Preparation method of high-purity molybdenum disulfide

A molybdenum disulfide and molybdenum trisulfide technology, applied in the production of molybdenum sulfide and bulk chemicals, can solve the problems of environmental pollution and complicated preparation of molybdenum disulfide, and achieve the effects of extremely low vapor pressure and good high temperature resistance.

Active Publication Date: 2021-10-01
洛阳申雨钼业有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of this, the purpose of the present invention is to provide a preparation method of high-purity molybdenum disulfide, to solve the existing molybdenum disulfide preparation is loaded down with trivial details, the problem of environmental pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A preparation method of high-purity molybdenum disulfide, comprising the following steps:

[0027] 1) Using 39.2g of ammonium molybdate and 25.6g of elemental sulfur as raw materials, cothermal reaction was carried out in 196g of ionic liquid (1,3-dimethylimidazolium tetrafluoroborate); the temperature of cothermal reaction was 200°C and the time was 12 hour, after the reaction finishes, filter while hot to obtain filter cake and be ammonium tetrathiomolybdate intermediate product 51.5g, yield 98.82%;

[0028] 2) Disperse ammonium tetrathiomolybdate into 300g of water, add 20% dilute sulfuric acid until the pH value of the solution is acidified to 2-3, and acidify ammonium tetrathiomolybdate to obtain 38g of molybdenum trisulfide, with a yield of 98.96%;

[0029] 3) Molybdenum trisulfide is placed in a dynamic tubular oxygen-free atmosphere furnace to control the temperature of 200°C to undergo disproportionation reaction, and 31.6g of molybdenum disulfide is obtained b...

Embodiment 2

[0031] A preparation method of high-purity molybdenum disulfide, comprising the following steps:

[0032] 1) Using 19.6g of ammonium molybdate and 22.4g of elemental sulfur as raw materials, co-heating reaction in 254.8g of ionic liquid (1-ethyl-3-methylimidazolium tetrafluoroborate), the temperature of co-heating reaction is 360°C , time 1 hour, after the reaction was completed, filtered while hot to obtain a filter cake which was 26.01 g of ammonium tetrathiomolybdate intermediate product, with a yield of 99.9%. The filtrate is cooled and crystallized and filtered to obtain excess elemental sulfur 9g and return to use;

[0033] 2) Disperse ammonium tetrathiomolybdate into 200g of water, add 20% dilute sulfuric acid to acidify to pH 2-3, acidify ammonium tetrathiomolybdate to obtain 19.02g of molybdenum trisulfide, yield 99.06%;

[0034] 3) Molybdenum trisulfide is placed in a dynamic tube-type oxygen-free atmosphere furnace to control the temperature of 300°C to undergo a d...

Embodiment 3

[0036] A preparation method of high-purity molybdenum disulfide, comprising the following steps:

[0037] 1) Using 29.4g of ammonium molybdate and 48g of elemental sulfur as raw materials, co-heating reaction in 294g of ionic liquid (1-ethyl-3-methylimidazolium hexafluorophosphate), the temperature of co-heating reaction is 280°C, and the time is 5 hour, after the reaction was completed, filtered while hot to obtain a filter cake which was 38.69 g of ammonium tetrathiomolybdate intermediate product, with a yield of 99.1%. The filtrate is cooled and filtered to obtain 28.6g of solid elemental sulfur, which is recycled;

[0038] 2) Disperse ammonium tetrathiomolybdate into 300g of water, add 20% dilute sulfuric acid for acidification, acidify ammonium tetrathiomolybdate to obtain 28.4g of molybdenum trisulfide, yield 98.6%;

[0039] 3) Molybdenum trisulfide is placed in a dynamic tubular oxygen-free atmosphere furnace to control the temperature of 450°C to undergo disproportion...

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Abstract

The invention belongs to the technical field of molybdenum disulfide preparation, and particularly relates to a preparation method of high-purity molybdenum disulfide. The method comprises the following steps: taking ammonium molybdate and elemental sulfur as raw materials, carrying out a co-thermal reaction in an ionic liquid, and performing filtering after the reaction is finished to obtain an ammonium tetrathiomolybdate intermediate product; acidifying the ammonium tetrathiomolybdate intermediate product to obtain molybdenum trisulfide; and desulfurizing molybdenum trisulfide to obtain molybdenum disulfide. The elemental sulfur is used as a thio compound, the elemental sulfur is generated when molybdenum trisulfide is desulfurized and converted into molybdenum disulfide, the elemental sulfur can be recycled to the reaction to serve as a raw material, material waste is avoided, and the production cost is further reduced.

Description

technical field [0001] The invention belongs to the technical field of molybdenum disulfide preparation, and in particular relates to a preparation method of high-purity molybdenum disulfide. Background technique [0002] Molybdenum disulfide black is slightly silvery gray, has metallic luster, feels greasy to the touch, is insoluble in water, and is an important solid lubricant, especially suitable for high temperature, high pressure, low temperature, and high vacuum environments. Molybdenum disulfide products have the advantages of good dispersibility and non-sticking. They can be added to various oils to form a colloidal state that will never stick, which can increase the lubricity and extreme pressure of the oil; it is also suitable for high temperature, high pressure, The mechanical working state of high speed and high load prolongs the life of the equipment. [0003] Existing preparation of MoS 2 Materials methods can be mainly divided into two categories: physical m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/06
CPCC01G39/06C01P2006/80Y02P20/54
Inventor 成兰兴赵怡丽牛海涛孟炳楠赵腾飞刘巧丽
Owner 洛阳申雨钼业有限责任公司
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