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A method for preparing graphene solution based on supercritical carbon dioxide induced solution phase transition technology

A technology of graphene solution and carbon dioxide, which is applied in the production of bulk chemicals, etc., can solve the problems of graphene and other problems, and achieve the effect of simple method, easy availability of raw materials, and cheap raw materials

Active Publication Date: 2016-06-15
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • 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 (Lotya.M.etal.J.Am.Chem.Soc .2009,131,3611;Sun.Z.Y.etal.Chem.Eur.J.2012,18,6792.), but so far, there is no relevant study on the use of supercritical carbon dioxide to induce solution phase Literature reports on the integration of graphene preparation and functionalization through transformation technology

Method used

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  • A method for preparing graphene solution based on supercritical carbon dioxide induced solution phase transition technology
  • A method for preparing graphene solution based on supercritical carbon dioxide induced solution phase transition technology
  • A method for preparing graphene solution based on supercritical carbon dioxide induced solution phase transition technology

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Experimental program
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Effect test

Embodiment 1

[0019] Dissolve 200mg of PVP in 10ml of deionized water, and then take 50mg of graphite powder and dissolve them in the above solution respectively. Ultrasonicate the prepared solution in a cold water bath (10°C) for 3 hours at a power of 240W to mix the graphite evenly in the solution; After 3 hours, the solution was quickly transferred to a 50ml high-pressure reactor, and carbon dioxide was filled into the reactor. Stir to make the solution fully contact with supercritical carbon dioxide. After the reaction, slowly empty the carbon dioxide in the reaction kettle within 1 hour; take out the solution in the reaction kettle, and ultrasonicate it in a 240W power cold water bath (10°C) for 2 hours; then in Centrifuge the solution under the conditions of 3000rpm and 45min, and take out the supernatant, which is the graphene solution.

[0020] Take a drop of graphene solution and drop it on the microgrid, dry it at room temperature and use transmission electron microscope to charac...

Embodiment 2-11

[0022] The solvent deionized water is changed into ethanol, and the volume concentration of ethanol is 10%, 20%, 30%, 40%, 50%, 60%, 70%, 80%, 90%, 95%, and others are all the same as in Example 1 .

Embodiment 12-18

[0024] The pressure of feeding carbon dioxide is adjusted to 6MPa, 8MPa, 10MPa, 12MPa, 14MPa, 18MPa, 20MPa respectively in turn, and the others are the same as in Example 1.

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Abstract

The invention belongs to the technical field of graphene preparation, and specifically discloses a method for preparing a graphene solution based on a supercritical carbon dioxide-induced solution phase transition technology. Disperse 25-50mg of graphite and 100-200mg of polyvinylpyrrolidone in 5-10ml of water or ethanol, and then place the dispersion in a supercritical carbon dioxide reaction device at 40-45°C and 6-20MPa Stir the reaction for 0.5-7h, release the pressure to normal pressure after the reaction, and remove unexfoliated graphite from the obtained reaction solution to obtain a graphene solution. The invention solves the problem that the current high-concentration defect-free graphene is difficult to prepare, and realizes one-step completion of high-yield, high-quality preparation and functionalized graphene. The method is simple and easy, the raw materials are cheap and easy to obtain, and it is environmentally friendly and pollution-free. At the same time, the polyvinylpyrrolidone non-covalently modified graphene makes the surface of graphene have polymer groups, does not destroy the structure of graphene, and also makes it in graphite It has good development prospects in the fields of olefin composite materials, photoelectric functional materials, and biomedicine.

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.etal. JPhysChemB 2004,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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