Preparation method for transparent polyimide/silicon dioxide hybrid film
A technology of transparent polyimide and silicon dioxide, which is applied in the field of polymer materials, can solve the problems that it is difficult to meet the basic requirements of transparent materials, limit the application of polyimide, and low light transmittance, and achieve excellent light transmittance, High light transmittance, high dispersion effect
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[0013] The preparation method of the transparent polyimide / silicon dioxide hybrid film that the present invention proposes comprises the following steps:
[0014] (1) equimolar 2,2'-bis(trifluoromethyl)diaminobiphenyl and 4,4'-bis(3-aminophenoxy)diphenylsulfone are dissolved in a polar solvent, and Stir to dissolve at room temperature, then add 4,4'-(hexafluoroisopropylene) diphthalic anhydride, the addition ratio is: 4,4'-(hexafluoroisopropylene) diphthalic anhydride and 2,2'-bis(trifluoro The molar ratio of methyl) diaminobiphenyl is (2.1~2.8): 1, stirring reaction 12 hours, obtain polyamic acid solution, wherein the consumption of polar solvent is 20wt% by the solid content in the polyamic acid solution calculate;
[0015] (2) Add 3-aminopropyltriethoxysilane in the polyamic acid solution of the above-mentioned step (1), and the addition ratio is: the content of the 3-aminopropyltriethoxysilane is as high as that in the above-mentioned step (1). 4, 5 mol% to 50 mol% of th...
Embodiment 1
[0020] Dissolve 2.88g (0.009mol) of 2,2'-bis(trifluoromethyl)diaminobiphenyl and 3.89g (0.009mol) of 4,4'-bis(3-aminophenoxy)diphenylsulfone in In 75g of N-methyl-2-pyrrolidone, after being completely dissolved, add 10g (0.023mol) 4,4'-(hexafluoroisopropene) diphthalic anhydride to the above solution at room temperature, stir for 12 hours, add 1.99g ( 0.009mol) 3-aminopropyltriethoxysilane, stirred for 6 hours to obtain a polyamic acid solution containing siloxane end groups, then added 2.86g orthosilicate ethyl ester and 1.88g of 0.1mol / L hydrochloric acid, continue to stir and react for 6 hours to obtain a mixed solution. After the reaction, spread the mixed solution on a flat plate, then dry at 80°C for 2 hours, cure at 150°C for 1 hour, cure at 250°C for 1 hour, and cure at 300°C for 1 hour. Hours, after cooling down to room temperature, the plate was placed in water to peel off the film to obtain a transparent polyimide / silicon dioxide hybrid film.
[0021] The polyimid...
Embodiment 2
[0023] Dissolve 2.88g (0.009mol) of 2,2'-bis(trifluoromethyl)diaminobiphenyl and 3.89g (0.009mol) of 4,4'-bis(3-aminophenoxy)diphenylsulfone in In 75g of N,N-dimethylformamide, after being completely dissolved, add 10g (0.023mol) 4,4'-(hexafluoroisopropylene) diphthalic anhydride to the above solution at room temperature, stir for 12 hours, add 1.99g (0.009mol) 3-aminopropyltriethoxysilane, stirred for 6 hours to obtain a polyamic acid solution containing siloxane end groups, then added 5.72g orthosilicate ethyl ester and 1.88g of 0.1mol / L hydrochloric acid, continue to stir and react for 6 hours to obtain a mixed solution. After the reaction, spread the mixed solution on a flat plate, then dry at 80°C for 2 hours, cure at 150°C for 1 hour, cure at 250°C for 1 hour, and cure at 300°C After cooling down to room temperature for 1 hour, the plate was placed in water to peel off the film to obtain a transparent polyimide / silicon dioxide hybrid film.
[0024] The polyimide / silico...
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