Method for preparing graphene solution based on supercritical carbon dioxide induction solution phase transformation technology

A graphene solution and carbon dioxide technology, applied in the production of bulk chemicals and other directions, can solve problems such as graphene, and achieve the effects of simple and easy method, good development prospects, and easy availability of raw materials

Active Publication Date: 2014-11-05
ZHENGZHOU UNIV
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  • Abstract
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  • Application Information

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Problems solved by technology

However, limited applications of supercritical fluid properties only yield thin graphene sheets rather than large-scale graphene sheets.
[0004] It has been reported that a graphene-based composite material was prepared by long-time ultrasonication of a surfactant (Lotya. M. et al. J. Am

Method used

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  • Method for preparing graphene solution based on supercritical carbon dioxide induction solution phase transformation technology
  • Method for preparing graphene solution based on supercritical carbon dioxide induction solution phase transformation technology
  • Method for preparing graphene solution based on supercritical carbon dioxide induction solution phase transformation technology

Examples

Experimental program
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Example Embodiment

[0018] Example 1

[0019] Dissolve 200 mg of PVP in 10ml of deionized water, then dissolve 50 mg of graphite powder in the above solution, and sonicate the prepared solution in a cold water bath (10℃) under 240W power for 3h to make the graphite mixed evenly in the solution ; Quickly transfer the solution after 3 hours of ultrasound to a 50ml autoclave, and fill the reactor with carbon dioxide. The flow rate of the carbon dioxide is 150 ml / h, and the solution is kept under pressure at 40℃ and 16MPa for 3h At the same time, stir the solution to make the solution fully contact with supercritical carbon dioxide. After the reaction, the carbon dioxide in the reactor is slowly emptied within 1h; the solution in the reactor is taken out and ultrasonicated in a 240W power cold water bath (10℃) 2h; then centrifuge the solution at 3000 rpm for 45 min, and take out the supernatant, which is the graphene solution.

[0020] Take a drop of graphene solution and drop it on the micro-grid. After...

Example Embodiment

[0022] Example 2-11

[0023] Change the solvent deionized water to ethanol, the volume concentration of ethanol is 10%, 20%, 30%, 40%, 50%, 60%, 70%, 80%, 90%, 95%, and the others are the same as in Example 1. .

[0024]

Example Embodiment

[0025] Examples 12-18

[0026] The pressure of introducing carbon dioxide was adjusted to 6 MPa, 8 MPa, 10 MPa, 12 MPa, 14 MPa, 18 MPa, 20 MPa, and the others were the same as in Example 1.

[0027]

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Abstract

The invention belongs to the technical field of graphene preparation, and particularly discloses a method for preparing a graphene solution based on a supercritical carbon dioxide induction solution phase transformation technology. The method comprises the following steps: dispersing 25-50mg of graphite and 100-200mg of polyvinyl pyrrolidone into 5-10ml of water or ethanol; putting a dispersion liquid in a supercritical carbon dioxide reaction device; stirring the dispersion liquid at the temperature of 40-45 DEG C and under the pressure of 6-20MPa for reacting for 0.5-7 hours; after the reaction ends, releasing the pressure to the normal pressure; and removing non-stripped graphite from a reaction liquid to obtain the graphene solution. By adopting the method, the problem of difficulty in preparing high-concentration non-defective graphene at present is solved, and high-yield and high quality preparation and functionalization of the graphene are finished in one step. The method is simple and feasible, raw materials are cheap and readily-available, environmental protection is facilitated, and pollution is prevented. Meanwhile, by adopting the polyvinyl pyrrolidone for modifying the graphene with a non-covalent bond, the surface of the graphene contains polymer groups, and the structure of the graphene is not damaged. The graphene solution has very good development prospects in the fields of graphene composite materials, photoelectric functional materials, biological medicine and the like.

Description

technical field [0001] The invention belongs to the technical field of graphene preparation, and in particular relates to a method for preparing a graphene solution based on supercritical carbon dioxide-induced solution phase transition technology. Background technique [0002] Graphene is another new nano-carbon material after fullerene and carbon nanotube, and is currently the most ideal two-dimensional nano-material. Due to its excellent physical and chemical properties, graphene has excellent performance in mechanics, electricity, optics and heat, and has great application prospects in the fields of electronics, biomedicine and energy. However, in order to realize the application of graphene, large-scale preparation of graphene must be realized. In recent years, people have made certain developments in the preparation of graphene, such as mechanical exfoliation (Novoselov, K.S. et al. Science 2004, 306, 666), crystal epitaxial growth (Berger, C. et al. J Phys Chem B ...

Claims

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Application Information

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IPC IPC(8): C08L39/06C08K3/04C01B31/04
CPCY02P20/54
Inventor 许群徐珊珊王楠赵阳
Owner ZHENGZHOU UNIV
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