Fluorine oxidized graphene/polyimide composite material, preparation method and application thereof
A technology of polyimide and composite materials, applied in the field of graphene oxyfluoride/polyimide composite materials and its preparation
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[0039] The present invention also provides a method for preparing graphene oxyfluoride. The method uses graphite oxide as a raw material to prepare the graphene oxyfluoride by using a hydrothermal method.
[0040] In one embodiment of the present invention, the preparation method includes the following steps:
[0041] The graphene oxide fluoride is prepared by mixing graphite oxide, oxidizing agent and hydrofluoric acid for hydrothermal reaction.
[0042]In one embodiment of the present invention, the mass percentage of the graphite oxide in the mixed solution is 2-15wt%; the oxidant in the mixed solution is 3-30wt%; the hydrofluoric acid is The mass percent content of the mixed solution is 3-25 wt %; the balance is water. Preferably, the graphite oxide accounts for 5-10wt% by mass of the mixed solution; the oxidant accounts for 5-25wt% by mass of the mixed solution; the hydrofluoric acid accounts for 5-25wt% by mass of the mixed solution The content is 5-20wt%; the balance ...
Embodiment 1
[0061] Step 1: Preparation of graphene oxyfluoride
[0062] Configure the mixed solution as follows:
[0063] 10g of graphite oxide, 12g of hydrogen peroxide (that is, 40g of hydrogen peroxide with a concentration of 30wt%), 15g of hydrofluoric acid (that is, 50g of hydrofluoric acid with a concentration of 30wt%).
[0064] Mix the above components evenly and add them to a hydrothermal reaction kettle with a polytetrafluoroethylene liner. In a closed environment, keep warm at 150°C for 6 hours. After cooling to room temperature, ultrasonically disperse the reaction solution for 1 hour. Perform high-speed centrifugation, filtration, and freeze-drying to obtain graphene oxyfluoride.
[0065] Step 2: Preparation of graphene oxyfluoride / polyimide composite
[0066] Weigh 1 g of graphene oxyfluoride prepared above, disperse 100 g of diphenyl ether diamine in 40 ml of N-methyl-2-pyrrolidone, ultrasonicate for 1 hour, and stir to form a slurry. When it is lowered to room temperatu...
Embodiment 2
[0070] Step 1: Preparation of graphene oxyfluoride
[0071] Configure the mixed solution as follows:
[0072] Cut and ultrasonically disperse 10 g of fluorinated graphite in 78 mL of water to obtain a uniformly dispersed dispersion containing fluorinated graphene, then add 12 g of sodium hydroxide, and stir until the sodium hydroxide is completely dissolved;
[0073] Transfer the above mixed solution to a hydrothermal reaction kettle with a polytetrafluoroethylene liner, and keep it warm at 160°C for 5 hours in a closed environment. After cooling to room temperature, ultrasonically disperse the reaction solution for 2 hours, then conduct Centrifuge, filter, and freeze-dry to obtain graphene oxyfluoride.
[0074] Step 2: Preparation of graphene oxyfluoride / polyimide composite
[0075] Weigh 3 g of graphene oxyfluoride prepared above, disperse 97 g of diphenyl ether diamine in 120 ml of N-methyl-2-pyrrolidone, ultrasonicate for 1.5 hours, and stir to form a slurry. When it is...
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