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Preparation method of high conductivity graphene

A graphene and graphite technology, applied in the field of graphene, can solve problems such as high cost, high equipment requirements, dangerous reaction, etc., and achieve the effects of avoiding pollution, reducing production cost and increasing dispersion speed.

Inactive Publication Date: 2017-12-01
SHANDONG OBO NEW MATERIAL CO LTD
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Problems solved by technology

An article "FeCl" reported on Scientific Reports in 2013 3 Few-Layer Graphene Prepared by Intercalation》via FeCl 3 Intercalated graphite, followed by chemical expansion with hydrogen peroxide, prepares high-quality few-layer graphite, but the intercalation reaction needs to be carried out under high temperature and high pressure, which has problems such as high equipment requirements, dangerous reaction and high cost.

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[0040] The invention provides a kind of preparation method of graphene, is characterized in that, comprises the following steps:

[0041] A) graphite, chromium trioxide and concentrated hydrochloric acid are reacted to obtain an intercalated graphite compound;

[0042] B) after mixing the intercalated graphite compound obtained by the above steps with hydrogen peroxide, obtain expanded graphite;

[0043] C) exfoliating the expanded graphite obtained in the above steps in the water phase to obtain graphene.

[0044] In the invention, graphite, chromium trioxide and concentrated hydrochloric acid are firstly reacted to obtain intercalation graphite compound.

[0045] The present invention has no special restrictions on the selection of the graphite, and the graphite materials well known to those skilled in the art can be used. Those skilled in the art can select and adjust according to actual production conditions, product requirements and quality requirements. The graphite of ...

Embodiment 1

[0073]Put 1g of expandable graphite (100 mesh, carbon content > 70%), 8.5g of chromium trioxide into a 100ml round bottom flask, add 7ml of concentrated hydrochloric acid (12mol / L), seal it, and add a tail gas absorption device (with chlorine gas generated , saturated NaOH absorption), the reaction system was stirred at 25°C for 10h, filtered, washed with pure water to remove unreacted concentrated hydrochloric acid and chromium trioxide, and vacuum-dried at 60°C for 12h to obtain graphite intercalation compound (GIC).

[0074] The intercalated graphite compound prepared in Example 1 of the present invention was characterized.

[0075] see figure 1 , figure 1 XRD diffraction patterns of the graphite used in Example 1 of the present invention and the prepared intercalated graphite compound (GIC).

[0076] From figure 1 It can be seen from the graph that the crystal structure of graphite changed significantly before and after intercalation, indicating that the intercalation w...

Embodiment 2

[0087] Put 1g of expandable graphite (50 mesh, carbon content > 75%), 5g of chromium trioxide into a 100ml round bottom flask, add 7ml of concentrated hydrochloric acid (10mol / L), seal, and add a tail gas absorption device (chlorine gas is generated, saturated NaOH absorption), the reaction system was stirred at 30°C for 5h, filtered, washed with pure water to remove unreacted concentrated hydrochloric acid and chromium trioxide, and vacuum-dried at 70°C for 6h to obtain graphite intercalation compound (GIC).

[0088] Put 0.2gGIC into 20ml of hydrogen peroxide, immerse and stand at 25°C for 24h, filter, and wash with pure water to obtain worm-like graphite aggregates (CEWG).

[0089] Finally, 0.1 g of CEWG obtained was added to 100 ml of an aqueous solution containing sodium dodecylbenzene sulfonate, wherein the concentration of sodium dodecylbenzene sulfonate was 0.2 mol / L, and ultrasonically treated at 2000 W for 2 hours to obtain graphene. After calculation and detection, t...

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Abstract

The invention provides a preparation method of graphene. The preparation method comprises the following steps: firstly, performing a reaction on graphite, chromium trioxide and concentrated hydrochloric acid to obtain an intercalated graphite compound; then mixing the intercalated graphite compound obtained in the previous step with hydrogen peroxide to obtain expanded graphite; and finally, peeling the expanded graphite obtained in the previous step in an aqueous phase to obtain the graphene. In order to overcome the defect of high temperature and high pressure of an existing conventional graphene liquid phase peeling method, a graphene preparation method of low-temperature intercalation, low temperature expansion and aqueous phase peeling is creatively achieved by optimizing and combining raw materials and refining the reaction steps by means of a low-temperature constant-pressure liquid phase peeling method. Therefore, the production cost is lowered, the environmental pollution caused by an organic solvent is also avoided, and the dispersing speed of graphene is also increased.

Description

technical field [0001] The invention belongs to the technical field of graphene, and relates to a preparation method of high-conductivity graphene, in particular to a low-temperature preparation method of high-conductivity graphene. Background technique [0002] Graphene is a new material with a single-layer sheet structure composed of carbon atoms. It is a carbon atom with sp 2 The hybridized orbitals form a hexagonal planar film with a honeycomb lattice, a two-dimensional material with a thickness of only one carbon atom. Since Geim et al first prepared graphene by micromechanical exfoliation method in 2004, graphene has attracted widespread attention because of its excellent properties such as high conductivity, high specific surface area, high strength and high electron mobility. In turn, it also promotes the rapid development of graphene preparation technology. It is precisely because of the above-mentioned excellent physical and chemical properties that it is widely...

Claims

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Application Information

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IPC IPC(8): C01B32/19
CPCC01P2004/03C01P2006/12C01P2006/40
Inventor 赵永彬张在忠姜彤彤李晓斐
Owner SHANDONG OBO NEW MATERIAL CO LTD
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