp) and the non-noble metal salt are added into ethanol, mixtures are placed in an ultrasonic dispersing instrument, a whole system is evenly dispersed due to ultrasound, and then the ethanol is dried by distillation and placed in a vacuum drying box to be dried for 4 h at the temperature of 80 DEG C; thirdly, thermal treatment is performed for the first time and nitrogen doped materials are obtained; fourthly, the nitrogen doped materials are completely washed through dilute acid; fifthly, thermal treatment is performed for the second time, and then the M-N-C oxygen reduction catalyst can be obtained.

Description

technical field [0001] The invention relates to an oxygen reduction catalyst and a preparation method thereof, specifically an M-N-S-C oxygen reduction catalyst and a preparation method thereof, and belongs 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 rep...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24H01M4/90H01M4/88
CPCY02E60/50
Inventor 黎华明阳梅陈红飙高勇杨端光
Owner XIANGTAN UNIV
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