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A kind of sulfur-substituted oxidized fluorinated graphene/polyamide composite material and its preparation method and application
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A composite material and fluorine oxide technology, which is applied in the field of sulfur-substituted graphene oxide fluoride and composite materials, sulfur-substituted graphene oxide fluoride/polyamide composite materials, to achieve good mechanical properties, good dispersion, and not easy to agglomerate Effect
Active Publication Date: 2020-06-30
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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[0003] In order to improve the deficiencies of the prior art, one of the objectives of the present invention is to provide a sulfur-substituted oxidized fluorinated graphene and its preparation method and application, the surface of the sulfur-substituted oxidized fluorinated graphene contains active groups, compared to Graphene, which is not easy to agglomerate, has good dispersion in polymers, and can directly form a strong interaction between polymer interfaces to realize the enhancement effect of sulfur-substituted graphene oxide fluoride in polymer-based composites
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Embodiment 1
[0061] Preparation of Sulfur-Substituted Oxyfluorinated Graphene
[0062] Weigh 2g of oxidized fluorinated graphite, put it into a porous plastic tube and stick it on the aluminum or nickel electrode, as the cathode and anode of electrolysis. Add 4.5g of mercaptan as electrolyte, 40ml of ethanol as electrolyte, and 2.0g of tetraethylammonium tetrafluoroborate as electrolytic aid. Under the action of 15V external DC power supply, electrolytic reaction takes 3 hours to obtain evenly dispersed sulfur-substituted oxidative fluorination Graphene solution; the dispersion is subjected to ultrasonic stripping, centrifugation, washing with an organic solvent, filtering, and freeze-drying. Collect samples.
[0063] The mass percentage of sulfur in the prepared sulfur-substituted oxidized fluorinated graphene was 1.26%, the mass percentage of oxygen was 6.7%, and the mass percentage of fluorine was 2.14%.
Embodiment 2
[0065] Preparation of Sulfur-Substituted Oxyfluorinated Graphene
[0066] Weigh 6g of oxidized fluorinated graphite, put it into a porous plastic tube and stick it on the aluminum or nickel electrode, as the cathode and anode of the electrolytic cell. Add 15g of thiourea as electrolyte, 120ml of acetylacetone as electrolyte, and 5.0g of tetraethylammonium tetrafluoroborate as electrolytic aid. Connect the positive and negative electrodes to a DC potentiostat, stir rapidly, and electrolytically peel off the graphite fluoride oxide at a DC potential of 15V for 3 hours to obtain a uniformly dispersed sulfur-substituted graphene oxide fluoride solution. The dispersion was centrifuged, washed with deionized water, filtered, and freeze-dried. Collect samples.
Embodiment 3
[0068] Preparation of sulfur-substituted oxidized fluorinated graphene / polyamide composites
[0069] Weigh 0.5 g of the sulfur-substituted fluorinated graphene oxide prepared in Example 1 above, and ultrasonically disperse it in 300 g of water to form a slurry; then add 500 g of caprolactam, continue ultrasonic dispersion for 30 minutes, and stir for 1 hour. ℃, remove 90wt% of water; move to the reaction kettle, add 2.5g of adipic acid, carry out stirring reaction at 270 ℃ for 2 hours, after the reaction is completed, place it in an oven for curing at 230 ℃ for 3 hours, you can get Sulfur-substituted oxidized fluorinated graphene / polyamide composites.
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Abstract
A thio-substituted oxidative fluorinated graphene / polyimide composite material and a preparation method and application thereof are disclosed. The thio-substituted oxidative fluorinated graphene / polyimide composite material has extremely good mechanical property, excellent heat-conducting property and ultrahigh conductivity. The thio-substituted oxidative fluorinated graphene contains active groupon the surface, is not easy to agglomerate and has good dispersity in a polymer in comparison with graphene, can directly form strong interaction between interfaces of the polymer to realize the reinforced effect of the thio-substituted oxidative fluorinated graphene in a polymer-based composite material. The thio-substituted oxidative fluorinated graphene can be used for preparation of the thio-substituted oxidative fluorinated graphene / polyimide composite material. The thio-substituted oxidative fluorinated graphene and polyamide resin can undergo steps of mixing, ultrasonic treatment, stirring, heating, drying and the like through a one-pot method to prepare the thio-substituted oxidative fluorinated graphene / polyimide composite material. The preparation process is simple and feasible,is convenient to operate, and has strong universality.
Description
technical field [0001] The invention belongs to the technical field of sulfur-substituted oxidized fluorinated graphene and composite materials, and specifically relates to a sulfur-substituted oxidized fluorinated graphene, a sulfur-substituted oxidized fluorinated graphene / polyamide composite material, a preparation method and application of the two. Background technique [0002] In 2004, researchers such as Geim of the University of Manchester peeled off a small amount of graphene from graphite and studied its properties, and found that it had special electronic properties and excellent mechanical, electrical, optical, thermal and magnetic properties, thus setting off graphene application research. upsurge. Graphene has excellent electrical, thermal and mechanical properties. It can be used as an ideal nanofiller for the preparation of high-strength conductive composite materials. It can also be mixed with polymer monomers dispersed in the solution and then polymerized to...
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