反应详情

A flask equipped with a stirrer, thermometer, and nitrogen inlet tube was charged with 4.4 grams (0.01 mol) of 2,2-bis(3,4-benzenedicarboxylic anhydride)perfluoropropane and 26.5 grams (0.09 mol) of 3,3',4,4'-biphenyltetracarboxylic dianhydride as a tetracarboxylic dianhydride component and 400 grams of N-methyl-2-pyrrolidone as a solvent. To the flask was added dropwise 69 grams of an N-methyl-2-pyrrolidone solution containing 20.8 grams (0.08 mol) of 1,2-bis(γ-aminopropyldimethylsilyl)ethane and 8.2 grams (0.02 mol) of 2,2-bis[4-(4-aminophenoxy)phenyl]propane as a diamine component while the temperature of the reaction system was controlled so as not to exceed 50° C. After dropwise addition, the reaction mixture was stirred for a further ten hours at room temperature. Then the flask was equipped with a reflux condenser connected to a water collecting container and 30 grams of xylene was added to the flask. The reaction system was heated to 160° C. and maintained at the temperature for four hours to effect reaction. There was obtained a polyimide resin solution which was yellowish brown and clear. During the reaction, 3.4 grams of water formed as a by-product. The polyimide resin solution was poured into methanol from which the polyimide resin was precipitated again and isolated. Vacuum drying at 60° C. for 24 hours yielded 52.8 grams of a polyimide resin.

1. customA flask equipped with a stirrer
2. customto exceed 50° C
3. additionAfter dropwise addition
4. customThen the flask was equipped with a reflux condenser
5. additionwas added to the flask
6. temperatureThe reaction system was heated to 160° C.
7. temperaturemaintained at the temperature for four hours
8. customreaction