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A kind of preparation method of molybdenum disulfide co-doped with fluorine and nitrogen

A technology of molybdenum disulfide and co-doping, which is applied in chemical instruments and methods, chemical/physical processes, physical/chemical process catalysts, etc., can solve the problems of difficult wide application and complicated operation, and achieve cost reduction and simple operation process , to avoid the effects of post-processing steps

Active Publication Date: 2020-07-28
YANSHAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Studies have shown that the active sites of molybdenum disulfide are mainly concentrated at the edge, and its entire basal surface is inert. WenXiao et al. (Adv. Energy Mater. 2017, 1602086) obtained a higher electrolysis rate by doping molybdenum disulfide with nitrogen. However, the entire basal surface is still inert. Hong Li et al. (Nat Mater 15,48-53) activated the basal surface by increasing the sulfur vacancies on the basal surface to make it catalytically active, but it required The surface provides tensile force, the operation is complicated, and it is difficult to be widely used

Method used

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  • A kind of preparation method of molybdenum disulfide co-doped with fluorine and nitrogen
  • A kind of preparation method of molybdenum disulfide co-doped with fluorine and nitrogen
  • A kind of preparation method of molybdenum disulfide co-doped with fluorine and nitrogen

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Effect test

Embodiment 1

[0023] Add 0.35 grams of sodium molybdate, 2 grams of thiourea, 0.7 grams of ammonium fluoride, and 45 ml of water into a stainless steel reactor with a volume of 75 ml, stir for 30 minutes, seal it, and fill it with 60%; In a crucible boiler, heat at 350° C. for 6 hours, then allow the reaction kettle to cool down to room temperature naturally, and take out the mixture. The above mixture was washed 6 times successively with absolute ethanol, 0.5 mol / liter of dilute hydrochloric acid and distilled water, filtered, and then placed in a vacuum drying oven with a vacuum degree of -1Mpa and vacuum-dried at 70°C for 12 hours to obtain Fluorine and nitrogen co-doped molybdenum disulfide with excellent catalytic activity for hydrogen production from water electrolysis.

[0024] Such as figure 1 As shown, it can be clearly seen that fluorine and nitrogen co-doped molybdenum disulfide are in the shape of petal balls, and the petal balls are stacked by flakes.

[0025] Such as figur...

Embodiment 2

[0028] Add 0.35 grams of sodium molybdate, 2 grams of thioacetamide, 0.7 grams of ammonium fluoride, and 45 ml of water into a stainless steel reaction kettle with a volume of 75 ml in sequence, stir for 30 minutes, seal, and the filling capacity is 60%; The kettle was placed in a crucible boiler, heated at 450°C for 12 hours, and then the reaction kettle was naturally cooled to room temperature, and the mixture was taken out. The above mixture was washed 3 times successively with absolute ethanol, 0.5 mol / liter of dilute hydrochloric acid and distilled water, filtered, and then placed in a vacuum drying oven with a vacuum degree of -1Mpa at 60 ° C for 24 hours to obtain Fluorine and nitrogen co-doped molybdenum disulfide with excellent catalytic activity for hydrogen production from water electrolysis.

[0029] Such as Figure 4 As shown, it can be seen that fluorine and nitrogen co-doped molybdenum disulfide have discontinuous lattices and disconnected lattices, which provi...

Embodiment 3

[0031] Add 0.35 gram of ammonium molybdate, 0.7 gram of thiourea, 0.7 gram of ammonium fluoroborate, and 45 ml of water into a stainless steel reactor with a volume of 75 ml, stir for 10 minutes, seal, and the filling capacity is 60%; then put the reactor into In a crucible boiler, heat at 350° C. for 12 hours, then allow the reaction kettle to cool down to room temperature naturally, and take out the mixture. The above mixture was washed 5 times successively with absolute ethanol, 0.5 mol / liter of dilute hydrochloric acid and distilled water, filtered, and then placed in a vacuum oven with a vacuum degree of -1Mpa and vacuum-dried at 70°C for 24 hours to obtain Fluorine and nitrogen co-doped molybdenum disulfide with excellent catalytic activity for hydrogen evolution in electrolysis of water.

[0032] Such as Figure 5 As shown, it can be seen that the molybdenum disulfide co-doped with fluorine and nitrogen has a microscopic mesoporous structure, which provides a fast ion ...

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Abstract

A method for preparing molybdenum disulfide co-doped with fluorine and nitrogen, which mainly includes adding molybdenum source, sulfur source, nitrogen source and fluorine source into a stainless steel reactor in sequence according to a certain mass ratio, adding water, and then stirring for 10 ~30 minutes, the filling amount is 60~80%, then put the above mixture into a stainless steel reactor and seal it, place it in a crucible boiler, heat it at 250~450℃ for 6~24h, and then wait for the reactor to naturally cool to At room temperature, take out the mixture; wash the above mixture 3 to 6 times with absolute ethanol, dilute hydrochloric acid and distilled water in sequence, filter, and place the resulting powder in a vacuum drying oven at 60 to 100°C for vacuum drying for 6 to 24 hours. The invention has the advantages of simple process, mild reaction conditions, no need to add any surfactant, high repeatability and low cost. The prepared fluorine and nitrogen co-doped molybdenum disulfide has excellent catalytic activity and shows excellent performance in acidic environment. It has catalytic activity for electrolyzing water and producing hydrogen, and has good cycle stability.

Description

technical field [0001] The invention relates to a preparation method of a hydrogen production catalyst by electrolysis of water. Background technique [0002] In today's society, fossil energy is the most important energy consumed in the world, but due to its limited reserves, with the continuous exploitation and use of human beings, the depletion of fossil energy will be inevitable. At the same time, due to the incomplete combustion of fossil energy, a large amount of greenhouse gases such as carbon dioxide will be produced, and the greenhouse effect of the atmosphere will also be enhanced, which has caused a series of extremely serious problems such as global warming, and its combustion may produce Some polluted flue gas will also pose a serious threat to the global ecological environment. Considering the above problems, the development of clean and renewable energy is the direction of energy development in the future. Among many energy carriers, hydrogen has attracted w...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/24B01J27/051B01J35/08
CPCB01J27/051B01J27/24B01J35/51
Inventor 高发明王远哲刘珊珊周军双王栋郝险峰
Owner YANSHAN UNIV
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