反应详情

温度

-20 °C

A 400-mL pressure vessel was loaded with 100 ml of deionized water and 10 mL of bis(perfluoro-n-butyl) sulfide containing 0.2 ml of ~15% [(CF3)2CF]2CCF2CF3 radical in [(CF3)2CF]2C=CFCF3 precursor (K. Scherer et al., J. Am. Chem. Soc., 1985, 107, 718). The pressure vessel was then chilled and maintained around -20° C. while pulling the air off with a vacuum pump and finally adding 50 g of tetrafluoroethylene. Polymerization set in during warm up, exotherming from 464 psi at 63° C. to 456 psi at 99° C. over a 13-minute period. The pressure thereafter dropped, falling to 17 psi four to five hours later at 101° C. The product was washed once with 200 mL of 1:1 methanol:water and twice with 200 mL of Freon® 113, filtered, and dried under vacuum, giving 49.8 g of white powder (~100% conversion). Under melt indexer conditions, no melt flow was observed at 372° C. with a 15-kg weight.

1. temperatureThe pressure vessel was then chilled
2. customPolymerization
3. temperatureduring warm up
4. waitexotherming from 464 psi at 63° C. to 456 psi at 99° C. over a 13-minute period
5. additionThe pressure thereafter dropped
6. customfalling to 17 psi four to five hours later at 101° C
7. washThe product was washed once with 200 mL of 1:1 methanol
8. filtrationwater and twice with 200 mL of Freon® 113, filtered
9. customdried under vacuum