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A kind of preparation method of cobalt sulfide and its product and application

A technology of sulfide and vulcanizing agent, applied in the direction of cobalt compounds, chemical instruments and methods, cobalt sulfide, etc., to achieve the effects of regular shape, uniform deposition, and low vulcanization reaction temperature

Active Publication Date: 2021-06-29
JIANGHAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the current methods of preparing cobalt sulfide are mostly sulfidation modification in a high-temperature hydrothermal environment or a tube furnace, and the prepared cobalt sulfide is in a crystalline state

Method used

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  • A kind of preparation method of cobalt sulfide and its product and application
  • A kind of preparation method of cobalt sulfide and its product and application
  • A kind of preparation method of cobalt sulfide and its product and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Weigh 3mmol of cobalt nitrate and 15mmol of urea and dissolve them in 60mL of deionized water. After the dissolution is complete, a purple-red solution is obtained. Pour the solution into a 100mL hydrothermal reaction kettle, then tighten the reaction kettle and put it in a blast oven at 90°C. Heating for 6 hours, after the reaction, a nano-precipitation of cobalt basic carbonate was obtained, which was washed with deionized water and absolute ethanol several times and dried by centrifugation to obtain a purple-red basic cobalt carbonate nano-particle powder, and then weighed 0.1g of the powder Pour into 30mL sodium sulfide solution (0.27mol / L), stir and react at 25°C for 0.01h, then pour the solution into a centrifuge tube and centrifuge several times to separate the precipitate, and finally dry the precipitate at low temperature to obtain amorphous cobalt sulfide nanoparticle powder.

Embodiment 2

[0044] Weigh 3mmol of cobalt nitrate, 15mmol of urea and 6mmol of ammonium fluoride and dissolve in 60mL of deionized water. After the dissolution is complete, a purple solution is obtained. In an oven, heat at 90°C for 6 hours. After the reaction, a nano-precipitate of cobalt basic carbonate is obtained. The precipitate is washed with deionized water and absolute ethanol several times and dried by centrifugation to obtain a purple-red basic cobalt carbonate nano-particle powder. Weigh 0.1g powder and pour it into 30mL sodium sulfide solution (0.27mol / L), stir and react at 0°C for 24 hours, then pour the solution into a centrifuge tube and centrifuge several times to separate the precipitate, and finally dry the precipitate at low temperature to obtain Amorphous cobalt sulfide nanoparticle powder.

Embodiment 3

[0046]Weigh 3mmol of cobalt nitrate and 15mmol of urea and dissolve them in 60mL of deionized water. After the dissolution is complete, a purple-red solution is obtained. At the same time, cut out 2.5cm*1cm of nickel foam and clean it with acetone, 3mol / L hydrochloric acid and deionized water. , then pour the mixed solution of cobalt nitrate and urea into a 100mL hydrothermal reaction kettle, and immerse the cleaned foamed nickel into the solution, then put the reaction kettle into a blast oven, heat at 90°C for 6h, and take out the foamed nickel After drying at low temperature, the basic cobalt carbonate supported by nickel foam can be obtained, and then the dried nickel foam-supported basic cobalt carbonate is immersed in 30mL sodium sulfide solution (0.27mol / L), reacted at 25°C for 24h, and then The foamed nickel is taken out and dried at a low temperature to obtain the amorphous cobalt sulfide nanomaterial supported by the foamed nickel.

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Abstract

The invention discloses a preparation method of cobalt sulfide and its products and applications. The preparation method includes the following steps: (1) weighing cobalt salt and urea, dissolving them in water, and stirring to obtain a uniformly mixed solution; (2) mixing The solution undergoes a hydrothermal reaction to obtain a basic cobalt carbonate precipitate; (3) centrifuging and drying the basic cobalt carbonate precipitate, adding it to an aqueous solution containing a sulfurizing agent for low-temperature vulcanization, and obtaining amorphous cobalt sulfide nanoparticles. The present invention quickly prepares cobalt sulfide nanomaterials with regular appearance and amorphous structure through low-temperature vulcanization; the vulcanization reaction temperature is low, the reaction time is short, significantly reduces energy consumption, and is beneficial to scale-up production; the prepared cobalt sulfide nanoparticles are Cobalt sulfide with an amorphous structure exhibits more excellent catalytic activity for electrochemical hydrogen evolution than crystalline cobalt sulfide.

Description

technical field [0001] The invention belongs to the field of material preparation, and in particular relates to a preparation method of cobalt sulfide and its product and application. Background technique [0002] With the accelerated promotion of fuel cell technology, the production of hydrogen energy has become an important part of its commercialization process. Hydrogen production by water electrolysis has the advantages of high conversion efficiency, simple process, no pollution, and high purity of hydrogen produced, so it is an ideal technology choice. At present, the actual voltage required for water electrolysis far exceeds the theoretical voltage of 1.23V, which is closely related to the excessive activation overpotential of the electrode. The development of low-cost, high-activity catalysts is one of the effective methods to reduce the overpotential of electrodes. Water electrolysis catalysts represented by transition metals such as iron, cobalt, and nickel not onl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G51/00B01J27/043C25B1/04
CPCB01J27/043C01G51/30C01P2002/72C01P2004/03C25B1/04Y02E60/36
Inventor 鲁望婷李旭文李雯慧梁思雨黄颖孙依妮魏锋
Owner JIANGHAN UNIVERSITY
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