A kind of graphene flame retardant film and its preparation method and application
A technology of flame-retardant film and graphene, which is applied in the direction of fire-resistant coatings, etc., can solve the problems of large deformation, poor thermal stability, and less residue, and achieve the effects of small deformation, good thermal stability, and good flame-retardant performance
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preparation example 1
[0053] Preparation Example 1 is used to prepare graphene oxide aqueous solution.
[0054] Examples 1-9 are used to prepare the graphene flame-retardant film of the present invention.
[0055] Preparation Example 1
[0056] Assemble a 250mL reaction bottle in an ice-water bath, add 80mL of concentrated sulfuric acid, add a solid mixture of 3g of graphite powder and 1.5g of sodium nitrate under stirring, then add 9g of potassium permanganate in batches, control the reaction temperature not exceeding 10°C, and stir 30min, then raise the temperature to about 35°C, continue to stir for 30min, then slowly add 150mL of deionized water, continue stirring for 20min, add an appropriate amount of hydrogen peroxide to reduce the residual oxidant, and turn the solution into bright yellow. Filtrate while hot, and wash with 5% by weight of HCl solution and deionized water until no sulfate is detected in the filtrate, put it into a dialysis bag for dialysis, and obtain a graphene oxide solut...
Embodiment 1
[0058] Dissolve 10mg of hexachlorocyclotrimeric phosphazene in 0.5mL of N,N-dimethylformamide, then mix well with 6mL of graphene oxide solution with a concentration of 3.5mg / mL, and pour the well-mixed solution into Form a film precursor in a glass petri dish, dry it at 60°C for 48h, and then use a hot press to reduce it at 800°C for 50min to obtain a graphene flame-retardant film M1 with an average thickness of 21 microns. Same) as can be seen, the content of graphene is 67.7% by weight, and the balance is flame retardant.
[0059] It can be seen from the scanning electron microscope that the internal structure of the graphene flame retardant film M1 is a layered structure.
[0060] figure 1 It is the X-ray powder diffraction pattern of graphene flame-retardant film M1, and the characteristic diffraction peak at 24.8° can be seen, indicating that graphene oxide is reduced to graphene.
[0061] figure 2 is the thermogravimetric analysis diagram of graphene flame retardant...
Embodiment 2
[0065] Dissolve 1.5mg of hexachlorocyclotrimeric phosphazene in 0.3mL of N,N-dimethylformamide, then mix with 6mL of graphene oxide solution with a concentration of 1mg / mL, pour the uniformly mixed solution into A film precursor is formed in a glass petri dish, dried at 50°C for 40h, and then reduced with a hot press at 1000°C for 10min to obtain a graphene flame-retardant film M2 with an average thickness of 6 microns, wherein the content of graphene is 80.0% by weight, and the balance is flame retardant.
[0066] It can be seen from the scanning electron microscope that the internal structure of the graphene flame retardant film M2 is a layered structure.
[0067] X-ray powder diffraction test was performed on the prepared graphene flame-retardant film M2, and a characteristic diffraction peak at 24.8° could be seen, indicating that graphene oxide was reduced to graphene.
[0068] Thermogravimetric analysis of the prepared graphene flame retardant film M2 shows that the gra...
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Abstract
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