反应详情

温度

5 °C

In a 500-mL five-necked flask equipped with a thermometer, a stirrer, a nitrogen inlet tube and a cooling tube with a fractionating device, 34.58 g (0.1 mol) of 1,3-bis(4-amino-α,α-dimethylbenzyl)benzene (4,4′-(m-phenylenediisopropylidene)dianiline also known as BisA-M) was dissolved in a solvent (68.65 g of γ-butyrolactone and 17.16 g of N,N-dimethylacetamide) in a nitrogen atmosphere. The obtained solution was cooled to 5° C. in an ice-water bath. While maintaining the temperature at 5° C., 22.62 g (0.1 mol) of 1,2,4,5-cyclohexanetetracarboxylic dianhydride and 0.50 g (0.005 mol) of triethylamine as an imidation catalyst were added at one time. After the addition, the temperature was raised to 180° C. to continue the reflux for 8 h while removing the distillate from time to time. After the completion of the reaction, the inside temperature was lowered to 100° C. by air cooling. Thereafter, the reaction solution was diluted by adding 143.6 g of N,N-dimethylacetamide and cooled while stirring, thereby obtaining a polyimide resin solution having a solid content of 20% by weight. The weight of the polyimide resin solution was 262.47 g and the total amount of the distillate was 4.86 g. A part of the polyimide resin solution was poured into 1 L of methanol to precipitate the polyimide. The polyimide separated by filtration was washed with methanol and then dried at 100° C. for 24 h in a vacuum dryer, thereby obtaining a white powder. In the IR spectrum thereof, the absorptions at 1702 cm−1 and 1772 cm−1 which were characteristic of imido group were found. The logarithmic viscosity of the polyimide was 0.94.

1. temperatureWhile maintaining the temperature at 5° C.
2. additionAfter the addition
3. temperaturethe temperature was raised to 180° C.
4. temperaturereflux for 8 h
5. customwhile removing the distillate from time to time
6. customAfter the completion of the reaction
7. customwas lowered to 100° C. by air
8. temperaturecooling
9. additionThereafter, the reaction solution was diluted
10. temperaturecooled