Co9S8/MoS2 composite material prepared by two-step method and application thereof to hydrogen separation reaction

A composite material and molybdenum salt technology, applied in the field of materials and energy, can solve the problems of not using hydrogen production technology, cumbersome preparation steps, environmental pollution, etc., achieve important economic value and social significance, increase specific surface area, and improve catalytic activity. Effect

Active Publication Date: 2018-11-23
青岛博亭科技有限公司
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Problems solved by technology

The catalyst uses carbon fiber as the substrate and chemical vapor deposition method, the preparation steps are cumbersome and the cost is increased, and the use of sulfur as the sulfur source will generate toxic gases during the calcination process, causing pollution to the environment
Geng Hongbo et al disclosed a yolk-shell structure of

Method used

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  • Co9S8/MoS2 composite material prepared by two-step method and application thereof to hydrogen separation reaction
  • Co9S8/MoS2 composite material prepared by two-step method and application thereof to hydrogen separation reaction
  • Co9S8/MoS2 composite material prepared by two-step method and application thereof to hydrogen separation reaction

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preparation example Construction

[0029] In a typical embodiment of the present invention, there is provided a kind of above-mentioned Co 9 S 8 / MoS 2 A method for preparing a composite material, the method comprising the following steps:

[0030] (1)Co 9 S 8 Preparation of hollow sphere precursor: Cobalt salt, glutathione, and thiourea were mixed, then hydrothermally treated, and the product was collected and dried to obtain Co with a hollow sphere structure. 9 S 8 Precursor; Co prepared by this method 9 S 8 The size of the hollow spheres is uniform and the yield is high. No pollution to the environment during the preparation process;

[0031] (2)Co 9 S 8 / MoS 2 Precursor preparation: take Co 9 S 8 The precursor is placed in a solution of molybdenum salt and L-cysteine ​​for hydrothermal treatment, and the product is collected and dried to obtain MoS 2 Nanoflowers grow on hollow spheres Co 9 S 8 on the precursor;

[0032] (3)Co 9 S 8 / MoS 2 Preparation: Co 9 S 8 / MoS 2 The precursor is ...

Embodiment 1

[0044] Weigh 0.48g Co(CH 3 COO) 2 4H 2 O, after mixing 0.15g thiourea and 0.0591g glutathione, conduct hydrothermal treatment and heat at 180°C for 6h. After heating, the material was centrifuged and dried to obtain Co 9 S 8 Precursor. Take 20mg of Co 9 S 8 Precursor is base, placed in 45mg (NH 4 ) 2 MoS 4 and 303mgL-cysteine ​​mixed solution, heat treatment at 200°C for 24h, after heating, centrifuge, rinse and dry to collect Co 9 S 8 / MoS 2 The precursor was then placed in a tube furnace for calcination, and then heated to 600 °C for 2 h under an argon atmosphere to obtain Co 9 S 8 / MoS 2 . The electrochemical catalytic performance of the catalyst was tested in 1.0mol / L KOH solution with a conventional three-electrode system. Preparation of working electrode: Take 10mg of powder catalyst and add it to 0.05mL 5w / w% Nafion solution, ultrasonically disperse, the system is in the form of ink, use a pipette to draw 5μL dropwise on the 4cm 2 The working electrode...

Embodiment 2

[0050] Weigh 0.96g Co(CH 3 COO) 2 4H 2 O, after mixing 0.3g thiourea and 0.1182g glutathione, carry out hydrothermal treatment and heat at 140°C for 12h. After heating, the material was centrifuged and dried to obtain Co 9 S 8 Precursor. Take 60mg of Co 9 S 8 The precursor is used as the base, placed in 90mg (NH 4 ) 2 MoS 4and 606mgL-cysteine ​​mixed solution, heat treatment at 200°C for 24h, after heating, centrifuge, rinse and dry to collect Co 9 S 8 / MoS 2 The precursor was then placed in a tube furnace for calcination, and then heated to 600 °C for 2 h under an argon atmosphere to obtain Co 9 S 8 / MoS 2 . The electrochemical catalytic performance of the catalyst was tested in 1.0mol / L KOH solution with a conventional three-electrode system. Preparation of the working electrode: Take 10 mg powder catalyst and add it to 0.05 mL 5% Nafion solution, ultrasonically disperse it, the system is in the form of ink, use a pipette to draw 5 μL dropwise on the 4 cm 2...

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Abstract

The invention discloses a Co9S8/MoS2 composite material prepared by a two-step method and application thereof to hydrogen separation reaction. The invention aims at improving the catalysis performanceof a catalyst on hydrogen gas separation reaction and the self stability. Firstly, a quantitative cobalt salt, thiourea and glutathione mixed solution is subjected to hydro-thermal treatment to obtain hollow ball structure Co9S8 precursors; then, the Co9S8 precursors are put into molybdenum salt and L-cysteic acid solution for secondary hydro-thermal treatment; in the process, MoS2 nanometer flower precursors grow at the Co9S8 of the hollow ball structures; finally, through roasting treatment, Co9S8/MoS2 is obtained. The compound has the unique three-dimensional nanometer structure, so that the great specific surface area is realized; more active sites are exposed. More remarkable, an interface structure exists between the Co9S8 and MoS2; the Co-Mo-S bonds favorable for improving the catalysis activity exist, so that the hydrogen separation catalysis activity can be improved. The method has the advantages that the advantages that the operation is simple; no pollution exists in the manufacturing process; the production is easy.

Description

technical field [0001] The invention belongs to the technical field of materials and energy, in particular to a two-step method for preparing Co 9 S 8 / MoS 2 Composite materials and their application in hydrogen evolution reactions. Background technique [0002] Hydrogen energy is one of the main clean energy sources. Hydrogen production by electrolysis of water is one of the most widely used technologies at present. This is mainly due to its simple process, pollution-free production process, and abundant raw materials. This method uses direct current to split water into hydrogen and oxygen through an electrolyte. Due to the low degree of separation of water and low ionic conductivity, it is necessary to add electrolytes to increase the conductivity of the solution. At present, Pt / C catalysts have high catalytic activity for hydrogen evolution reaction, but their commercial application is limited due to their high price and limited reserves. Therefore, finding and res...

Claims

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Application Information

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IPC IPC(8): B01J27/051B01J35/02B01J35/08C25B1/04C25B11/06
CPCB01J27/0515B01J35/023B01J35/08C25B1/04C25B11/04Y02E60/36
Inventor 王宗花于婧张立学
Owner 青岛博亭科技有限公司
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