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Preparation method and application of phosphorized WS2 nanosphere catalyst

A technology of catalysts and nanospheres, applied in the field of nanomaterials, can solve the problems of electrochemical research without WS2, and achieve the effects of controllable shape, simple operation and low cost

Active Publication Date: 2021-08-03
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Through the above analysis, although there are many WS in the prior art 2 studies, but there is no WS on phosphating 2 Electrochemical studies, nor for WS 2 Relevant disclosures about the advantages and disadvantages of P electrochemical performance

Method used

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  • Preparation method and application of phosphorized WS2 nanosphere catalyst
  • Preparation method and application of phosphorized WS2 nanosphere catalyst
  • Preparation method and application of phosphorized WS2 nanosphere catalyst

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preparation example Construction

[0040] Such as figure 1 As shown, the WS provided by the present invention2 The preparation method of P nanosphere catalyst comprises the following steps:

[0041] S101 Dissolve tungsten hexacarbonyl and sulfur powder in an organic solvent under the protection of an inert gas, and mix them uniformly at room temperature to obtain a brown mixed solution; fully react the brown mixed solution in a high-pressure reactor at 100°C-250°C , the brown mixed solution is fully reacted for 10-24h;

[0042] S102 After cooling the reacted autoclave to room temperature, the mixture is centrifuged to obtain a black precipitate, which is purified;

[0043] S103 React the purified black precipitate with sodium hypophosphite for 2-3 hours in a tube furnace with inert gas at 200°C-300°C to obtain WS 2 |P nanosphere catalyst.

[0044] The WS provided by the embodiment of the present invention 2 The preparation method of P nanosphere catalyst specifically comprises the following steps:

[0045]...

Embodiment 1

[0054] Example 1: Preparation of WS according to the invention 2 |P nanosphere catalyst

[0055] First, 0.33 g of sublimed sulfur powder and 1.76 g of tungsten hexacarbonyl were dissolved in 35 mL of organic solvent under the protection of nitrogen, and stirred rapidly at room temperature for 20 min, and then the mixture was transferred to a stainless steel autoclave, and the high pressure The reactor was placed in an oven at 230°C and kept for 24 hours; finally, after the temperature of the autoclave was cooled to room temperature, the mixture was centrifuged and washed to obtain a black precipitate, which was dispersed by ultrasonic waves, and deionized water and acetone were used to Alternately washed several times, finally collected by centrifugation, dried in a vacuum freeze dryer for 2 hours to obtain a purified black precipitate; the purified black precipitate was reacted with sodium hypophosphite at 300°C in a tube furnace with argon for 2 hours, Get WS 2 |P nanosphe...

Embodiment 2

[0060] Embodiment 2: WS provided by the embodiment of the present invention 2 |P nanosphere catalyst includes the following steps:

[0061] First, 0.33 g of sublimed sulfur powder and 1.76 g of tungsten hexacarbonyl were dissolved in 35 mL of organic solvent under the protection of nitrogen, and stirred rapidly at room temperature for 20 min, and then the mixture was transferred to a stainless steel autoclave, and the high pressure The reactor was placed in an oven at 230°C and kept for 24 hours; finally, after the temperature of the autoclave was cooled to room temperature, the mixture was centrifuged and washed to obtain a black precipitate, which was dispersed by ultrasonic waves, and deionized water and acetone were used to Alternately washed several times, finally collected by centrifugation, dried in a vacuum freeze dryer for 2 hours to obtain a purified black precipitate; the purified black precipitate was reacted with sodium hypophosphite at 200°C in a tube furnace wit...

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Abstract

The invention discloses a preparation method of a phosphorized WS2 nanosphere catalyst, which comprises the following steps of S101, dissolving tungsten hexacarbonyl and powdered sulfur in an organic solvent under the protection of inert gas, and uniformly mixing at room temperature to obtain a brown mixed solution, fully reacting the brown mixed solution in a high-pressure reaction kettle at 100-250 DEG C, wherein the brown mixed solution fully reacts for 10-24 hours, S102, cooling the high-pressure reaction kettle after the reaction to room temperature, centrifuging the mixture to obtain a black precipitate, and purifying, S103, enabling the purified black precipitate to react with sodium hypophosphite for 2-3 h at the temperature of 200-300 DEG C in a tubular furnace filled with inert gas, and then acquiring the product. The invention provides the WS2P nanosphere catalyst prepared by the method and application of the WS2P nanosphere catalyst. The preparation method of the WS2P nanosphere catalyst is simple, and nanosheet cluster type nanoparticles with uniform size and high specific surface area are obtained.

Description

technical field [0001] The invention relates to the technical field of nanomaterials, in particular to a phosphating WS 2 Preparation method and application of nanosphere catalyst. Background technique [0002] The massive burning of traditional fossil fuels has made environmental pollution worse, making people look for other renewable energy sources. Hydrogen energy has a high energy density, and the only product produced after combustion is water, making it the most promising candidate energy carrier. Electrochemical water splitting offers a feasible route to generate hydrogen, involving two half-reactions, the hydrogen evolution reaction (HER) at the cathode and the oxygen evolution reaction (OER) at the anode. However, the actual efficiency of hydrogen release during electrochemical water splitting is limited by the kinetics of the hydrogen release reaction (HER, 2H + +2e - →H 2 ) are strictly limited. Therefore, high-performance HER catalysts are urgently needed t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B11/054C25B11/091C25B1/04C23C16/28C01G41/00B82Y30/00B82Y40/00
CPCC25B1/04C23C16/28C01G41/00B82Y30/00B82Y40/00Y02E60/36
Inventor 林健健孙蕾高孟友郑德华
Owner QINGDAO UNIV OF SCI & TECH
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