Preparation method of high-purity phase spherical molybdenum disulfide

A nano-molybdenum disulfide, spherical technology, applied in the direction of molybdenum sulfide, nanotechnology, nanotechnology, etc., can solve the problems of uneven surface of molybdenum disulfide spheres, achieve uniform size, prevent agglomeration, and regular shape

Active Publication Date: 2016-07-20
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the surfactant molecules that have not formed micelles in the system exist in the form of ions and are adsorbed on the surface of molybdenum disulfide, resulting in uneven surface of molybdenum disulfide spheres and a wide range of particle size distribution (such as comparative example 1)

Method used

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  • Preparation method of high-purity phase spherical molybdenum disulfide
  • Preparation method of high-purity phase spherical molybdenum disulfide
  • Preparation method of high-purity phase spherical molybdenum disulfide

Examples

Experimental program
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Effect test

Embodiment 1

[0033] The mixed solution (V 无水乙醇 / V 去离子水 =1 / 19), add 2 mL of hydrazine hydrate after stirring evenly, transfer the solution into a high-pressure reactor with a volume of 100 mL after mixing evenly, seal it and place it in a 200°C incubator, keep it warm for 24 hours, cool to room temperature, and use After washing with deionized water and absolute ethanol, place it in a vacuum oven at 70°C for 8 hours to obtain the high-purity spherical nanomolybdenum disulfide required in this case.

[0034] Depend on figure 1 It can be seen that the product is composed of nanospheres with a particle size of about 400nm, the particle size distribution range of the spheres is narrow, the spherical structure is complete, and the dispersibility of the spheres is good.

[0035] Depend on figure 2 The XRD shows that the structure of molybdenum disulfide is 2H-MoS 2 .

Embodiment 2

[0037] The mixed solution (V 无水乙醇 / V 去离子水 =3 / 17), after stirring evenly, add 2mL of hydrazine hydrate, after mixing evenly, move the solution into a 100mL autoclave, seal it and place it in a 200°C incubator, keep it warm for 24h, cool to room temperature, and use After washing with deionized water and absolute ethanol, place it in a vacuum oven at 70°C for 8 hours to obtain the high-purity spherical nanomolybdenum disulfide required in this case. For the experimental results, see image 3 .

Embodiment 3

[0039] The mixed solution (V 无水乙醇 / V 去离子水 =1 / 3), after stirring evenly, add 2mL of hydrazine hydrate, after mixing evenly, transfer the solution into a 100mL autoclave, seal it and place it in a 180°C incubator, keep it warm for 12h, cool to room temperature, and use After washing with deionized water and absolute ethanol, place it in a vacuum oven at 70°C for 8 hours to obtain the spherical nanomolybdenum disulfide required in this case. For the experimental results, see Figure 4 .

[0040] According to the SEM image, the spherical structure of the prepared nanomolybdenum disulfide is complete, and the size distribution is narrow at about 400nm.

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Abstract

The invention relates to a preparation method of high purity phase spherical molybdenum disulfide. The method comprises the following steps: ammonium heptamolybdate, thioacetamide, and a surfactant are dissolved in a solvent with uniformly mixing; a reducing agent is added, the prepared solution is transferred into a high pressure reaction vessel, the high pressure reaction vessel is sealed, the sealed high pressure reaction vessel is placed into a thermotank at 120-250 DEG C for 3-72 hours; temperature is cooled to room temperature, after filtering, washing and drying processes, spherical nanometer molybdenum disulfide is obtained. The prepared high purity phase nanometer molybdenum disulfide has the advantages of structured morphology, uniform and adjustable size, high sphericility, good dispersibility, simple synthesis process, mild condition, low cost, and simple synthesizer. The high purity phase nanometer molybdenum disulfide has wide applications to electrode materials, lubrication materials and catalysis fields, and is hopeful to be used in industrial production.

Description

technical field [0001] The present invention relates to inorganic nano material molybdenum disulfide (MoS 2 ) preparation field, especially a preparation method of spherical nanomolybdenum disulfide. Background technique [0002] Molybdenum disulfide has good optical, electrical, lubricating, catalytic and other properties, so it has good application potential in electronic detection, solid lubrication, heterogeneous catalysis, gas storage materials and petrochemical industries. Molybdenum disulfide has a typical layered structure, and the layers are combined by weak van der Waals force, which is easy to peel off, and ions are easily inserted between the layers. Each molybdenum atom in the monoatomic layer is surrounded by six sulfur atoms, in the shape of a triangular prism, exposing many Mo-S facets, which can be used as catalytic active centers. Nano-sized molybdenum disulfide has the advantages of quantum size effect, surface effect, and more exposed active centers, wh...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/06B82Y30/00
Inventor 田志坚李敏王冬娥周志远马怀军赵愉生曲炜阎立军
Owner PETROCHINA CO LTD
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