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Preparation method of fullerene/tetraphenylferriporphyrin self-assembled structure oxygen reduction electrocatalyst

A technology of tetraphenyl iron and electrocatalyst, which is applied in structural parts, electrodes, circuits, etc., can solve the problems of high cost, poor stability, HER and OER catalysis are not as good as Pt, etc., and achieve self-assembly with complete morphology and low production cost , evenly distributed effect

Active Publication Date: 2021-12-17
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The current noble metal platinum-based electrocatalysts with excellent performance can significantly increase the reaction rate of HER and ORR, but the catalysis of the OER process is very limited, while the ruthenium-based and iridium-based catalysts have high catalytic activity for OER, but not for HER and OER. Not as good as Pt / C
In addition, noble metal catalysts suffer from the shortcomings of small reserves, high cost, and poor stability, which cannot meet large-scale commercial applications.

Method used

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  • Preparation method of fullerene/tetraphenylferriporphyrin self-assembled structure oxygen reduction electrocatalyst
  • Preparation method of fullerene/tetraphenylferriporphyrin self-assembled structure oxygen reduction electrocatalyst
  • Preparation method of fullerene/tetraphenylferriporphyrin self-assembled structure oxygen reduction electrocatalyst

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Experimental program
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Effect test

Embodiment 1

[0026] 1) Preparation of metalloporphyrin: Take 1 mole of tetraphenylporphyrin, 5.4 moles of ferric nitrate nonahydrate and 80 mL of DMF solvent, stir evenly under a nitrogen atmosphere, heat up to 100 ° C and reflux for 6 hours. After the reaction is completed, Naturally cool to room temperature, then add 80mL of ultrapure water to it and let stand for 12h, filter with suction, wash with isopropanol, and dry in vacuum at 60°C for 8h to obtain tetraphenyliron porphyrin;

[0027] 2) Preparation of self-assembled structure: take fullerene C at a mass ratio of 1:1 60 and tetraphenyliron porphyrin were poured into beakers respectively, and 1mg / mL fullerene toluene solution and 0.6mg / mL tetraphenyliron porphyrin suspension in isopropanol were prepared, and the two beakers were covered with a layer After the plastic wrap, put it into an ultrasonic machine for ultrasonic dissolution and dispersion;

[0028] 3) Filter the fullerene toluene solution that has been ultrasonically disper...

Embodiment 2

[0035] 1) Preparation of metalloporphyrin: take 1 mole of tetraphenylporphyrin, 12.8 moles of ferric nitrate nonahydrate and 90 mL of DMF solvent, stir evenly under a nitrogen atmosphere, heat up to 110 ° C and reflux for 6 hours. After the reaction is completed, Naturally cool to room temperature, then add 135mL of ultrapure water and let it stand for 24h, filter with suction, wash with isopropanol, and dry in vacuum at 60°C for 8h to obtain tetraphenyliron porphyrin;

[0036] 2) Preparation of self-assembled structure: take fullerene C at a mass ratio of 1:2 60 and tetraphenyliron porphyrin into beakers respectively, prepare 1.5 mg / mL fullerene toluene solution and 1 mg / mL tetraphenyl iron porphyrin suspension in isopropanol, and cover the two beakers with a layer After the plastic wrap, put it into an ultrasonic machine for ultrasonic dissolution and dispersion;

[0037] 3) Filter the fullerene toluene solution that has been ultrasonically dispersed using a needle filter, ...

Embodiment 3

[0041] 1) Preparation of metalloporphyrin: Take 1 mole of tetraphenylporphyrin, 14 moles of ferric nitrate nonahydrate and 100 mL of DMF solvent, stir evenly under a nitrogen atmosphere, heat up to 120 ° C, condense and reflux for 6 hours, and wait for the reaction to complete Naturally cool to room temperature, then add 200mL of ultrapure water and let it stand for 24h, filter with suction, wash with isopropanol, and dry in vacuum at 80°C for 10h to obtain tetraphenyliron porphyrin;

[0042] 2) Preparation of self-assembled structure: take fullerene C at a mass ratio of 1:3 60 and tetraphenyliron porphyrin into beakers respectively, prepare 2mg / mL fullerene toluene solution, 2mg / mL tetraphenyliron porphyrin suspension in isopropanol, and cover the two beakers with a fresh-keeping layer Put the film into an ultrasonic machine for ultrasonic dissolution and dispersion;

[0043] 3) Filter the fullerene toluene solution that has been ultrasonically dispersed using a needle filte...

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Abstract

The invention relates to a preparation method of a fullerene / tetraphenyl ferriporphyrin self-assembled structure oxygen reduction electrocatalyst. The preparation method comprises the following steps: carrying out condensation reflux on tetraphenyl porphyrin, iron nitrate nonahydrate and a DMF solvent, and carrying out vacuum drying to obtain tetraphenyl ferriporphyrin; preparing a fullerene toluene solution, mixing the fullerene toluene solution with the isopropyl alcohol suspension of tetraphenyl ferriporphyrin, performing standing, carrying out suction filtration, washing, and carrying out vacuum drying to obtain a sample with a self-assembly structure; taking a self-assembled sample and flatly spreading in a magnetic boat, putting the magnetic boat into a quartz tube protected by hydrogen and argon mixed gas, performing a heat preservation reaction at the temperature of 600-800 DEG C, performing natural cooling to the room temperature, and obtaining the fullerene / tetraphenylferriporphyrin self-assembled structure oxygen reduction electrocatalyst. The process for preparing the C60 / FeTPP self-assembly structure through a liquid-liquid interface precipitation method is mature, simple to operate, low in production cost and easy for industrial production. A donor-acceptor system with charge transfer can be effectively constructed, and the half-wave potential of the donor-acceptor system can reach 0.86 V (vs.RHE).

Description

technical field [0001] The invention belongs to the technical field of energy catalysis, and in particular relates to a preparation method of a fullerene / tetraphenyliron porphyrin self-assembled structure oxygen reduction electrocatalyst Background technique [0002] With the rapid development of economy, people's dependence on energy is getting higher and higher. However, the storage capacity of traditional fossil energy is decreasing, which makes the problem of energy shortage increasingly prominent. Therefore, the development of renewable energy has received great attention. Based on the above reasons, efficient energy conversion and storage devices have become a research hotspot in this field. [0003] Among electrochemical devices that have been widely studied at present, the performance of metal-air batteries (such as zinc-air batteries) is mainly determined by oxygen reduction reaction (ORR) and oxygen evolution reaction (OER); the performance of electrolytic water de...

Claims

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Application Information

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IPC IPC(8): C25B11/095C25B1/04H01M4/90
CPCC25B11/095C25B1/04H01M4/9008Y02E60/50
Inventor 曹丽云王海冯永强黄剑锋陈俊生冯伟航胡郁竹雒甜蜜
Owner SHAANXI UNIV OF SCI & TECH
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