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Method for polymer assisted supercritical stripping of transition metal sulfide

A polymer-assisted, transition metal technology, used in chemical instruments and methods, molybdenum sulfide, tungsten compounds, etc., can solve the problems of long production cycle, surface and end defects, high production cost, and achieve economical and environmental protection in the production process. Less, complete crystal form effect

Inactive Publication Date: 2017-12-05
CHINA UNIV OF PETROLEUM (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chemical vapor deposition method is expected to realize the controllable synthesis of large-area two-dimensional materials, but this method is difficult to scale production, which limits its application
The liquid phase ultrasonic method uses ultrasonic action to insert organic solvents (surface energy is similar to that of layered materials) or surfactant molecules into the interlayer to overcome the cohesive energy density between adjacent layers and achieve peeling, but the preparation During the process, the high-energy ultrasonic effect will cause the size of graphene nanosheets to become smaller, and defects will be introduced on the surface and ends, which limits the application of two-dimensional materials in molecular electronic devices, etc.
The shear-assisted liquid phase exfoliation method uses shear to overcome the van der Waals force between layers to obtain a single-layer or few-layer structure. The main method is mechanical stirring. Large-scale mechanical stirring equipment not only consumes a lot of energy, but also it is difficult to achieve high speed of large-scale mixers. At the same time, there is a dead angle in the reactor.
[0004] It can be seen that the common disadvantages of the current methods for preparing transition metal sulfide two-dimensional nanomaterials are high production costs, great environmental pollution, or long production cycles, and difficulty in large-scale preparation.

Method used

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  • Method for polymer assisted supercritical stripping of transition metal sulfide
  • Method for polymer assisted supercritical stripping of transition metal sulfide
  • Method for polymer assisted supercritical stripping of transition metal sulfide

Examples

Experimental program
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Embodiment 1

[0038] This embodiment provides a method for polyvinylpyrrolidone shear-assisted supercritical stripping of molybdenum disulfide, which adopts a device such as figure 1 As shown, the device comprises a gas cylinder 1, a refrigerator 2, a high-pressure pump 3, a shear-assisted supercritical device 4, a buffer tank 5 and a mechanical pump ( figure 1 not identified in);

[0039] Gas cylinder 1 communicates with refrigerator 2, refrigerator 2 communicates with high-pressure pump 3, high-pressure pump 3 communicates with shearing auxiliary supercritical device 4, shearing auxiliary supercritical device 4 communicates with buffer tank 5, buffer tank 5 communicates with mechanical pump connected, the shear assisted supercritical device 4 is internally provided with a reactor and a heating device, and the volume of the buffer tank 5 is 10 times the volume of the reactor, and the reactor is provided with a stirring shaft and a temperature detector, and the bottom of the stirring shaft ...

Embodiment 2

[0044] This embodiment provides a method for polyvinylpyrrolidone shear-assisted supercritical exfoliation of tungsten disulfide, which uses the device in Example 1 to perform polyvinylpyrrolidone shear-assisted supercritical exfoliation of tungsten disulfide, which specifically includes the following steps:

[0045] Mix 5 grams of multi-layer tungsten disulfide raw materials with a thickness of more than 20 layers and 1 gram of polyvinylpyrrolidone according to the mass ratio and place them in the reaction kettle of the shear-assisted supercritical device 4. The tungsten disulfide raw materials and polyvinylpyrrolidone The dosage accounts for 1 / 4 of the reactor volume, then close the reactor, open the first valve K1 and the second valve K2, the CO in cylinder 1 2 Freezing by refrigerator 2 to form liquid CO 2 , and pass in the reactor of shearing auxiliary supercritical device 4 by high pressure pump 3, until the indication of pressure gauge T2 shows that the pressure in the ...

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Abstract

The invention provides a method for polymer assisted supercritical stripping of transition metal sulfide. The method comprises the following steps: mixing the transition metal sulfide with polyvinylpyrrolidone according to a mass ratio (1-10):1, and placing the obtained mixture in a shearing assisted supercritical device; introducing CO2 into the shearing assisted supercritical device, and carrying out shearing assisted supercritical stripping at a temperature of 32-200 DEG C under a reaction pressure of 8-20 MPa for 10 min to 48 h; and reducing the pressure in the pressure in the shearing assisted supercritical device to half of the reaction pressure or less within 0.1 s after the supercritical stripping, releasing the pressure in the shearing assisted supercritical device to normal pressure, and collecting the above prepared few-layer transition metal sulfide.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial preparation and relates to a method for polymer-assisted supercritical stripping of transition metal sulfides. Background technique [0002] Two-dimensional nanomaterials are a focus research topic in the field of nanomaterials research. In the study of all 2D materials, transition metal sulfides have attracted extensive attention because of the electronic characteristics of superior charge carrier mobility and tunable charge carrier behavior, such as the semiconducting properties and special layered structure of molybdenum disulfide , so that it exhibits many excellent physical and chemical properties, such as large specific surface area, high reactivity, strong adsorption capacity, good catalytic performance, etc., so it is used in lubrication, catalysis, sensing, nano-optoelectronic devices, high-performance composite materials, and Electrochemical hydrogen storage and lithium storage hav...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/06C01G41/00B82Y40/00
CPCB82Y40/00C01G39/06C01G41/00Y02P20/54
Inventor 田晓娟李永峰巫家业李云
Owner CHINA UNIV OF PETROLEUM (BEIJING)
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