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A method for preparing graphene based on thermal cracking of template-solid carbon source

A technology of solid-phase carbon source and template agent, which is applied in the direction of graphene, chemical instruments and methods, nano-carbon, etc., can solve the difficulty of controlling the size and shape of the final product graphene, narrow selection range of solid-phase carbon source, and high production efficiency Low-cost problems, to achieve the effect of low production cost, high safety, simple operation

Active Publication Date: 2020-07-28
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Invention patent CN 103663441 B discloses a method involving the preparation of nano-metal graphene materials using phthalocyanine compounds, phthalocyanine polymers and their derivatives as starting materials, although the final product is obtained under the action of a specific metal catalyst , the process is relatively simple, but the cracking time required by this method is longer and the selection range of its solid-phase carbon source is narrower, and the preparation efficiency is lower; the patent CN104370285A discloses a macro-preparation of high-quality graphene using biomineralized materials The method of the biomineralization material (such as diatomaceous earth) is calcined at a high temperature, and then the carbon source is deposited on it to obtain graphene. Although this method is efficient and environmentally friendly, it requires an additional supply of hydrogen when using a gas-phase carbon source. Atmosphere, the size and shape of the final product graphene are difficult to control

Method used

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  • A method for preparing graphene based on thermal cracking of template-solid carbon source
  • A method for preparing graphene based on thermal cracking of template-solid carbon source
  • A method for preparing graphene based on thermal cracking of template-solid carbon source

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Embodiment 1

[0033] A method for preparing graphene based on thermal cracking of template-solid-phase carbon source, the steps are as follows:

[0034] (1) pickling treatment, adopting the mixed acid of sulfuric acid and nitric acid whose volume ratio is 1 / 2 to carry out pickling treatment on diatomite with a particle size of 20-51nm, the SEM picture of raw diatomite is as follows figure 1 shown;

[0035] (2) Melt blending, the diatomite powder after pickling treatment is melt blended with PP with a number average molecular weight of 20,000 to 40,000, the temperature of melt blending is 54°C higher than the melting point of PP, and the diatomite powder is mixed with The ratio of the mass ratio of PP is 1 / 9;

[0036] (3) Thermal cracking, heat up to 1000°C under the protection of argon at a flow rate of 100sccm and then keep warm for 100min to obtain a composite material of graphene / template agent, wherein the thermal cracking is carried out in a tube furnace, and the heating rate is 10°C / ...

Embodiment 2

[0040] A method for preparing graphene based on thermal cracking of template-solid-phase carbon source, the steps are as follows:

[0041] (1) pickling treatment, adopting nitric acid to carry out pickling treatment to the montmorillonite whose particle size is 500~1300nm;

[0042] (2) Melt blending, the montmorillonite powder after pickling treatment is melt blended with PE with a number average molecular weight of 20,000 to 30,000, the temperature of melt blending is 70°C higher than the melting point of PE, and the montmorillonite powder is mixed with PE The ratio of the mass ratio of PE is 3 / 17;

[0043] (3) Thermal cracking, heat up to 800°C under the protection of argon at a flow rate of 150sccm and then keep warm for 5min to obtain a composite material of graphene / template agent, wherein thermal cracking is carried out in a tube furnace, and the rate of heating is 18°C / min;

[0044] (4) Remove the template agent, wash the graphene / template agent composite material wi...

Embodiment 3

[0047] A method for preparing graphene based on thermal cracking of template-solid-phase carbon source, the steps are as follows:

[0048] (1) pickling treatment, adopting hydrochloric acid to carry out pickling treatment to the kaolin that particle diameter is 1800nm;

[0049] (2) Solution blending, the kaolin powder after the pickling treatment is blended with the PAN solution with a number average molecular weight of 20,000 to 25,000, and the ratio of the mass ratio of the kaolin powder to PAN is 3 / 9;

[0050] (3) Thermal cracking, heat up to 900°C under the protection of argon at a flow rate of 160sccm and then keep warm for 52min to obtain a composite material of graphene / template agent, wherein thermal cracking is carried out in a tube furnace, and the rate of heating is 30°C / min;

[0051] (4) Remove the template agent, wash the graphene / template agent composite material with hydrofluoric acid and freeze-dry to obtain graphene, wherein the freeze-drying temperature is ...

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Abstract

The invention relates to a method for preparing graphene on the basis of template agent-solid phase carbon source thermal cracking. The method comprises the following steps of (1) acid washing treatment: using sulfuric acid, nitric acid, hydrochloric acid or mixed acid of two acids from sulfuric acid, nitric acid, hydrochloric acid for performing acid washing treatment on template agent powder; (2) melting or solution mixing: performing melting or solution mixing on the template agent powder subjected to the acid washing treatment and the solid phase carbon source; (3) thermal cracking: underthe inert gas protection, raising the temperature to a thermal cracking temperature; performing heat insulation to obtain a composite material of the graphene / template agent; (4) template agent removal: performing acid washing and freeze drying treatment on the graphene / template agent composite material to obtain graphene. The layer number of the finally prepared graphene powder is 1 to 10; the electric conductivity is 1 to 1000S / cm. The preparation method is simple; the carbon source selection is wide; the low-cost preparation of the graphene can be realized; the prepared graphene and composite material thereof can be directly applied to the fields of functional paint, fiber and the like; wide application prospects are realized.

Description

technical field [0001] The invention belongs to the field of graphene preparation, in particular to a method for preparing graphene based on template agent-solid-phase carbon source thermal cracking. Background technique [0002] Since 2004, a professor of physics at the University of Manchester used a very simple mechanical exfoliation method to successfully separate and observe a single-layer two-dimensional graphene nanocrystal structure from graphite for the first time. Stable existence at non-absolute zero" conclusion, graphene as a new nanomaterial has attracted widespread attention worldwide, and set off a research boom in the fields of basic research and applied research. Single-layer graphene refers to a two-dimensional structure formed by the arrangement of carbon atoms on a layer of dense, wrapped honeycomb crystal lattices, that is, it presents a sp 2 The single-layer honeycomb lattice structure composed of hybridized carbon atoms has a thickness of only 0.335nm...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/184
CPCC01B2204/04C01B2204/22C01P2002/82C01P2004/03C01P2004/04
Inventor 王彪陈彦坤李凤美
Owner DONGHUA UNIV