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Preparing method of graphene powder

A graphene powder and graphite technology, applied in the field of graphene powder preparation, can solve the problems of serious environmental protection burden, high cost and low efficiency, and achieve the effects of reducing industrial cost, complete lattice structure and high quality

Active Publication Date: 2018-01-05
HUAQIAO UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the preparation methods of graphene include: mechanical exfoliation method, chemical vapor deposition method (Chemical VaporDeposition, CVD), chemical oxidation-reduction method, electrochemical exfoliation, SiC thermal decomposition method, etc., wherein the chemical oxidation-reduction method based on the Hummers method It is the most mainstream and is used by most laboratories, but the graphene prepared by it has many defects, and its performance is far behind that of high-quality graphene prepared by mechanical exfoliation and CVD.
Moreover, a large amount of waste acid is produced, and the burden on environmental protection is serious
Although the mechanical exfoliation method can relatively completely preserve the integrity of graphene, there are problems of unstable products, low efficiency and high cost.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1) In the Erlenmeyer flask, add 0.1g of graphite, 0.4g of potassium persulfate and 10ml (about 20g) of chlorosulfonic acid in sequence, and stir for 1min to mix evenly; the graphite is natural flake graphite or pyrolytic graphite, and the carbon The content is greater than 90%, the same below.

[0031] 2) Slowly add distilled water dropwise to the system in step 1), and add 1ml of distilled water dropwise in total for reaction, and a mixed solution system is obtained after the reaction is completed;

[0032] 3) Insert the 50W ultrasonic probe into the liquid surface of the mixed solution system obtained in step 2), ultrasonically treat for 2h, wash with distilled water to neutrality, centrifuge at 3000rpm for 10min, remove the unreacted graphite in the lower layer, and collect the wet graphene in the upper layer;

[0033] 4) The wet graphene obtained in step 3) is freeze-dried for 5h to obtain graphene powder.

[0034] figure 1 It is the surface topography figure of t...

Embodiment 2

[0036] 1) In the Erlenmeyer flask, add 0.1g of graphite, 0.4g of ammonium persulfate and 26ml (about 50g) of chlorosulfonic acid in sequence, stir magnetically for 1min and mix well;

[0037] 2) Slowly add distilled water dropwise to the system in step 1), add 5ml of distilled water dropwise in total, and carry out the reaction. After the reaction is completed, a mixed solution system is obtained;

[0038] 3) Insert the 2000W ultrasonic probe into the liquid surface of the mixed solution system obtained in step 2), ultrasonically treat for 5min, wash with distilled water to neutrality, centrifuge at 3000rpm for 10min, remove the unreacted graphite in the lower layer, and collect the wet graphene in the upper layer;

[0039] 4) The wet graphene obtained in step 3) is freeze-dried for 5h to obtain graphene powder.

Embodiment 3

[0041] 1) In the Erlenmeyer flask, add 0.1g of graphite, 3g of potassium bicarbonate and 10ml (about 20g) of chlorosulfonic acid in sequence, stir magnetically for 1min and mix well;

[0042] 2) Slowly add 1ml of distilled water to the system in step 1), stir and react for 5 minutes, and obtain a mixed solution system after the reaction is completed;

[0043] 3) Insert the 50W ultrasonic probe into the liquid surface of the mixed solution system obtained in step 2), ultrasonically treat for 2h, wash with distilled water to neutrality, centrifuge at 1000rpm for 30min, remove the unreacted graphite in the lower layer, and collect the wet graphene in the upper layer;

[0044] 4) The wet graphene obtained in step 3) is freeze-dried for 10 h to obtain graphene powder.

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Abstract

The invention discloses a preparing method of graphene powder. The method includes the following steps of evenly mixing and stirring graphite powder, an intercalation expanding agent and chlorosulfonic acid, adding distilled water, conducting ultrasonic treatment, washing, centrifuging and freeze-drying after the reaction is completed to prepare less-layer graphene powder. Water and chlorosulfonicacid react to induce the rapid decomposition of the intercalation expanding agent to prepare graphene, the reaction is completed rapidly, no oxidization reaction is involved, the structure of the prepared graphene is not damaged, and the sp2 crystal face structure of graphene is complete; the preparing method is simple in preparation process, low in cost and suitable for large-scale industrial production of graphene.

Description

technical field [0001] The invention belongs to the technical field of graphene preparation, and in particular relates to a preparation method of graphene powder. Background technique [0002] Graphene, as a new type of carbon material, has attracted much attention since its discovery in 2004. It has high light transmittance, electrical conductivity and specific surface area, as well as excellent mechanical properties, and has broad application prospects and great commercial value in the fields of composite materials, energy materials, and communications. [0003] At present, the preparation methods of graphene include: mechanical exfoliation method, chemical vapor deposition method (Chemical VaporDeposition, CVD), chemical oxidation-reduction method, electrochemical exfoliation, SiC thermal decomposition method, etc., wherein the chemical oxidation-reduction method based on the Hummers method It is the most mainstream and is used by most laboratories, but the graphene prep...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/184C01B32/19
Inventor 陈国华刘赟杰赵立平
Owner HUAQIAO UNIVERSITY
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