Preparation method for polyamic acid and method for preparing polyimide by polyamide acid
A polyamic acid and primary amine technology, which is applied in the field of polyimide synthesis, can solve the problems of viscosity, polyimide easy to agglomerate, and polyimide reaction period is long, so as to simplify the synthesis process and ensure dispersion. the effect of shortening the synthesis cycle
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Embodiment 1
[0031] Take 20.0g of diaminodiphenyl ether powder, 55.28g of bisphenol S diether dianhydride powder, 0.15g of triethylhexyl phosphoric acid and 0.38g of tripolyphosphate, add them together to 752.84g of n-hexane, and gradually heat under stirring , Polycondensation reaction at 50°C for 25 hours.
[0032] Filter the system after cooling down to normal temperature, dry at -0.095MPa and 170°C for 3 hours, and then pulverize to obtain light yellow polybisphenol S diether tetracarbonyl diphenyl ether imide resin powder, the product yield is 95.4% .
[0033] Use m-cresol as a solvent to test the intrinsic viscosity of a solution with a concentration of 0.5g of pure resin / 100ml: after dissolving the resin in m-cresol, a clear solution is obtained, and the solution is tested. The intrinsic viscosity of the resin is 0.53dL / g.
Embodiment 2
[0035] Take 10.8g of m-phenylenediamine powder, 52g of bisphenol A diether dianhydride powder, 0.63g of methyl amyl alcohol and 0.50g of tributyl phosphate, and add them together to 418.67g of o-xylene, and gradually heat under stirring conditions, at 60 The polycondensation reaction was carried out at ℃ for 18 hours.
[0036] After the system was lowered to normal temperature, it was filtered, dried at -0.09MPa and 180°C for 4 hours, and pulverized to obtain milky white polybisphenol A diether tetraformyl mphenylene imide resin powder with a product yield of 95.1%.
[0037] Using m-cresol as a solvent, the intrinsic viscosity test is carried out with a solution with a concentration of 0.5g pure resin / 100ml: after dissolving the resin in m-cresol, a clear solution is obtained, and the solution is tested. The intrinsic viscosity of the resin is 0.50dL / g.
Embodiment 3
[0039] Take 41.0g of bisphenol A diether diamine powder, 29.29g of biphenyl dianhydride powder, 0.35g of hydroxypropyl cellulose and 0.77g of triphenyl phosphite, add them together to 390.5g of butyl acetate, and stir Gradually heated and polycondensed at 100°C for 12 hours.
[0040] After the system was lowered to normal temperature, it was filtered, dried at -0.098MPa and 200°C for 5 hours, and crushed to obtain bright yellow polybiphenyltetracarboxylic bisphenol A dietherimide resin powder with a product yield of 94.7%.
[0041]Using m-cresol as a solvent, the intrinsic viscosity test is carried out with a solution with a concentration of 0.5g of pure resin / 100ml: after dissolving the resin in m-cresol, a clear solution is obtained, and the solution is tested. The intrinsic viscosity of the resin is 0.52dL / g.
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