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Preparation method and application of nitrogen-doped MXene loaded cobalt phthalocyanine composite material

A composite material and nitrogen-doped technology, which is applied in the field of preparation of nitrogen-doped MXene functionalized composite materials and nitrogen-doped MXene-loaded cobalt phthalocyanine composite materials, can solve the problem of difficult determination of carbonization degree, easy generation of harmful gases, and influence on catalysis Activity and other issues, to achieve the effect of increasing catalytic active sites, good oxygen reduction catalytic activity, and reducing charge transfer resistance

Active Publication Date: 2022-04-15
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, high-temperature calcination is generally used in the preparation of nitrogen-doped MXene, which not only consumes a lot of energy, but also is more complicated to operate, and it is easy to generate harmful gases
It is in a carbonized state during preparation, and the degree of carbonization is not easy to determine, resulting in material deformation and reduction of carbon defects, which affects its catalytic activity and has certain limitations.

Method used

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  • Preparation method and application of nitrogen-doped MXene loaded cobalt phthalocyanine composite material
  • Preparation method and application of nitrogen-doped MXene loaded cobalt phthalocyanine composite material
  • Preparation method and application of nitrogen-doped MXene loaded cobalt phthalocyanine composite material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1. Synthesis of MXenes with F-terminal groups

[0034] Pour 10ml of 40% HF solution into the beaker and add 1g of Ti 3 AlC 2 The powder (200 mesh) was stirred at 25°C for 24 hours, washed by centrifugation with deionized water, filtered and dried for 12 hours to obtain MXene.

[0035]2. Preparation of nitrogen-doped MXene

[0036] Dissolve 20g of urea in 50ml of deionized water, add 0.05g of MXene, stir to form a homogeneous solution, pour it into a closed polytetrafluoroethylene autoclave, and move it into a dry box, and keep it at 150°C for 24 hours. After the reaction, it was centrifuged and washed with deionized water and ethanol, and filtered and dried to obtain nitrogen-doped MXene.

[0037] 3. Preparation of nitrogen-doped MXene-supported cobalt phthalocyanine composites

[0038] Pour 0.02 g of cobalt phthalocyanine into 10 ml of DMF solvent and sonicate for 0.5 h; pour 0.02 g of nitrogen-doped MXene into 10 ml of DMF solvent and sonicate for 0.5 h. Then the...

Embodiment 2

[0040] 1. Synthesis of MXenes with F-terminal groups

[0041] Pour 20ml of 49% HF solution into the beaker and add 2g of Ti 3 AlC 2 The powder was stirred at 35°C for 24 hours, washed by centrifugation with deionized water, and filtered and dried for 24 hours to obtain MXene.

[0042] 2. Preparation of nitrogen-doped MXene

[0043] Dissolve 30g of urea in 50ml of deionized water, add 0.1g of MXene, stir to form a homogeneous solution, pour it into a polytetrafluoroethylene autoclave, and move it into a dry box, and keep it at 180°C for 12 hours. After the reaction, it was centrifuged and washed with deionized water and ethanol, and filtered and dried to obtain nitrogen-doped MXene.

[0044] 3. Preparation of nitrogen-doped MXene-supported cobalt phthalocyanine composites

[0045] Pour 0.005 g cobalt phthalocyanine into 10 ml DMF solvent and sonicate for 1 hour; pour 0.02 g nitrogen-doped MXene into 10 ml DMF solvent and sonicate for 1 hour. Then the cobalt phthalocyanine ...

Embodiment 3

[0047] The as-synthesized nitrogen-doped MXene-supported cobalt phthalocyanine composite was tested as an oxygen reduction catalyst for ORR.

[0048] Use electrochemical workstation and RDE rotating disk electrode to carry out electrocatalytic performance test, adopt three-electrode system (auxiliary electrode is platinum electrode; Reference electrode is calomel electrode, the composite material obtained in embodiment 1 is as working electrode) in oxygen saturated In the case of 0.1mol / L KOH solution, carry out LSV test with the rotating speed of 1600rpm (as a catalyst, the reaction of catalysis is O 2 +2H 2 O+4e - →4OH - (i.e. oxygen reduction reaction)). In practical applications, it is loaded on the cathode of a fuel cell as a catalyst. In this paper, the potential is converted to a standard hydrogen electrode. Before the test, oxygen is passed for 20 minutes to saturate the electrolyte. At 1600rpm and a scan rate of 50mv / s, the electrode material is activated by volta...

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Abstract

The invention relates to a preparation method and application of a nitrogen-doped MXene loaded cobalt phthalocyanine composite material. The method comprises the following steps: firstly, chemically etching Ti3AlC2 through a hydrofluoric acid solution to prepare MXene (namely Ti3C2F2) of which the surface adsorbs an F end group, then selecting urea as a nitrogen doping agent, loading a nitrogen element onto the MXene through a one-step hydrothermal method, and then combining cobalt phthalocyanine and the nitrogen-doped MXene to prepare the catalyst. The catalyst is applied to ORR, and the obtained catalytic material has good oxygen reduction catalytic activity and wide application prospects.

Description

technical field [0001] The invention belongs to the technical field of MXene composite materials, in particular to a nitrogen-doped MXene functionalized composite material, and more specifically to a preparation method of a nitrogen-doped MXene-loaded cobalt phthalocyanine composite material and an application for oxygen reduction reaction. Background technique [0002] With the advent of the global energy crisis and the increasing environmental pollution and greenhouse effect caused by the burning of fossil fuels, the development of clean energy is imminent. People are paying more and more attention to the storage and conversion of sustainable energy, and fuel cells, as one of the most promising clean energy converters, have high research value. In a fuel cell, fuel is oxidized at the anode, and the released electrons are transferred through an external circuit to the cathode, where oxygen is reduced. However, since the oxygen reduction reaction is a four-electron reaction...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/86H01M4/88H01M4/90H01M4/36
CPCY02E60/10Y02E60/50
Inventor 张文林何婷婷杨德新刘仕萌余文杰段艳菊于丰收李春利
Owner HEBEI UNIV OF TECH
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