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Oxygen reduction catalyst including pyrryl tetrazine ring and preparation method of oxygen reduction catalyst

A technology of pyrrolyl tetrazine epoxy and pyrrolyl tetrazine ring, which is applied in the field of fuel cell science, can solve the problems of unfavorable catalyst industrial preparation, complex catalyst preparation methods, and difficult control of preparation process conditions, etc., so as to facilitate diffusion transfer , Excellent methanol resistance, good ORR catalytic activity

Inactive Publication Date: 2017-06-13
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The above-mentioned catalysts have defects such as complicated preparation methods and difficult control of preparation process conditions, which are not conducive to the industrial preparation of catalysts. Therefore, it is of great significance to develop ORR catalysts with low price, simple preparation process, high activity and strong stability.

Method used

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  • Oxygen reduction catalyst including pyrryl tetrazine ring and preparation method of oxygen reduction catalyst
  • Oxygen reduction catalyst including pyrryl tetrazine ring and preparation method of oxygen reduction catalyst
  • Oxygen reduction catalyst including pyrryl tetrazine ring and preparation method of oxygen reduction catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Example 1 Synthesis of 3,6-bis(pyrrolyl)-1,2,4,5-tetrazine monomer

[0048] Dissolve 1.18 g of pyrrole in 20 mL of dry tetrahydrofuran, add 1.56 g of KOH, and stir for 30 min below 0°C. In addition, the tetrahydrofuran solution containing 3,6-bis(3,5-dimethylpyrazolyl)-1,2,4,5-tetrazine was slowly added dropwise to the above-mentioned pyrrole salt solution, and reacted at room temperature for 1 hour, and then Reflux overnight. Then use petroleum ether and ethyl acetate (12:1) to pass the column, and vacuum dry to constant weight for use. Monomer 3,6-(dipyrrolyl)-1,2,4,5-tetrazine 1 H NMR chart such as figure 1 Shown.

[0049] The reaction of Example 1 is as follows:

[0050]

Embodiment 2

[0051] Example 2 Preparation of oxygen reduction catalyst containing pyrrolyl tetrazine ring

[0052] 1) Synthesis of poly(3,6-dipyrrole-1,2,4,5-tetrazine): 127.2mg of 3,6-bis(pyrrolyl)-1,2,4,5-tetrazine (DPT ) Dissolve in 25mL of 1,2-dichloroethane, add 186.4mg of dimethoxymethane, and finally add 393.9mg of FeCl 3 , React at 45°C for 5h, 80°C for 19h, settle with methanol, wash with methanol several times, finally Soxhlet extraction for 48h, vacuum dry to constant weight. The infrared spectrum of poly(3,6-dipyrrole-1,2,4,5-tetrazine) is as follows figure 2 Shown.

[0053] The synthetic route of poly(3,6-dipyrrole-1,2,4,5-tetrazine) is shown below:

[0054]

[0055] 2) Preparation of oxygen reduction catalyst containing pyrrolyl tetrazine ring: Take 30 mg of the poly(3,6-dipyrrole-1,2,4,5-tetrazine) prepared in step 1) into a porcelain crucible and place it in a tube In the furnace. Under nitrogen atmosphere, from room temperature to 4℃min -1 The heating rate is increased to 900...

Embodiment 3

[0058] 1) Synthesis of poly(3,6-dipyrrole-1,2,4,5-tetrazine): 127.2 mg of 3,6-bis(pyrrolyl)-1,2,4,5-tetrazine (DPT ) Dissolve in 35mL of 1,2-dichloroethane, then add 364.8mg of dimethoxymethane, and finally add 777.6mg of FeCl 3 , React at 30°C for 4h, 90°C for 24h, settle with ethanol, wash with ethanol several times, finally Soxhlet extraction for 24h, and vacuum dry to constant weight.

[0059] 2) Preparation of oxygen reduction catalyst containing pyrrolyl tetrazine ring: Take 30 mg of the poly(3,6-dipyrrole-1,2,4,5-tetrazine) prepared in step 1) into a porcelain crucible and place it in a tube In the furnace. Under nitrogen atmosphere, from room temperature to 5℃min -1 The heating rate is increased to 1000℃, after 1h of constant temperature, and then at 5℃min -1 The temperature drop rate is cooled to room temperature, and the nitrogen-doped carbon material oxygen reduction catalyst containing pyrrolyl tetrazine ring is obtained.

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Abstract

The invention discloses an oxygen reduction catalyst including a pyrryl tetrazine ring and a preparation method of the oxygen reduction catalyst. Monomer (pyrryl)n-1 and 2,4,5-tetrazine (n is 1 or 2) react with a catalyst and an alkylate reagent, a pyrryl tetrazine ring polymer is obtained, the pyrryl tetrazine ring polymer is subjected to thermal treatment in an inert atmosphere, and finally the oxygen reduction catalyst easy to operate, economical, efficient, high in stability and high in catalytic activity is obtained. Industrial production is promoted.

Description

Technical field [0001] The invention relates to a preparation method of an oxygen reduction catalyst, in particular to an oxygen reduction catalyst containing a pyrrolyl tetrazine ring and a preparation method thereof, and belongs to the field of fuel cell science and technology. Background technique [0002] The increase in traditional energy consumption and environmental pollution is a problem that needs to be solved urgently, and the fuel cell (Fuell Cell, FC) is an environmentally friendly and efficient new energy device. Its main function is to convert chemical energy into electrical energy. , Is a relatively green energy device, recognized as the best choice to replace traditional energy. [0003] Oxygen reduction reaction (ORR) is one of the important electrocatalytic reactions, and it is a key step in fuel cells and metal-air batteries. However, fuel cells restrict their rapid development due to their high cost and poor stability. The high cost is mainly because the cathod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/88H01M4/90
CPCH01M4/88H01M4/9008Y02E60/50
Inventor 陈红飙孙滔阳梅刘益江黎华明
Owner XIANGTAN UNIV
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