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Preparation method of flower-shaped hollow molybdenum disulfide microspheres

A technology of hollow microspheres and molybdenum disulfide, which is applied in the direction of molybdenum sulfide and nanotechnology, can solve the problems that the shape of molybdenum disulfide hollow microspheres is difficult to control, the nanoparticles are easy to agglomerate, and affect the large-scale application. The effect of simple and easy to control, obvious layered structure, high specific surface area and tribological properties

Inactive Publication Date: 2012-10-03
无锡润鹏复合新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] However, because the nanoparticles are easy to agglomerate during the preparation process, the morphology of the molybdenum disulfide hollow microspheres obtained by the prior art is not easy to control, and the prior art process is complicated, which affects its large-scale application in the fields of tribology and photochemistry.

Method used

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  • Preparation method of flower-shaped hollow molybdenum disulfide microspheres
  • Preparation method of flower-shaped hollow molybdenum disulfide microspheres
  • Preparation method of flower-shaped hollow molybdenum disulfide microspheres

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Experimental program
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Effect test

Embodiment 1

[0041] 0.2g C 13 H 22 ClN was dissolved in 70ml of distilled water, and then 1.40g CS(NH 2 ) 2 , 0.725gNH 2 OH·HCl and 0.88g(NH 4 ) 2 MoO 4 . After dissolving completely, use 2mol·L -1 The HCl adjusts the pH to around 6. After stirring for 30 minutes, the mixture was transferred to a 100ml stainless steel reactor, placed in a vacuum drying oven at 180°C for 24 hours, and cooled to room temperature. After centrifugal separation, the reaction product was washed repeatedly with deionized water and absolute ethanol, and finally dried at 80° C. under vacuum for 10 hours to obtain gray-black product powder, namely, flower-like hollow molybdenum disulfide microspheres.

[0042] figure 1 XRD spectra of flower-like hollow molybdenum disulfide microspheres, all diffraction peaks are identical to those of pure MoS 2 The crystal standard diffraction pattern of the hexagonal phase (PDF No. 37-1492) is consistent. Therefore, the synthesis of hydrothermal reaction should be nano-scale MoS 2 . ...

Embodiment 2

[0044] Dissolve 13.6g F127 in 70ml distilled water, then add 1.40g CS(NH 2 ) 2 , 0.725gNH 2 OH·HCl and 0.88g(NH 4 ) 2 MoO 4 . After dissolving completely, use 2mol·L -1 The HCl adjusts the pH to around 6. After stirring for 30 minutes, the mixture was transferred to a 100ml stainless steel reactor, placed in a vacuum drying oven at 180°C for 24 hours, and cooled to room temperature. After centrifugal separation, the reaction product was washed repeatedly with deionized water and absolute ethanol, and finally dried at 80° C. under vacuum for 10 hours to obtain gray-black product powder, namely, flower-like hollow molybdenum disulfide microspheres.

Embodiment 3

[0046] 0.383g(C 8 H 17 ) 2 (CH 3 ) 2 NCl was dissolved in 60ml of distilled water, and then 2.28gCS(NH 2 ) 2 , 1.45g NH 2 OH·HCl and 1.01g(NH 4 ) 2 MoO 4 . After dissolving completely, use 2mol·L -1 The HCl adjusts the pH to around 5. After stirring for 20 minutes, the mixture was transferred to a 100ml stainless steel reactor, placed in a vacuum drying oven at 140°C for 30 hours, and cooled to room temperature. After the reaction product is separated by filtration, it is washed repeatedly with deionized water and absolute ethanol, and air-dried to obtain gray-black product powder, namely, flower-like hollow molybdenum disulfide microspheres.

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Abstract

The invention relates to a preparation method of flower-shaped hollow molybdenum disulfide microspheres, belonging to the technical field of nanometer material preparation. The method provided by the invention comprises the following steps of: (1) solution preparation: dissolving (NH4)2MoO4, CS(NH2)2, NH2OH.HCl and a surfactant into water, dissolving to obtain the solution, and then adjusting the pH value to 5-6.5 by acid; (2) agitating the solution obtained in step (1), and then transferring to a reaction kettle, sealing and reacting at a constant temperature, and then cooling to the room temperature to obtain the reaction product; (3) separating the reaction product, washing and drying to obtain the flower-shaped hollow molybdenum disulfide microspheres. The shape of the flower-shaped hollow molybdenum disulfide microspheres prepared by the method provided by the invention is controllable. The method provided by the invention is simple in process and low in cost; the prepared product is high in purity and high in yield, has an important application in the field of tribology and photochemistry, and is expected to be applied to large-scale industrial production.

Description

Technical field [0001] The invention belongs to the technical field of nano-material preparation. Specifically, the invention relates to a method for preparing flower-shaped hollow molybdenum disulfide microspheres. Background technique [0002] Nanostructured materials have unique physical, chemical, electrical, magnetic and mechanical properties. Because of its advantages such as low density and large specific surface area, it has potential application prospects in the fields of filling materials, drug delivery, catalysis and so on. Therefore, it is of great significance to carry out research on the preparation of such materials. Existing studies have shown that transition metal disulfides have unique properties, and they can be used as photosensitive materials, catalysts, lubricants, and cathode materials for high-energy batteries. [0003] Molybdenum disulfide (MoS 2 ) It has a layered structure similar to graphite and belongs to the hexagonal crystal system. It is a compound...

Claims

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Application Information

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IPC IPC(8): C01G39/06B82Y40/00
Inventor 李长生唐国钢唐华孙建荣范有志钱周
Owner 无锡润鹏复合新材料有限公司
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