Preparation method of hollow cobalt sulfide microsphere catalyst

A cobalt sulfide and catalyst technology, which is applied in cobalt sulfide, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of high operating temperature, complicated methods, harmful raw materials, etc., and achieve increased active area, good reproducibility, and long reaction time short effect

Inactive Publication Date: 2018-06-12
FUZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Chinese patent CN 106865624A discloses a preparation method of cobalt sulfide, which utilizes cobalt chloride hexahydrate and sodium dimethyldithiocarbamate to obtain the product through a two-step process. The consumptio...

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  • Preparation method of hollow cobalt sulfide microsphere catalyst
  • Preparation method of hollow cobalt sulfide microsphere catalyst
  • Preparation method of hollow cobalt sulfide microsphere catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Dissolve 2 mmol of cobalt nitrate hexahydrate and 8 mmol of thioacetamide in 50 mL of water, and magnetically stir at room temperature for 10 min, while slowly dripping 1.4 mL of ethylenediamine solution, and continue stirring for 5 min. The obtained solution was sealed in a 70 mL stainless steel autoclave lined with polytetrafluoroethylene, and reacted at 180 °C for 16 h. Then it was cooled to room temperature, and the precipitate was taken out, and washed with deionized water and absolute ethanol three times at a speed of 1200 r, each time for 4 min. Finally, the product was vacuum-dried at 50 °C for 24 h to obtain cobalt sulfide with hollow microsphere structure.

Embodiment 2

[0030] Dissolve 2 mmol of cobalt nitrate hexahydrate and 8 mmol of thiourea in 50 mL of water, stir magnetically at room temperature for 10 min, and slowly add 2.6 mL of ethylenediamine solution dropwise, and continue stirring for 5 min. The obtained solution was sealed in a 70 mL stainless steel autoclave lined with polytetrafluoroethylene, and reacted at 180 °C for 20 h. Then it was cooled to room temperature, and the precipitate was taken out, and washed three times with deionized water and absolute ethanol at a speed of 1200r, each time for 4 min. Finally, the product was vacuum-dried at 50 °C for 24 h to obtain cobalt sulfide with hollow microsphere structure.

Embodiment 3

[0032] Dissolve 2 mmol of cobalt nitrate hexahydrate and 8 mmol of sulfur powder in 50 mL of water, stir magnetically at room temperature for 10 min, and slowly add 3.2 mL of ethylenediamine solution dropwise, and continue stirring for 5 min. The obtained solution was sealed in a 70 mL stainless steel autoclave lined with polytetrafluoroethylene, and reacted at 180 °C for 20 h. Then it was cooled to room temperature, and the precipitate was taken out, and washed three times with deionized water and absolute ethanol at a speed of 1200r, each time for 4 min. Finally, the product was vacuum-dried at 50 °C for 24 h to obtain cobalt sulfide with hollow microsphere structure.

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Abstract

The invention discloses a preparation method of a hollow cobalt sulfide microsphere catalyst. The method comprises the following steps: dissolving a cobalt source and a sulfur source into a solvent and adding a certain amount of ethylene diamine; sealing the solution into a stainless steel high-pressure reactor with the volume of 70mL, which has a polytetrafluoroethylene lining; cooling the solution to room temperature after reaction and taking out precipitate; washing and drying to obtain a cobalt sulfide material. The method disclosed by the invention has the advantages of simplicity, controllability, short reaction time, low cost and easiness in mass production. The prepared cobalt sulfide material has a hollow microsphere structure consisting of nanometer acicular crystals, and has theadvantages of higher specific surface area, higher porosity and good electrochemical hydrogen production performance. Under the condition of strong base, the cobalt sulfide material still has lower catalytic starting point potential of 27.9mV (when the electric current density is 1mA cm<-2>); electric potential is only 89.7mV when the current density is 10mA cm<-2>; the preparation method has a good prospect of wide application in producing hydrogen by using brine electrolysis under the alkaline conditions.

Description

technical field [0001] The invention belongs to the field of material preparation, and in particular relates to a method for preparing a hollow cobalt sulfide microsphere catalyst. Background technique [0002] At present, the problem of energy shortage and environmental pollution is becoming more and more prominent. Therefore, the development of clean and renewable energy has become increasingly urgent. Among them, hydrogen energy is considered to be an ideal energy source. At the same time, hydrogen plays a role in the development of renewable energy such as wind energy and solar energy. Therefore, hydrogen production by electrolysis of water is the only way for sustainable development. [0003] In order to increase the reaction rate and reduce the loss of electrical energy, the traditional electrochemical hydrogen production materials are mostly noble metals. For example, in acidic solution, platinum catalysts can efficiently carry out hydrogen evolution reaction (HER) i...

Claims

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Application Information

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IPC IPC(8): C01G51/00C25B1/04C25B11/06
CPCC01G51/30C01P2004/03C01P2004/34C01P2006/40C25B1/04C25B11/075Y02E60/36
Inventor 钱兴刘宏宇吴伟敏
Owner FUZHOU UNIV
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