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Method for preparing graphite by compressing CO2 fluid under ultrasonic assistance

An ultrasonic and graphene technology, which is applied in the field of graphene prepared by compressing CO2 fluid assisted by ultrasonic waves, can solve the problems of reduced electrical performance, increased product area, and high cost, and achieves simple and easy post-processing, simple process, and easy operation. The effect of low temperature

Active Publication Date: 2012-07-18
SHANGHAI LEVSON ENTERPRISE GRP
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent (application number: 201110048734.3) discloses "a method for preparing graphene material based on chemical deposition method". Using this method, the product area is relatively increased, and the crystal form is relatively complete, but the temperature is too high, and there is a certain risk sex
Chinese patent (application number: 200910023384.8) discloses a "method for growing graphene epitaxially on 4H-SiC silicon surface" which can increase the area of ​​graphene, but the substrate is expensive and the cost is high, so it is not suitable for mass production
Chinese patent (application number: 201110065030.7) discloses "a method for preparing graphene oxide by chemical exfoliation", which is a relatively mature method at the present stage because of its low cost and simplicity, but because it redoxes graphite, making it Its electrical and other properties are reduced, and it is difficult to prepare high-quality graphene flakes
Therefore, the above methods have certain limitations

Method used

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  • Method for preparing graphite by compressing CO2 fluid under ultrasonic assistance
  • Method for preparing graphite by compressing CO2 fluid under ultrasonic assistance
  • Method for preparing graphite by compressing CO2 fluid under ultrasonic assistance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add a certain amount of graphite powder and sodium lauryl sulfate to the reaction kettle 4, and pass into the compressed CO with a temperature of 35°C and a pressure of 9.0MPa from the side. 2 Fluid, hold pressure for 50min. And simultaneously turn on the ultrasonic instrument 8, the power is controlled at 100W, and the time is 45min. After the reaction is over, take out the material from the kettle, put it into a solution of sodium dodecyl sulfate with a certain concentration, obtain the primary product, and cool it down. Through testing and characterization, the obtained graphene accounts for about 70%, with excellent properties, most of which have a diameter of 0.5 to 2 microns, and the number of layers is about 5 to 9 layers. The transmission electron microscope photos of prepared graphene are as follows figure 1 shown.

Embodiment 2

[0024] Weigh a certain amount of graphite powder and sodium dodecylbenzenesulfonate and add them to the reaction kettle 4, and then feed into the compressed CO with a temperature of 35°C and a pressure of 10.0MPa from the side. 2 Fluid, hold pressure for 45min. And simultaneously turn on the ultrasonic instrument 8, the power is controlled at 250W, and the time is 30min. After the reaction, the materials are taken out and put into a solution of sodium dodecylbenzenesulfonate with a certain concentration to obtain primary products, which are then cooled. Through testing and characterization, the obtained graphene accounts for about 85% and has excellent properties. Most of the graphene has a diameter of 50-500 nanometers, the number of layers is about 3-8 layers, and the single-layer graphene accounts for about 25%.

Embodiment 3

[0026] A certain amount of graphite powder and sodium lauryl sulfate are added to the reaction kettle 4, and supercritical CO with a temperature of 40 ° C and a pressure of 11.0 MPa is introduced from the side. 2 Fluid, hold pressure for 30min. And at the same time turn on the ultrasonic instrument, the power is controlled at 600W, and the time is 20min. After the reaction is finished, the material is taken out and put into a solution of sodium dodecyl sulfate with a certain concentration to obtain the primary product, which is then cooled. Through testing and characterization, the obtained graphene has excellent properties, most of which have a diameter of 20-100 nanometers, and the number of layers is about 2-4, of which single-layer graphene accounts for about 30%.

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Abstract

The invention relates to a method for preparing graphite by compressing CO2 fluid under ultrasonic assistance. CO2 is filled to clearances between graphite layers, and graphite is stripped under the ultrasonic assistance to form the graphite. Compared with the prior art, the method has the advantages of mild experiment condition, short treatment time, low required pressure, high yield, good quality, environment friendliness and suitability for large scale production; and moreover, the method is a physical process, so the perfection of the grapheme is ensured.

Description

technical field [0001] The invention belongs to the field of new nanometer materials, in particular to an ultrasonic-assisted compressed CO 2 Process for preparing graphene from a fluid. Background technique [0002] The two-dimensional material graphene is an allotrope of carbon, and graphite with less than 10 layers is collectively called graphene. Graphene is the new material with the thinnest, lightest, strongest, hardest, highest carrier mobility, and highest current density tolerance found so far. Graphene has good thermal properties, mechanical properties, crystallization properties, and extremely good electrical properties. It is currently the material with the best electrical conductivity. It has a wide range of application prospects and can be used as molecular detection, supercapacitors, thermal interface materials, and integrated circuits. , biological devices, antibacterial substances, etc. [0003] At present, graphene preparation methods mainly include: mec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/19
Inventor 王燕赵亚平王武聪李思宁金鹤阳
Owner SHANGHAI LEVSON ENTERPRISE GRP
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