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A kind of preparation method of flower-shaped molybdenum disulfide hollow microspheres

A technology of molybdenum disulfide and hollow microspheres, 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: 2015-09-16
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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  • A kind of preparation method of flower-shaped molybdenum disulfide hollow microspheres
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  • A kind of preparation method of flower-shaped molybdenum disulfide hollow microspheres

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Embodiment 1

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

[0042] figure 1 It is a flower-like molybdenum disulfide hollow microsphere XRD pattern, all diffraction peaks are consistent with pure MoS 2 The crystal standard diffraction pattern (PDF No.37-1492) of the hexagonal phase is consistent. Therefore, nanoscale MoS should be synthesized by hydrotherm...

Embodiment 2

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

Embodiment 3

[0046] 0.383g (C 8 h 17 ) 2 (CH 3 ) 2 NCl was dissolved in 60ml of distilled water, and then 2.28g of CS (NH 2 ) 2 , 1.45g NH 2 OH·HCl and 1.01g (NH 4 ) 2 MoO 4 . After completely dissolving, use 2mol·L -1 Adjust the pH to around 5 with HCl. After stirring for 20 min, the mixture was transferred to a 100 ml stainless steel reaction kettle, placed in a vacuum oven at 140° C. for 30 h, and cooled to room temperature. After the reaction product was separated by filtration, it was repeatedly washed with deionized water and absolute ethanol, and air-dried to obtain a gray-black product powder, that is, flower-shaped molybdenum disulfide hollow 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 nanomaterial preparation, and in particular, the invention relates to a preparation method of flower-shaped molybdenum disulfide hollow microspheres. Background technique [0002] Nanostructured materials possess unique physical, chemical, electrical, magnetic and mechanical properties. Due to its advantages such as low density and large specific surface area, it has potential application prospects in the fields of filling materials, drug delivery, and catalysis. 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, cathode materials for high-energy batteries, etc. [0003] Molybdenum disulfide (MoS 2 ) has a layered structure similar to graphite, belongs to the hexagonal crystal system, and is a compou...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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