Solution synthesis method of atomically-dispersive metal oxygen reduction catalyst

An atomic-level, reducing agent technology, applied in the fields of materials science and engineering technology and chemistry, can solve the problems of low effective utilization of metal atoms and precious metal atoms and high application costs

Active Publication Date: 2018-10-16
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] At present, atomically dispersed metal oxygen reduction catalysts have the problem of low effective utilization o...

Method used

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  • Solution synthesis method of atomically-dispersive metal oxygen reduction catalyst
  • Solution synthesis method of atomically-dispersive metal oxygen reduction catalyst
  • Solution synthesis method of atomically-dispersive metal oxygen reduction catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] First, configure the metal precursor solution: 0.01mol / L CoCl 2 Solution, wherein the first solvent is a water / ethanol mixed solution with a volume ratio of 1:9; reducing agent solution: 5.0mol / L N containing 0.05mol / L KOH 2 h 5 OH hydrazine hydrate solution; dispersion: 2.5mg ml -1 Nitrogen-doped mesoporous carbon dispersions.

[0058]Subsequently, the CoCl 2 The solution, hydrazine hydrate solution and dispersion liquid were placed in a low-temperature box, cooled to minus 60°C and kept warm for 30 minutes. CoCl 2 After the solution is mixed with hydrazine hydrate solution, the following reactions will occur:

[0059] 2CoCl 2 +N 2 h 5 OH+4KOH→2Co+4KCl+5H 2 O+N 2

[0060] Thus, in choosing CoCl 2 Solution and the relative amount of hydrazine hydrate solution, choose 5ml CoCl 2 solution and 20ml of hydrazine hydrate solution. With syringe pump control, 5ml CoCl 2 Solution in 0.125ml min -1 Add dropwise to 20ml of reducing agent solution at a rate of The...

Embodiment 2

[0066] First, configure the metal precursor solution: 0.02mol / L CoCl 2 solution, wherein the first solvent is a water / ethanol mixed solution with a volume ratio of 1:9; reducing agent solution: 5.0mol / L N containing 0.10mol / L KOH 2 h 5 OH hydrazine hydrate solution; dispersion: 2.5mg ml -1 Nitrogen-doped mesoporous carbon dispersions.

[0067] Subsequently, the CoCl 2 The solution, hydrazine hydrate solution and dispersion liquid were placed in a low-temperature box, cooled to minus 45°C and kept warm for 30 minutes. With syringe pump control, 5ml CoCl 2 Solution in 0.25ml min -1 Add dropwise to 20mL of reducing agent solution at a rate of The mixed liquid was continued to react at minus 45° C. for 2 hours, then mixed with 20 mL of nitrogen-doped mesoporous carbon dispersion, and stirred for 3-5 hours.

[0068] Subsequently, the mesoporous carbon-supported cobalt single-atom sample was filtered and cleaned by low-temperature vacuum filtration, and then dried naturally a...

Embodiment 3

[0071] First, configure the metal precursor solution: 0.005mol / L Co(NO 3 ) 2 solution, wherein the first solvent is a water / tetrafluorohydrofuran mixed solution with a volume ratio of 1:9; reducing agent solution: 5.0mol / L N containing 0.05mol / L KOH 2 h 5 OH hydrazine hydrate solution; dispersion: 2.5mg ml -1 Nitrogen-doped mesoporous carbon dispersions.

[0072] Subsequently, the Co(NO 3 ) 2 The solution, hydrazine hydrate solution and dispersion liquid were placed in a low-temperature box, cooled to minus 30°C and kept for 30 minutes. With syringe pump control, 5ml Co(NO 3 ) 2 Solution in 0.5ml min -1 Add dropwise to 20mL of reducing agent solution at a rate of The mixed liquid was continued to react at minus 30° C. for 2 hours, then mixed with 20 mL of nitrogen-doped mesoporous carbon dispersion, and stirred for 3-5 hours.

[0073] Subsequently, the mesoporous carbon-supported cobalt single-atom sample was filtered and cleaned by low-temperature vacuum filtration,...

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Abstract

The invention provides a solution synthesis method of an atomically-dispersive metal oxygen reduction catalyst, comprising: (1) mixing a metal compound and a first solvent to form a metal precursor solution; (2) mixing a reducing agent and a second solvent to form a reducing agent solution; (3) mixing a carrier material and a third solvent to form a dispersion; (4) mixing the metal precursor solution and the reducing agent solution by dropwise adding and stirring so as to obtain a solution containing an atomically-dispersive metal; and (5) adding the dispersion into the solution containing theatomically-dispersive metal, stirring such that the carrier material is used to adsorb the automatically-dispersive metal to obtain the atomically-dispersive metal oxygen reduction catalyst, whereinthe steps (4) and (5) have the ambient temperature of -100 DEG C to 0 DEG C. The catalyst prepared via the method has the advantages of high density, high yield, high efficiency, high applicability and the like, the method is suitable for large-scale preparation of catalysts having high metal loading capacity, and the cost is significantly reduced.

Description

technical field [0001] The invention relates to the fields of material science and engineering technology and chemistry, in particular to a method for synthesizing an atomic-level dispersed metal oxygen reduction catalyst from a solution. Background technique [0002] For supported catalysts, the smaller the metal particle size, the better. This is because the catalytic active sites of the above-mentioned catalysts exist on the surface of the metal particles, and the inside of the catalyst does not react with the reactants. Thus, the maximum exposure of the active sites of the metal particles can improve the catalytic activity and reduce the cost. At present, metal atoms can be used as active sites in the catalytic reaction process, that is to say, single atoms can be used for catalysis. Compared with traditional nanoscale metal catalysts, atomically dispersed metal catalysts can not only significantly improve the effective utilization of metal atoms as active sites for ca...

Claims

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Application Information

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IPC IPC(8): B01J37/16B01J37/08B01J37/06B01J37/00B01J27/24B01J23/755B01J23/75B01J23/745
CPCB01J23/745B01J23/75B01J23/755B01J27/24B01J35/0046B01J37/00B01J37/06B01J37/08B01J37/16
Inventor 伍晖黄凯魏呵呵张潇源
Owner TSINGHUA UNIV
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