A kind of high thermal conductivity polyimide film and its production process
A polyimide film and production process technology, applied in the field of high thermal conductivity polyimide film and its production process, can solve the problems of dark color, tear resistance and little improvement in thermal conductivity, etc. Spectral properties, weakening the effect of CTC, and improving the thermal conductivity
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Embodiment 1
[0044] Preparation of diamine monomers:
[0045] Step S1, under the protection of argon, add 4'-chloro-4-nitro-[1,1'-biphenyl]-2-carbonitrile, K 2 HPO 4, N,N-dimethylacetamide, cooled to 0°C, added trifluoromethanesulfonyl chloride, reacted with light source for 7h, added deionized water, extracted twice with ethyl acetate, combined the organic phases and washed with saturated brine , and then dried with anhydrous magnesium sulfate, and the solvent was removed by rotary evaporation to obtain intermediate 1, in which 4'-chloro-4-nitro-[1,1'-biphenyl]-2-carbonitrile, K 2 HPO 4 , The molar ratio of N,N-dimethylacetamide and trifluoromethanesulfonyl chloride is 1:3:50:1, and the wavelength of the light source is 280nm;
[0046] Step S2, add 0.9 mol of intermediate 1, 0.45 mol of sodium sulfide nonahydrate, and 410 mL of N,N-dimethylacetamide into a three-necked flask, and under nitrogen protection, heat up to 170°C for 24 hours, filter, and wash the filter cake with water , dr...
Embodiment 2
[0050] Preparation of diamine monomers:
[0051] Step S1, under the protection of argon, add 4'-chloro-4-nitro-[1,1'-biphenyl]-2-carbonitrile, K 2 HPO 4 , N, N-dimethylacetamide, cooled to 0°C, added trifluoromethanesulfonyl chloride, reacted with light source for 7 hours, added deionized water, extracted twice with ethyl acetate, combined the organic phases and washed with saturated brine , and then dried with anhydrous magnesium sulfate, and the solvent was removed by rotary evaporation to obtain intermediate 1, in which 4'-chloro-4-nitro-[1,1'-biphenyl]-2-carbonitrile, K 2 HPO 4 , The molar ratio of N,N-dimethylacetamide and trifluoromethanesulfonyl chloride is 1:3:50:1, and the wavelength of the light source is 350nm;
[0052] Step S2, add 0.91 mol of intermediate 1, 0.45 mol of sodium sulfide nonahydrate, and 420 mL of N,N-dimethylacetamide into a three-necked flask, and under nitrogen protection, heat up to 170°C for 24 hours, filter, and wash the filter cake with wat...
Embodiment 3
[0056] Preparation of diamine monomers:
[0057] Step S1, under the protection of argon, add 4'-chloro-4-nitro-[1,1'-biphenyl]-2-carbonitrile, K 2 HPO 4 , N,N-dimethylacetamide, cooled to 0°C, added trifluoromethanesulfonyl chloride, reacted with light source for 8h, added deionized water, extracted 4 times with ethyl acetate, combined the organic phases and washed with saturated brine , and then dried with anhydrous magnesium sulfate, and the solvent was removed by rotary evaporation to obtain intermediate 1, in which 4'-chloro-4-nitro-[1,1'-biphenyl]-2-carbonitrile, K 2 HPO 4 , The molar ratio of N,N-dimethylacetamide and trifluoromethanesulfonyl chloride is 1:3:50:1, and the wavelength of the light source is 780nm;
[0058] Step S2, add 0.92 mol of intermediate 1, 0.46 mol of sodium sulfide nonahydrate, and 430 mL of N,N-dimethylacetamide into a three-necked flask, and under nitrogen protection, heat up to 170°C for 24 hours, filter, and wash the filter cake with water ...
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