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Method for supercritical fluid in-situ preparation of graphene/fluoropolymer composite material

A supercritical fluid, in-situ preparation technology, applied in the field of supercritical fluid in-situ preparation of graphene/fluoropolymer composite materials, can solve the problems of difficulty in dispersion, agglomeration, easy stacking, etc., and achieves low cost, mild conditions, and low cost. The effect of simple process

Active Publication Date: 2015-01-07
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the graphene obtained by using this technology also has problems such as easy stacking and agglomeration, and difficulty in dispersing during use.

Method used

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  • Method for supercritical fluid in-situ preparation of graphene/fluoropolymer composite material
  • Method for supercritical fluid in-situ preparation of graphene/fluoropolymer composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 10 parts of DMF, 1 part of natural graphite powder and 100 parts of 1,1-dihydroperfluorooctyl acrylate (FOA) were mixed ultrasonically for 5 minutes until uniform, and then added to a high-pressure mixer. Pump 300 parts of liquid supercritical carbon dioxide into a high-pressure mixer and mix evenly, then send the mixture to a high-pressure reactor. The temperature in the autoclave was increased to 31° C., the pressure was controlled between 7 and 10 MPa, and kept for 6 hours. Add 1 part of azobisisobutyronitrile (AIBN) into the autoclave, raise the temperature of the autoclave to 50° C., and control the pressure between 15 and 30 MPa. After the material stays in the autoclave for 36 hours, it is quickly sprayed into the normal pressure production tank; after the carbon dioxide and organic solvent in the production tank are removed, the final product is obtained.

Embodiment 2

[0033] Mix 5 parts of DMF, 1 part of expanded graphite powder and 200 parts of 1,1-dihydroperfluorooctyl methacrylate (FOMA), mix it with mechanical stirring for 1 hour until uniform, and then add it to the high-pressure mixer . Pump 500 parts of liquid supercritical carbon dioxide into a high-pressure mixer and mix evenly, then send the mixture to a high-pressure reactor. The temperature in the autoclave was raised to 40° C., the pressure was controlled between 8 and 10 MPa, and kept for 6 hours. Put 1 part of azobisisobutyronitrile (AIBN) into the autoclave, and heat the autoclave to 80° C., and control the pressure between 10 and 25 MPa. After the material stays in the autoclave for 48 hours, it is quickly sprayed into the normal pressure production tank. After removing the carbon dioxide and the organic solvent in the product tank, the final product is obtained.

Embodiment 3

[0035] Mix 1 part of DMF, 1 part of expanded graphite powder and 500 parts of 2-(N-methylperfluorooctylsulfonamide) ethyl acrylate (MeFOSEA) by ultrasonic mixing for 200 minutes until uniform, then add to the high-pressure mixer middle. Pump 100 parts of liquid supercritical carbon dioxide into a high-pressure mixer and mix evenly, then send the mixture to a high-pressure reactor. The temperature in the autoclave was raised to 70° C., the pressure was controlled between 30 and 40 MPa, and kept for 24 hours. Add 2 parts of azobisisobutyronitrile (AIBN) into the autoclave, heat the autoclave to 150° C., and control the pressure between 30 and 40 MPa. After the material stays in the autoclave for 36 hours, it is quickly sprayed into the normal pressure production tank. After removing the carbon dioxide and the organic solvent in the product tank, the final product is obtained.

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Abstract

The invention relates to a method for supercritical fluid in-situ preparation of a graphene / fluoropolymer composite material. The method comprises the following steps: dissolving fluoropolymer monomers in a supercritical fluid, simultaneously performing intercalation on graphite by utilizing the supercritical fluid and the polymer monomers, and initiating polymerization reaction by taking the supercritical fluid as a polymerization medium to generate a fluoropolymer so as to promote significant enlargement of spacing intervals between graphite layers, finally and fast strip the graphite after intercalation in a supercritical pressure fast pressure relief process layer by layer and prepare a fluoropolymer conductive and heat-conducting composite material with good dispersion of graphene. Compared with the prior art, according to the graphene / fluoropolymer composite material prepared by the method provided by the invention, due to the wrapping of the fluoropolymer, the re-stacking of graphene layers is avoided, and the problem that graphene is very easy to agglomerate is solved; for the fluoropolymer, by adopting the method, graphene can be uniformly dispersed in a polymer material, and thus a functional novel conductive and heat-conducting composite material is obtained.

Description

technical field [0001] The invention belongs to the technical field of preparation of functional materials, and in particular relates to a method for in-situ preparation of graphene / fluorine-containing polymer composite materials by supercritical fluid. Background technique [0002] At present, the techniques for preparing graphene mainly include CVD method, redox method, etc., but a common problem faced by these preparation methods is the dispersion of graphene during use. Due to the strong attraction of the π-π bond between the graphene planes, the prepared graphene powder is easy to stack layers, which makes the original exfoliated sheets reunite, which is directly reflected in the prepared graphene powder. It is difficult to disperse during use and has poor activity when combined with other complexes. [0003] Fluoropolymers are alkane polymers in which some or all of the hydrogen is replaced by fluorine. It is a kind of special material with excellent weather resistanc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F120/24C08F220/24C08F220/14C08F220/06C08F120/38C08F2/44C08G65/22C08K7/24C08K3/04
CPCY02P20/54
Inventor 高寒阳胡国新
Owner SHANGHAI JIAO TONG UNIV
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