Preparation method of mono-atomic cobalt based nitrogen-sulfur dually-doped carbon material catalyst

A catalyst, double-doping technology, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve problems such as expensive precursors, achieve simple and easy methods, significant cost advantages, and improve dispersion. Effects of Sexual and Intrinsic Activity

Inactive Publication Date: 2018-10-23
CHONGQING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In view of the general complexity of existing technologies, such as MOF method, TiO2 template method, etc., and expensive precursors, the purpose of the present invention is to propose a method for preparing highly efficient catalytically active single-atom carbon material catalysts by changing the metal ligand method

Method used

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  • Preparation method of mono-atomic cobalt based nitrogen-sulfur dually-doped carbon material catalyst
  • Preparation method of mono-atomic cobalt based nitrogen-sulfur dually-doped carbon material catalyst
  • Preparation method of mono-atomic cobalt based nitrogen-sulfur dually-doped carbon material catalyst

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Experimental program
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Effect test

Embodiment 1

[0029] (1) Preparation of precursor

[0030] According to the mass ratio of urea: glucose 60: 1, the total mass of urea glucose: the mass ratio of cobalt chloride hexahydrate is 30: 1, the molar ratio of cobalt chloride hexahydrate: sodium thiocyanide is 1: 2, and the urea is weighed , glucose, cobalt chloride hexahydrate, sodium thiocyanate; the above mixture was dissolved in 30-50mL of absolute ethanol, ultrasonically stirred for 5-10 minutes, placed in a blast drying oven at 40°C-60°C, and dried for 4 ~6h, until the ethanol is completely volatilized, and the mixture is recrystallized in a beaker. Then the recrystallized solid was taken out and placed in a ball mill with a rotation speed of 600rpm-800rpm and a number of turns of 2 to obtain a uniform catalyst precursor of urea, glucose, cobalt chloride hexahydrate and sodium thiocyanate.

[0031] (2) Preparation of single-atom cobalt-based nitrogen-sulfur double-doped carbon catalyst (CoNSG1)

[0032] First, place the abov...

Embodiment 2

[0037] (1) Preparation of precursor

[0038] According to the mass ratio of urea:glucose 60:1, the mass ratio of urea glucose:cobalt chloride hexahydrate is 240:1, the molar ratio of cobalt chloride hexahydrate:sodium thiocyanate is 1:2, weigh urea, glucose , cobalt chloride hexahydrate, sodium thiocyanate; dissolve the above mixture in 30-50mL of absolute ethanol, stir ultrasonically for 5-10 minutes, place in a blast drying oven at 40°C-60°C, and dry for 4-6h , until the ethanol was completely evaporated, and the mixture was recrystallized in a beaker. Then the recrystallized solid was taken out and placed in a ball mill with a rotation speed of 600rpm-800rpm and a number of turns of 2 to obtain a uniform catalyst precursor of urea, glucose, cobalt chloride hexahydrate and sodium thiocyanate.

[0039] (2) Preparation of single-atom cobalt-based nitrogen-sulfur double-doped carbon catalyst (CoNSG2)

[0040] First, place the above-prepared precursor in a tube furnace, raise ...

Embodiment 3

[0053] (1) Preparation of precursor

[0054] According to the mass ratio of urea:glucose 60:1, the mass ratio of nitrogen-carbon precursor:cobalt chloride hexahydrate is 360:1, the molar ratio of cobalt chloride hexahydrate:sodium thiocyanate is 1:2, and the nitrogen Carbon precursor, cobalt chloride hexahydrate, sodium thiocyanate; dissolve the above mixture in 30-50mL of absolute ethanol, stir ultrasonically for 5-10 minutes, place in a blast drying oven at 40°C-60°C, and dry 4 ~ 6h, until the ethanol is completely volatilized, and the mixture is recrystallized in the beaker. Then the recrystallized solid was taken out and placed in a ball mill with a rotation speed of 600rpm-800rpm and a number of turns of 2 to obtain a uniform catalyst precursor of urea, glucose, cobalt chloride hexahydrate and sodium thiocyanate.

[0055] (2) Preparation of single-atom cobalt-based nitrogen-sulfur double-doped carbon catalyst (CoNSG3)

[0056] First, place the above-prepared precursor i...

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Abstract

A metal ligand is changed, and through precisely controlled carbonization and metal high temperature reduction, a metal mono-atomic nitrogen-sulfur dually-doped carbon material is obtained. An S-containing ligand is added to prevent the generation of metal carbides during the pyrolysis process; the temperature and time of pyrolysis are controlled to avoid the precipitation of a carbon layer; metalions are anchored in a carbon skeleton of graphene; exposed metal nitrides and metal sulfides on the surface can be easily removed by acids; mono-atom level dispersion of metals in a graphene structure is realized, and at the same time, more active sites are exposed. The adjusting function of S during the pyrolysis process is smartly utilized to synthesize a metal mono-atomic catalyst, all metalatoms (100%) are utilized, and the dispersion, stability, and characteristic activity of the catalyst are all improved. Furthermore, the synergistic effect is generated by co-doping of nitrogen and sulfur and the catalytic activity is further enhanced. The prepared mono-atomic catalyst has excellent hydrogen evolution / oxygen reduction catalytic activity, the operation is simple, the industrial production is easy, and the catalyst can be widely applied to fuel cells that take a proton exchange membrane as the electrolyte.

Description

technical field [0001] The invention relates to the field of material chemistry, especially the field of fuel cell catalysts, in particular to a hydrogen evolution / oxygen reduction bifunctional electrocatalyst used on the cathode of a proton membrane fuel cell, specifically a single-atom cobalt-based nitrogen-sulfur double-doped carbon material catalyst. Background technique [0002] Proton exchange membrane fuel cells (PEMFCs) have the characteristics of high energy conversion efficiency, environmental friendliness and pollution-free, and are very suitable as the power source of new energy vehicles. The new type of automobile driven by proton exchange membrane fuel cells can effectively alleviate the energy and environmental problems brought about by the development of industrialization, and provide new opportunities for the sustainable development of the automobile industry in the future. Currently, the voltage loss of fuel cells mainly comes from the oxygen reduction rea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24
CPCB01J27/24
Inventor 魏子栋陈琳慧王尧何倩唐浩王艺霖
Owner CHONGQING UNIV
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