A kind of preparation method of transition metal phosphide nano hollow sphere

A transition metal and phosphide technology, applied in the direction of phosphide, can solve the problems of unsuitable operation, expensive raw materials, and many by-products, and achieve the effects of stable structure, large specific surface area, and mild reaction conditions

Active Publication Date: 2019-03-22
CHANGZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The methods of preparing phosphides include elemental chemical method, solid-state double decomposition method, phosphine reaction method, organic metal decomposition method, electrolytic molten salt method, etc. Most of the preparation methods need to be carried out under high temperature and high pressure, and some require very expensive raw materials. In many reactions, highly toxic substances such as phosphine are used as phosphorus sources, which are not suitable for operation and produce many by-products

Method used

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  • A kind of preparation method of transition metal phosphide nano hollow sphere
  • A kind of preparation method of transition metal phosphide nano hollow sphere
  • A kind of preparation method of transition metal phosphide nano hollow sphere

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Weigh 20mg of cobalt oxide nanospheres and disperse them in 50mL of ethylene glycol solvent;

[0023] (2) Add 100 mg of sodium hypophosphite to the dispersion obtained in step (1), and react in an oil bath at 100° C. for 12 hours;

[0024] (3) The product obtained in step (2) is washed with water and ethanol by suction filtration for several times, and vacuum-dried at 60° C.;

[0025] (4) Etching the product obtained in step (3) for 12 hours at 20°C in a 1mol / L hydrochloric acid solution;

[0026] (5) The product obtained in step (4) is centrifuged, washed with water, and vacuum-dried at 60° C. to obtain transition metal cobalt phosphide hollow spheres.

Embodiment 2

[0028] (1) Weigh 40mg of nickel oxide nanospheres and disperse them in 50mL of ethylene glycol solvent;

[0029] (2) Add 100 mg of sodium hypophosphite to the dispersion obtained in step (1), and react in an oil bath at 100° C. for 12 hours;

[0030] (3) The product obtained in step (2) is washed with water and ethanol by suction filtration for several times, and vacuum-dried at 60° C.;

[0031] (4) Etching the product obtained in step (3) for 12 hours at 40°C in a 1mol / L sulfuric acid solution;

[0032] (5) The product obtained in step (4) is centrifuged, washed with water, and vacuum-dried at 60° C. to obtain transition metal nickel phosphide hollow spheres.

Embodiment 3

[0034] (1) Weigh 60mg of manganese oxide nanospheres and disperse them in 50mL of ethylene glycol solvent;

[0035] (2) Add 100 mg of sodium hypophosphite to the dispersion obtained in step (1), and react in an oil bath at 100° C. for 12 hours;

[0036] (3) The product obtained in step (2) is washed with water and ethanol by suction filtration for several times, and vacuum-dried at 60° C.;

[0037] (4) Etching the product obtained in step (3) for 12 hours at 20°C in a 1mol / L hydrochloric acid solution;

[0038] (5) The product obtained in step (4) is centrifuged, washed with water, and dried under vacuum at 60° C. to obtain transition metal manganese phosphide hollow spheres.

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Abstract

The invention relates to a preparation method of transition metal phosphide nano hollow spheres. The preparation method includes following steps: preparing transition metal oxide nanospheres; adopting an anion exchange method to exchange the transition metal oxide nanospheres, and pickling to obtain hollow transition metal phosphide nanospheres. The preparation method has the advantages that hollow transition metal phosphide prepared by the method is mild in needed reaction condition, stable in structure and large in specific surface area, and hollow spherical structure can provide more reaction active sites for chemical reaction, thereby being more conducive to application of electrocatalysis and chemical catalysis.

Description

technical field [0001] The invention relates to a preparation method of transition metal phosphide nano hollow spheres, belonging to the technical field of material synthesis. Background technique [0002] In recent years, the rapid consumption of fossil fuels and the resulting environmental pollution have attracted more and more attention. Hydrogen energy, as a green and environmentally friendly renewable energy, has also become a hot spot of scientific research. Hydrogen production by electrolysis of water has the advantages of convenient operation, high degree of automation, and no pollution to the environment. It is an effective way to produce high-purity hydrogen. However, the kinetics of the hydrogen evolution reaction in water electrolysis is very slow and requires a high overpotential to generate a large current density. Therefore, it is necessary to develop efficient and stable catalysts. [0003] At present, the most commonly used hydrogen evolution reaction catal...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/08
CPCC01B25/08C01P2004/04C01P2004/34
Inventor 秦勇王淑敏何晶晶储富强孔泳陶永新
Owner CHANGZHOU UNIV
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