Prepn process of self-holing polyimide with organosilicon block
A technology of polyimide and organosilicon, which is applied in the field of preparation of organosilicon block spontaneous porous polyimide, can solve the problems of complexity, low enough dielectric constant of material, difficulty in control, etc., and achieve stable performance and good transparency Wave performance, effect of low dielectric constant
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Embodiment 1
[0030] Dissolve 100g of diaminomethyl silicone oil (Mn=1000) in 5L of solvent (DMF:THF=1:1) in a stirring vessel, add 218g of PMDA and 198g of ODA and react at 50°C for 2 hours, then add 23.6g of MDI at 40°C The reaction was continued for 4 hours. The reaction was carried out under the protection of nitrogen. Finally, a silicone block polyamic acid solution dispersion of A:B:C:D=1:10:8:1 was prepared, poured out to form a film, and imidized under nitrogen protection at 300°C for 2 hours. The dielectric constant of the material is k=2.5, the Young's modulus is 1.1GPa, the thermal decomposition temperature is greater than 450°C, and it does not swell in water or DMF. The dielectric properties remain unchanged after being placed in a humid environment for 6 months.
[0031] The dielectric analysis of the sample is to first coat the high-purity conductive silver paste on both sides of the sample, and use it as a test electrode after drying, and accurately measure the effective a...
Embodiment 2
[0034] Dissolve 400g of diaminophenyl silicone oil (Mn=2000) in 10L solvent (DMAc:THF=1:1) in a stirring vessel, add 294gBTDA and 118.8gMDA and react at 60°C for 3 hours, then add 34.8g TDI at 50°C The reaction was continued for 5 hours. The reaction was carried out under the protection of argon. Finally, a silicone block polyamic acid solution dispersion of A:B:C:D=1:5:3:1 was prepared, poured out to form a film, and imidized under argon protection at 350°C for 4 hours. The dielectric constant k of the material is 2.6, the Young's modulus is 1.5GPa, the thermal decomposition temperature is greater than 500°C, and it does not swell in water, DMF, or DMAc. The dielectric properties remain unchanged after being placed in a humid environment for 8 months.
[0035] Test method is the same as embodiment 1.
Embodiment 3
[0037] Dissolve 300g of diaminohydrogen-containing methyl silicone oil (Mn=3000) in 2L of solvent (DMSO: DMAc: THF = 1: 1: 2) in a stirred vessel, add 444g of 6FDA and 232.4g of 4,4 6FDAm and react at 70°C After 2.5 hours, 41.6 g of IPDI was added and the reaction was continued for 4 hours at 60°C. The reaction was carried out under the protection of argon. Finally, a silicone block polyamic acid solution dispersion of A:B:C:D=1:10:7:2 was prepared, poured out to form a film, and imidized at 280°C for 2.5 hours under the protection of argon. The dielectric constant of the material is k=2.3, the Young's modulus is 1.2GPa, the thermal decomposition temperature is higher than 400°C, and it does not swell in water, DMF, or DMAc. The dielectric properties remain unchanged after being placed in a humid environment for 3 months.
[0038] Test method is the same as embodiment 1.
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