反应详情

温度

2.5 °C

2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane (36.63 g ) and 200 g of N-methyl-2-pyrrolidone (NMP) were sequentially charged into a 1 L round-bottom flask. The mixture was stirred until it was completely dissolved. While maintaining the flask at 0-5° C., 39.98 g of 2,2-bis(3,4-benzenedicarboxylic anhydride) perfluoropropane and 3.28 g of 5-norbornene-2,3-dicarboxylic anhydride (NDA) were added to the mixture. After the resulting mixture was stirred at room temperature for 16 hours, 40 g of toluene was added to the flask. Using a Dean-Stark distillation equipment, the reaction solution was refluxed at 170° C. for 3 hours to complete the reaction. The reaction solution thus prepared was allowed to cool to room temperature, and slowly poured into a 1:4 methanol-water mixture to obtain precipitates. The precipitates were filtered and dried in a vacuum drying oven at 40° C. for 24 hours to obtain 80 g of a soluble polyimide resin. Resin (20 g) thus obtained in powder form was charged into a 1 L round-bottom flask and dissolved in 100 g of N-methyl-2-pyrrolidone (NMP). The resulting solution was cooled on ice and then 2.73 g of triethylamine (TEA) was added thereto, with maintaining the temperature at 0˜5° C. After stirring for 10 minutes, 2.84 g of chloromethylethylether was slowly added to the solution. After the resulting solution was stirred for 3 hours while maintaining at low temperature, triethylammonium chloride salt was filtered off. The filtrate was slowly poured into a 1:2 methanol-distilled water mixture with vigorous stirring to form precipitates as a fine white solid. The precipitates thus formed were filtered and collected, washed with distilled water, and dried in a vacuum oven at 40° C. for 36 hours to prepare 20 g of a soluble polyimide represented by the following Formula, as a white powder:

1. dissolutionwas completely dissolved
2. stirringAfter the resulting mixture was stirred at room temperature for 16 hours
3. distillationa Dean-Stark distillation equipment
4. temperaturethe reaction solution was refluxed at 170° C. for 3 hours
5. customthe reaction
6. customThe reaction solution thus prepared
7. temperatureto cool to room temperature
8. customto obtain
9. customprecipitates
10. filtrationThe precipitates were filtered
11. customdried in a vacuum
12. customdrying oven at 40° C. for 24 hours