Phthalic Anhydride → Phthalamic acid

温度

25 °C

The following example illustrates the synthesis of a phthalimide-terminatedimide polymer with theoretical number average molecular weight of 11,600 g/mole. 3,4'-Oxydianiline (ODA) (47.5 mmole, 9.5117 g) and 1,3-bis(3-aminophenoxy)benzene (APB) (2.50 mmole, 0.7308 g) were dissolvedin N-methylpyrrolidinone (NMP) ( ~ 35 mL) in a flask equipped with a mechanical stirrer, condenser and nitrogen inlet. 3,3',4,4'-Biphenyl tetracarboxylic dianhydride (BPDA) (48.043 mmole, 14.1354 g) and phthalic anhydride (PA) (3.914 mmole, 0.5797 g) were slurried in NMP (~ 35 mL) and were added to the solution. Afterwashing with ~ 30 mL of NMP to provide a 20% solids content reaction, an exotherm of 10°-15° C. was observed. The exotherm quickly subsided and the reaction was stirred at 25° C. for 16 hours to form the phthalamide acid-terminated polyamide acid. The inherent viscosity (ninh) of the phthalamide acid-terminated polyamide acid was 0.54 dL/g in NMP at 25° C. To imidize, toluene (30 mL) was added and the reaction was heated at 160° C. for 24 hours. After cooling, a powder precipitated which was washed twice in water and dried to afford a yellow solid in high yield. The resulting phthalimide-terminated polyimide was insoluble in NMP and had a glass transition temperature 253° C. and melting endotherms at ~ 340 and ~ 373° C. A film cast from the polyamide acid solution and dried one hour each at 100°, 225°, and 371° C. had a Tg of 253° C. and a Tm at 340° C. and 373° C., and was tough and creasible.

1. customequipped with a mechanical stirrer, condenser and nitrogen inlet
2. additionwere added to the solution
3. customan exotherm of 10°-15° C.

ORDレコード

ord-fd14e24632d14bc1a7884eebc4f2d283

出典データセット

uspto-grants-1999_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05866676