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Method for preparing nano tungsten disulfide with fullerene structure

A technology of fullerene structure and tungsten disulfide, applied in chemical instruments and methods, tungsten compounds, inorganic chemistry, etc., can solve the problems of long reaction time, complex process and high preparation cost, and achieve short reaction time and high reaction efficiency. , The effect of low preparation cost

Inactive Publication Date: 2011-05-11
CHANGAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above method has the disadvantages of complex process, long reaction time and high preparation cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Sodium tungstate is dissolved in deionized water at room temperature, the concentration range is 10g / 100ml, and the above solution is ion-exchanged with a cationic ion exchange resin to obtain a yellow transparent tungstic acid sol; add the formed tungstic acid sol After adding 2% polyethylene glycol dispersant, it was dried at a temperature of 100° C. to obtain a xerogel.

[0032] The tungstic acid xerogel was reduced with hydrogen at 580°C for 1 hour to obtain low-priced tungsten oxide powder mainly composed of purple-black tungsten dioxide. Mix 10 grams of low-priced tungsten oxide powder with elemental sulfur at a molar ratio of 1:20, and place it in a stainless steel container for high-temperature self-pressurization reaction. The heating temperature of the stainless steel container is 800°C, keep it warm for 1 hour, and then cool it down to room temperature Open the stainless steel reaction vessel to obtain tungsten disulfide powder. XRD detection shows that the ...

Embodiment 2

[0034] Sodium tungstate was dissolved in deionized water at room temperature, the concentration range was 10g / 100ml, and the above solution was ion exchanged with cationic ion exchange resin to obtain yellow transparent tungstic acid sol; the formed tungstic acid sol was added to 5 % dimethyl sulfoxide dispersion stabilizer, dried at a temperature of 100 ° C to obtain a xerogel.

[0035] The tungstic acid xerogel was reduced with hydrogen at 600°C for 1 hour to obtain low-priced tungsten oxide powder mainly composed of purple-black tungsten dioxide. Mix 10 grams of low-priced tungsten oxide powder with elemental sulfur at a molar ratio of 1:30, and place it in a stainless steel container for high-temperature self-pressurization reaction. The heating temperature of the stainless steel container is 750°C, keep it warm for 1 hour, and then cool it down to room temperature Open the stainless steel reaction vessel to obtain tungsten disulfide powder with a particle size of about 10...

Embodiment 3

[0037] Sodium tungstate is dissolved in deionized water at room temperature, the concentration range is 5g / 100ml, and the above solution is ion exchanged with cationic ion exchange resin to obtain yellow transparent tungstic acid sol; the formed tungstic acid sol is added to After adding 1% polyethylene glycol dispersant and 5% dimethyl sulfoxide stabilizer, it was dried at a temperature of 100° C. to obtain a xerogel.

[0038] The tungstic acid xerogel was reduced with hydrogen at 590°C for 1 hour to obtain low-priced tungsten oxide powder mainly composed of black tungsten dioxide. Mix 8 grams of low-priced tungsten oxide powder with elemental sulfur at a molar ratio of 1:20, and place it in a stainless steel container for high-temperature self-pressurization reaction. The heating temperature of the stainless steel container is 850°C, keep it warm for 1 hour, and then cool it down to room temperature Open the stainless steel reaction vessel to obtain tungsten disulfide powder...

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Abstract

The invention discloses a method for preparing nano tungsten disulfide with a fullerene structure. The preparation process adopts a two-step method: firstly, obtaining tungstate sol by acidizing sodium tungstate or exchanging cations through sodium tungstate; adding organic dispersing agent in the tungstate sol; obtaining nano WO[3-x] by adopting hydrogen reduction in a reducing furnace; secondly, after mixing the nano WO[3-x] and elemental sulfur, carrying out self-pressurization reaction in a closed metal vessel to obtain powder material of the nano tungsten disulfide with the fullerene structure. The diameter of the compound nano tungsten disulfide particle with the fullerene structure of the invention is 5 to 100 nanometers; the section diameter of a part of nanotube or rod-like substance in the tungsten disulfide particle is 5 to 100nm with the length over tens of microns. The nano material with the fullerene structure is novel solid lubricant. The method for preparing the nano tungsten disulfide with the fullerene structure has simple process, high production efficiency and low production cost and is suitable for preparing the nano material with the fullerene structure with macroscopic quantity.

Description

technical field [0001] The invention relates to a preparation method of nanometer tungsten disulfide with fullerene structure. Background technique [0002] The research team led by R.Tenne, a scientist from the Weizmann Institute of Science in Israel, invented the fullerene structure nano-tungsten disulfide, and used the fluidized bed process to use the corresponding nano-scale tungsten oxide as the precursor to realize the macroscopic Quantitative synthesis, and applied for patent technology in this area in my country, among which 01806119.2 relates to a device for producing inorganic fullerene (IF) nanoparticles and nanotubes. The invention also relates to a synthetic IF-WO 3 In the method of nanoparticle and nanotube, the nanoparticle is spherical, and its size is 0.01 to 0.5 micron, and the length of the nanotube is 0.1 to hundreds of microns, and its cross-sectional size is up to 200 nanometers. The above method has the defects of complex process, long reaction time a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G41/00
Inventor 赵鹏李东林
Owner CHANGAN UNIV