反应详情

In a three neck 500 mL round-bottom flask was weighed bisphenol-Z (35.0000 g, 130.42 mmol), potassium carbonate (36.0505 g, 260.45 mmol), 4,4′-difluorobenzophenone (28.4587 g, 130.42 mmol), toluene (115 g) and N,N-dimethylacetamide (233 g). The flask was fitted with a condenser and a thermometer. The light yellow mixture was stirred and heated to reflux. The water formed was azeotropically distilled with toluene. On complete removal of water and toluene, the solution was stirred at reflux for about 2 hours. The viscous polymer solution was precipitated in water, and a white fibrous polymer was isolated by filtration. The white polymer was stirred in boiling water for about 1 hour, filtered, and then stirred in boiling methanol for about 1 hour and filtered. The fibrous white polymer was then dried in an vacuum oven for about 16 hours at 100° C. The yield was about 54.35 g. The number average molecular weight of the polymer was about 11.5K.

1. customThe flask was fitted with a condenser
2. temperatureheated to reflux
3. distillationwas azeotropically distilled with toluene
4. customOn complete removal of water and toluene
5. stirringthe solution was stirred
6. temperatureat reflux for about 2 hours
7. customThe viscous polymer solution was precipitated in water
8. customa white fibrous polymer was isolated by filtration
9. stirringThe white polymer was stirred
10. customfor about 1 hour
11. filtrationfiltered
12. stirringstirred
13. customfor about 1 hour
14. filtrationfiltered
15. customThe fibrous white polymer was then dried in an vacuum oven for about 16 hours at 100° C