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A method for preparing molybdenum disulfide microparticles by ammonium dodecamolybdenum phosphopolyacid

A technology of ammonium heteropolyacid and molybdenum disulfide, which is applied in the direction of molybdenum sulfide and nanotechnology, can solve the problems of complicated reaction steps and high manufacturing costs, and achieve the effect of simple operation and high application value

Active Publication Date: 2021-09-21
HEFEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These preparation methods all have the disadvantages of high manufacturing cost and complicated reaction steps.

Method used

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  • A method for preparing molybdenum disulfide microparticles by ammonium dodecamolybdenum phosphopolyacid
  • A method for preparing molybdenum disulfide microparticles by ammonium dodecamolybdenum phosphopolyacid

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Experimental program
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Effect test

Embodiment 1

[0017] Weigh 1.5g of ammonium dodecamolybdenum phosphopolyacid, dissolve in 50g, 12% potassium hydroxide solution, fully mix 3g of thioacetamide and the above solution under heating and stirring, and then use 5.5mol / L hydrochloric acid to adjust the pH value to 4. After the reaction, the obtained precipitated product was washed, filtered and dried to obtain molybdenum disulfide, which was then crystallized by heating at 480°C and used as a catalyst.

[0018] figure 1 , 2 They are the XRD pattern and scanning electron microscope pattern of the product obtained by reacting molybdenum disulfide with ammonium dodecamolybdenum phosphopolyacid and thioacetamide in Example 1, respectively. figure 1 Four of the main diffraction peaks can be attributed to (002), (100), (103), and (110) of molybdenum disulfide particles, indicating that molybdenum disulfide has been successfully prepared. figure 2 It shows that the molybdenum disulfide is granular, and the average size of the particl...

Embodiment 2

[0020] Weigh 1.5g of ammonium dodecamolybdenum phosphopolyacid, dissolve in 75g, 10% potassium hydroxide solution, fully mix 3.75g of thioacetamide and the above solution under heating and stirring, and then use 4mol / L Phosphoric acid was used to adjust the pH value to 3. After the reaction, the precipitated product was washed, filtered and dried to obtain molybdenum disulfide, which was then crystallized by heating at 300°C and used as a solid lubricant.

Embodiment 3

[0022] Weigh 1.5g of ammonium dodecamolybdenum phosphopolyacid, dissolve in 37.5g, 15% potassium hydroxide solution, fully mix 2.25g of thioacetamide and the above solution under heating and stirring, then use 7mol / L of hydrochloric acid to adjust the pH value to 3.5. After the reaction, the obtained precipitated product was washed, filtered and dried to obtain molybdenum disulfide, which was then crystallized by heating at 500°C and used as a catalyst.

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Abstract

The invention discloses a method for preparing molybdenum disulfide particles by ammonium dodecamolybdenum phosphopolyacid, and relates to the technical field of preparation of lubricants and catalysts. Dissolve the molybdenum source with lye first, then fully mix it with the sulfide solution under stirring and heating conditions, then add acid to neutralize the excess alkali, and adjust the pH value to acidic, then use the oxidizing and reducing properties of the molybdenum source The sulfide undergoes redox reaction. After the reaction is completed, it is filtered and separated, dried, and finally placed in an isolated air to heat and crystallize to obtain molybdenum disulfide particles that can be used as catalysts and solid lubricants. The present invention selects ammonium dodecamolybdenum phosphopolyacid, which is insoluble in water and strong acid, as raw material, utilizes the treatment method of alkali first and then acid, and then utilizes its oxidative property to directly oxidize sulfide, and at the same time, itself is reduced to Mo(VI) , eventually precipitated as molybdenum disulfide. The prepared molybdenum disulfide particles have high potential application value in the fields of lubricants and catalysts.

Description

technical field [0001] The invention relates to the technical field of lubricant and catalyst preparation, in particular to a method for preparing molybdenum disulfide particles from ammonium dodecamolybdenum phosphopolyacid. Background technique [0002] Ammonium dodecamolybdenum phosphopolyacid (H 12 Mo 12 N 3 o 40 P) or its hydrate (H 12 Mo 12 N 3 o 40 P·xH 2 O) The solubility in water is very small and can be dissolved in alkali. It is mainly used for the analysis of phosphorus and tin, alkaloid reagents and cation exchange reagents. [0003] Molybdenum disulfide has excellent lubricating and catalytic properties, and its performance is related to the size of its constituent particles. Generally, the performance is better when the size is smaller, so the preparation of molybdenum disulfide particles has attracted attention. At present, there are mainly the following preparation methods. One is to use soluble molybdate and sulfide to react to generate molybdenum...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G39/06B82Y40/00
Inventor 胡坤宏陈敏原治坤胡恩柱李芹
Owner HEFEI UNIV