Preparation method of nanometer molybdenum disulfide

A nano-molybdenum disulfide and molybdenum disulfide technology, which is applied in the direction of molybdenum sulfide and nanotechnology, can solve the problems of harsh electrolysis conditions, high energy consumption, and high cost, and achieve increased product added value, uniform particle size distribution, and low manufacturing costs. Effect

Inactive Publication Date: 2019-06-11
HENAN CHEM IND RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these methods have the following shortcomings: high energy consumption in the preparation process, low yield, high cost, and not environmentally friendly, which seriously hinder the development of MoS 2 Large-scale, high-volume production of materials, resulting in limited range of applications
[0005] Chinese patent application CN108640154A discloses a molybdenum disulfide nanomaterial and its preparation method. The patent application uses ionic liquid as the electrolyte and uses molybdenum disulfide rod electrolysis to prepare nano molybdenum disulfide, but the price of the ionic liquid is high and the electrolysis conditions are harsh. , the post-processing process is cumbersome, which is not conducive to large-scale production
Chinese patent application CN108862387A discloses a preparation method of heterosexual nanomolybdenum disulfide. The method first uses a variety of oxide nanoparticles as carriers, and uses ammonium molybdate as the molybdenum precursor species to impregnate the oxide carrier. The supported molybdenum disulfide material is prepared under sulfidation conditions, and finally the oxide support is removed by chemical etching with hydrofluoric acid, and a special-shaped nano-scale molybdenum disulfide material in the range of several nanometers to tens of nanometers can be obtained. The cost is high, and the hydrogen fluoride used Severe acid corrosion, great harm to human body

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Weigh 20g of ammonium nitrate, add 80ml of deionized water to make an intercalation agent solution; put 20g of molybdenum disulfide (D50=10μm) into a 250ml three-necked reaction flask, and vacuum the container through one of the three-necked reaction flasks. The vacuum degree is controlled at 20Kpa, and the prepared intercalation agent solution is sucked into the three-necked reaction flask through the other port of the three-necked reaction flask. Remove and return to normal pressure, soak at a temperature of 60°C for 10 hours; filter the soaking slurry, wash the obtained solid molybdenum disulfide with deionized water, and dry in vacuum at a drying temperature of 60°C for a drying time of 6 hours; Put the molybdenum disulfide of the intercalation agent into a microwave oven, adjust the power to 136KW, hold it for 15 minutes, take it out, and use the wet classification technology to obtain 8g of nano-scale molybdenum disulfide powder with a particle size D50 of 90nm. T...

Embodiment 2

[0023] Weigh 50g of potassium nitrate, add 150ml of deionized water to make an intercalation agent solution; put 30g of ordinary molybdenum disulfide (D50=21μm) into a 250ml three-necked reaction bottle, and vacuumize the container through one of the three-necked reaction bottles , the vacuum degree is controlled at 6.5Kpa, and the prepared intercalant solution is sucked into the three-necked reaction flask through the other port of the three-necked reaction flask. Release the vacuum, return to normal pressure, soak at a controlled temperature of 50°C for 8 hours; filter the soaking slurry, wash the obtained solid molybdenum disulfide three times with deionized water, and dry in vacuum at a drying temperature of 50°C for 6 hours. Put the dried molybdenum disulfide containing the intercalation agent into a microwave oven, adjust the power to 160KW, hold it for 10 minutes, take it out, and use wet classification technology to obtain 15g of nano-scale molybdenum disulfide powder w...

Embodiment 3

[0025] Weigh 20g of ammonium perchlorate, add 150ml of deionized water (it seems to exceed the range of 1:0.8-10), and make an intercalation agent solution; put 10g of ordinary molybdenum disulfide (D50=6μm) into a 250ml three-necked reaction bottle During the process, vacuumize, and the vacuum degree is controlled at 1.39Kpa. The prepared intercalation agent solution is sucked into the three-necked reaction flask through the other port of the three-necked reaction flask. Release the vacuum at the vent port of the container, return to normal pressure, soak at a controlled temperature of 40°C for 6 hours; filter the soaking slurry, wash the obtained solid molybdenum disulfide with ion-free water, and dry in vacuum at a drying temperature of 60°C for 8 hours. Put the dried molybdenum disulfide containing the intercalation agent into a microwave oven, adjust the power to 120KW, keep it for 30 minutes, take it out, and use wet classification technology to obtain 3g of nano-scale mo...

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Abstract

A preparation method of nanometer molybdenum disulfide comprises the following steps: a, preparing an intercalator solution, wherein the mass ratio of the intercalator to non-ionized water is 1:(0.8-10); b, loading molybdenum disulfide into a three-mouth sealed container, and vacuumizing the container to controlling the vacuum degree at 1.3-60 Kpa; the prepared intercalant solution is drawn into the container through a port of the closed container, and enabling the prepared intercalator solution to be sucked into the container through a mouth of the sealed container, opening the sealed container to release the vacuum environment and restore a normal pressure, and controlling the temperature at 20-80 DEG C for soaking for 10-24 hours, wherein the suction amount of the intercalator solutionguarantees that the molybdenum disulfide solid is completely submerged; c, filtering the soaking solution, and then washing the resulting solid molybdenum disulfide with ionized water after the filtering, and conducting vacuum drying at a drying temperature of 40 to 60 DEG C for 2 to 12 hours; and d, placing the dried molybdenum disulfide containing an intercalator in a microwave oven, adjusting the power to 100 to 180 KW, maintaining the time of 5 to 60 minutes, and then using a wet classification technology to obtain nanometer molybdenum disulfide powder.

Description

technical field [0001] The invention relates to the technical field of molybdenum disulfide preparation, in particular to a method for preparing nanometer molybdenum disulfide. Background technique [0002] Molybdenum disulfide is an important solid lubricant, especially suitable for high temperature, high pressure, low temperature and high vacuum environments. It also has diamagnetism, can be used as a linear photoconductor and a semiconductor showing P-type or N-type conductivity, and has the functions of rectification and energy conversion. Molybdenum disulfide can also be used as a catalyst for the dehydrogenation of complex hydrocarbons. [0003] Molybdenum disulfide is known as "the king of high-grade solid lubricating oil". Molybdenum disulfide is a solid powder made from natural molybdenum concentrate powder through chemical purification. Creamy feeling, insoluble in water. The product has the advantages of good dispersion and no sticking. It can be added to vario...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/06B82Y40/00
Inventor 成兰兴赵增兵谢存明赵怡丽孟新志杨国松张圆春陈波杨舒程黄文蕊成馨荷周涛王倩倩陈天天郭歌李雅楠丁为公张碧波
Owner HENAN CHEM IND RES INST
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