反应详情

Into a 500 ml Morton flask equipped with a mechanical stirrer, a reflux condenser, a nitrogen bypass, a pH probe and a phosgene dip tube was placed 6.88 g of resorcinol, 100 ml of methylene chloride, 20 ml of water and 0.5 ml of 75 wt % aqueous methyltributylammonium (MTBA). The pH was adjusted to and maintained at 7 with 25 wt % of NaOH as 29 g of a 35 wt % solution of diacid chlorides (DACS) in methylene chloride (delivers 50 mmol of 50/50 isophthaloyl chloride (IPC)/terephthaloyl chloride (TPC)) was added over 4 minutes. The pH was raised to 10 and 100 μl of triethylamine (TEA), 50 mg of water and 0.21 g of phenol were added. The pH was maintained at 10 and 4.0 g of phosgene was added at 0.5 g/min. The final pH was 10.1. The polymer solution was separated from the brine by centrifugation and washed 1 time with 1N HCl and 3 times with deionized water. The polymer was isolated by hot water crumbing in a blender and collected by filtration and washed with water and dried in a vacuum oven at 110° C. overnight.

1. customInto a 500 ml Morton flask equipped with a mechanical stirrer, a reflux condenser
2. additionwas added over 4 minutes
3. additionwere added
4. additionwas added at 0.5 g/min
5. customThe polymer solution was separated from the brine by centrifugation
6. washwashed 1 time with 1N HCl and 3 times with deionized water
7. customThe polymer was isolated by hot water crumbing in a blender
8. filtrationcollected by filtration
9. washwashed with water
10. customdried in a vacuum oven at 110° C. overnight