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Method for preparing porous defect-enriched molybdenum disulfide

A molybdenum disulfide and defect-rich technology, which is applied in the fields of molybdenum sulfide, chemical instruments and methods, chemical/physical processes, etc., can solve the problems of increased difficulty in recovery of supported molybdenum disulfide, inability to fully utilize the catalyst, difficulty in improving catalytic activity, etc. problems, to achieve the effect of improving vulcanization efficiency, cheap raw materials, and good product morphology

Active Publication Date: 2016-12-07
合肥庐阳科技创新集团有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But loaded MoS 2 The active components are easy to lose during use, which reduces its service life, and because the active components of the catalyst are loaded on a carrier with a high specific surface area, it is a two-dimensional bound structure, which cannot effectively contact the substrate and cannot fully exert Intrinsic catalytic activity of the catalyst [12]
Therefore, loaded MoS 2 It is difficult to improve the catalytic activity. In addition, as environmental protection becomes stricter, the recovery of supported molybdenum disulfide is also significantly more difficult. Therefore, it is urgent to develop non-supported molybdenum disulfide catalysts with higher activity density and more environmental protection.

Method used

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  • Method for preparing porous defect-enriched molybdenum disulfide
  • Method for preparing porous defect-enriched molybdenum disulfide
  • Method for preparing porous defect-enriched molybdenum disulfide

Examples

Experimental program
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Effect test

Embodiment 1

[0050] In this example, porous and defect-rich molybdenum disulfide is prepared according to the following steps:

[0051] (1) Weigh 3.0g of ammonium molybdate tetrahydrate and 6.0g of sodium chloride, dissolve them in 50mL of deionized water respectively, mix the two evenly under magnetic stirring, and when the temperature is raised to 70°C, the clear solution begins to change. It was turbid, and white flocs were precipitated after a few minutes. The reaction was stopped for 30 minutes, filtered while hot, and washed with deionized water several times to obtain a white flocculent solid, which was dried at room temperature to obtain nano-scale porous polymolybdate.

[0052] (2) Weigh 0.5070g nanoscale porous polymolybdate NaNH 4 MoO 10 ·H 2 O and 2.5095 g thiourea, the nanoporous polymolybdate NaNH 4 MoO 10 ·H 2 O was put into a polytetrafluoroethylene beaker, thiourea was added into the lining of the polytetrafluoroethylene reactor, and a small amount of water was poured...

Embodiment 2

[0055] In this example, porous and defect-rich molybdenum disulfide is prepared according to the following steps:

[0056] (1) Weigh 3.0g of ammonium molybdate tetrahydrate and 6.0g of sodium chloride, dissolve them in 50mL of deionized water respectively, mix the two evenly under magnetic stirring, and when the temperature is raised to 70°C, the clear solution begins to change. It was turbid, and white flocs were precipitated after a few minutes. The reaction was stopped for 30 minutes, filtered while hot, and washed with deionized water several times to obtain a white flocculent solid, which was dried at room temperature to obtain nano-scale porous polymolybdate.

[0057] (2) Weigh 0.5070g nanometer polymolybdate NaNH 4 MoO 10 ·H 2 O and 1.5095 g thiourea, the nanoporous polymolybdate NaNH 4 MoO 10 ·H 2 O was put into a polytetrafluoroethylene beaker, thiourea was added into the lining of the polytetrafluoroethylene reactor, and a small amount of water was poured in to ...

Embodiment 3

[0061] In this example, porous and defect-rich molybdenum disulfide is prepared according to the following steps:

[0062] (1) Weigh 3.0g of ammonium molybdate tetrahydrate and 6.0g of sodium chloride, dissolve them in 50mL of deionized water respectively, mix the two evenly under magnetic stirring, and when the temperature is raised to 70°C, the clear solution begins to change. It was turbid, and white flocs were precipitated after a few minutes. The reaction was stopped for 30 minutes, filtered while hot, and washed with deionized water several times to obtain a white flocculent solid, which was dried at room temperature to obtain nano-scale porous polymolybdate.

[0063] (2) Weigh 0.5070g nanoscale porous polymolybdate NaNH 4 MoO 10 ·H 2 O and 2.5095 g thiourea, the nanoporous polymolybdate NaNH 4 MoO 10 ·H 2 O was put into a polytetrafluoroethylene beaker, thiourea was added to the lining of the polytetrafluoroethylene reactor, and a small amount of water was poured i...

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Abstract

The invention discloses a method for preparing a porous defect-enriched molybdenum disulfide, and is characterized in that the method comprises the steps: adding a soluble acid or a soluble salt in an aqueous solution of molybdate, then heating, and making molybdate ions subjected to stepwise polymerization into porous heterozygous ordered aggregates under induction of cation; and centrifuging, washing and drying the product, transferring the product to a reactor kettle, taking a compound containing negative bivalent sulfur elements as a sulfur source, and thus obtaining the porous defect-enriched molybdenum disulfide through a hydrothermal-gas phase in-situ vulcanization method. The method has the advantages of simple operation, and cheap and easily obtained raw materials, and the obtained product has the advantages of good morphology and large specific surface area, and can be used for large-scale synthesis.

Description

technical field [0001] The invention relates to a preparation technology of molybdenum disulfide as a catalytic material, in particular to a preparation method of porous and defect-rich molybdenum disulfide. Background technique [0002] With the development of the economy, the consumption of fossil fuels continues to increase, which brings unprecedented environmental pressure to human society. The solution is to clean the fossil energy and develop new green energy. Hydrodesulfurization is one of the most effective means of fossil energy purification. At present, the catalyst used in hydrodesulfurization is molybdenum disulfide and its composite materials. [1,2] . Nonetheless, fossil energy sources are finite and non-renewable. Currently, there is an urgent need to develop new green energy sources. A large number of authoritative documents have proved that using sunlight as energy and using efficient catalysts to photolyze water to produce hydrogen is an effective means o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/06B01J27/051B01J35/10
CPCC01G39/06B01J27/051C01P2006/12C01P2002/72C01P2004/04B01J35/613B01J35/615
Inventor 刘文宏何帅陈天云苗世顶凤仪
Owner 合肥庐阳科技创新集团有限公司
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