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A kind of liquid phase exfoliation preparation method of graphene

A liquid-phase exfoliation and graphene technology, applied in the direction of graphene, single-layer graphene, nano-carbon, etc., can solve the problems of low production efficiency and poor product performance, and achieve low cost, high single-layer ratio and short preparation time short effect

Active Publication Date: 2018-01-19
SHANGHAI HIWAVE COMPOSITE MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to address the deficiencies in the prior art, propose a liquid-phase exfoliation preparation method for graphene, utilize the stripping agent to promote the separation of graphite flakes, prepare the method for high-quality graphene, and solve the low production efficiency of the prior art , poor product performance and other issues, this method is simple to operate, low in cost, green and environmentally friendly, and is expected to realize the industrial production of graphene

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  • A kind of liquid phase exfoliation preparation method of graphene

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Embodiment 1

[0032] The present embodiment provides a liquid phase exfoliation method to prepare graphene, and the basic operation steps are as follows:

[0033] In the first step, a hydroquinone aqueous solution with a concentration of 10 wt % was prepared, and 1 g of expanded graphite was dispersed in 999 g of the solution to obtain a mixed solution of 0.1 wt % graphite.

[0034] In the second step, the mixed liquid in the first step was processed by magnetic stirring for 5 hours to make it uniformly dispersed, and the stirring speed was 500 rpm to obtain the graphite pre-stripping dispersion.

[0035] In the third step, the graphite pre-exfoliation dispersion is subjected to ultrasonic exfoliation for 0.5 hours, and the selected ultrasonic frequency is 10KHz, and a graphene mixed dispersion system is preliminarily obtained.

[0036] The fourth step is to use a centrifuge to centrifuge the graphene mixed dispersion system. The selected centrifuge speed is 5000 rpm, the centrifugation tim...

Embodiment 2

[0040] The main difference from Example 1 is that in Example 2, the stripping agent was replaced, the concentration of graphite dispersion was increased, and the method of ball milling was used for mechanical stripping, and other relevant process parameters were changed at the same time.

[0041] The basic operation steps of graphene prepared by the present embodiment 2 liquid phase exfoliation method are as follows:

[0042] In the first step, a sodium phenoxide aqueous solution with a concentration of 0.5 wt% is prepared, and 1 g of oriented pyrolytic graphite is dispersed in 4 g of the solution to obtain a 20 wt % graphite solution.

[0043] In the second step, use magnetic stirring to process the mixed solution for 0.5 hour to make it uniformly dispersed, and the stirring speed is 2000rpm to obtain the graphite pre-stripping dispersion;

[0044]In the third step, the obtained graphite pre-exfoliation dispersion is poured into a ball mill tank, and zirconia is used as a bal...

Embodiment 3

[0049] The main difference from Example 1 is that in Example 3, the stripping agent solution was replaced, and the method of ultrasonic combined with shear emulsification was used for graphite stripping, and other relevant process parameters were changed at the same time.

[0050] Present embodiment 3 liquid phase exfoliation method prepares the basic operating steps of graphene as follows:

[0051] In the first step, a glycerol solution of catechol with a concentration of 1wt% is prepared, and 1g of graphite oxide powder is dispersed in 9g of the solution to obtain a mixed solution of 10wt% graphite.

[0052] In the second step, magnetic stirring was used to process the mixed liquid for 3 hours to make it uniformly dispersed at a stirring speed of 1000 rpm to obtain a graphite pre-stripping dispersion.

[0053] In the third step, the obtained graphite pre-exfoliation dispersion was subjected to ultrasonic exfoliation for 5 hours, and the selected ultrasonic frequency was 20 k...

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Abstract

The invention provides a liquid-phase stripping preparation method of graphene. The liquid-phase stripping preparation method comprises the steps that first, an aromatic compound is used as a stripping agent to prepare a stripping agent solution, graphite powder is added, and graphite pre-stripping dispersion liquid is obtained after sufficient stirring; second, the graphite pre-stripping dispersion liquid obtained in the first step is subjected to stripping dispersion through ultrasonic and / or mechanical shear to obtain a graphene mixed dispersion system; third, the graphene mixed dispersion system obtained in the second step is centrifuged, the upper-layer solution can be taken for dialysis, and impurities are remove to obtain a pure graphene product. The liquid-phase stripping preparation method can effectively separate graphite flake layers, a large amount of graphene is obtained within a short period of time, and the prepared graphene is single-layer or double-layer graphene and is good in conductive / thermal performance and excellent in comprehensive performances. The liquid-phase stripping preparation method has the advantages of being simple in operation, high in efficiency and green, being environmentally-friendly and the like, and achievement of industrialized graphene preparation is hopeful.

Description

technical field [0001] The invention belongs to the technical field of graphene preparation, in particular to a method for preparing graphene by liquid phase exfoliation. Background technique [0002] Graphene is a regular hexagonal "honeycomb" sheet composed of a single layer of carbon atoms, which has an ideal two-dimensional crystal structure. Graphene has a very large specific surface area (2630m 2 / g) and super large carrier mobility (15000cm 2 / (V·s)), its thermal conductivity can reach 5000W / (m·K). At the same time, it is the strongest among the tested materials, with a strength of 130GPa, which is more than 100 times stronger than steel. As a new type of material with the thinnest, highest strength, and excellent electrical and thermal conductivity discovered so far, graphene is known as the "king of new materials" and has great application prospects in the fields of energy storage, catalysis, electronics, and biomedicine. In this context, the large-scale prepara...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/19
CPCC01B2204/02
Inventor 毛琳王鹏鹏陈乐生
Owner SHANGHAI HIWAVE COMPOSITE MATERIALS CO LTD
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