반응 #929628

반응 방정식

sodium hydroxide

hydrochloric acid

p-acetoxystyrene

azobisisobutylonitrile

→

poly(p-hydroxystyrene)

용매

water

hexane

water

butyl acetate

water

tetrahydrofuran

반응 조건

후처리

1. 1
   workup.STIRRINGThereafter, the mixture was stirred for 5 hours
2. 2
   기타a polymerization reaction
3. 3
   기타the precipitation of a white resin
4. 4
   기타The resin thus obtained
5. 5
   기타was dried
6. 6
   workup.DISSOLUTIONdissolved in 150 ml of methanol
7. 7
   온도The reaction solution was then heated
8. 8
   온도under reflux for 3 hours
9. 9
   기타hydrolysis
10. 10
    기타the precipitation of a white resin
11. 11
    기타The resin thus obtained
12. 12
    여과was collected by filtration
13. 13
    세척washed with water
14. 14
    기타dried
15. 15
    기타The resin thus obtained
16. 16
    workup.STIRRINGwith vigorous stirring
17. 17
    기타The reprecipitation procedure
18. 18
    기타The resin thus obtained
19. 19
    기타was dried at a temperature of 120° C. in a vacuum drier for 12 hours

실험 절차

In 120 ml of butyl acetate was dissolved 32.4 g (0.2 mol) of p-acetoxystyrene. To the solution was then added 0.033 g of azobisisobutylonitrile (AIBN) with stirring in a stream of nitrogen at a temperature of 80° C. every 2.5 hours three times in all. Thereafter, the mixture was stirred for 5 hours to undergo a polymerization reaction. The reaction solution was then poured into 1,200 ml of hexane to cause the precipitation of a white resin. The resin thus obtained was dried, and then dissolved in 150 ml of methanol. To the solution was added a solution of 7.7 g (0.19 mol) of sodium hydroxide in 50 ml of water. The reaction solution was then heated under reflux for 3 hours to undergo hydrolysis. Thereafter, the reaction solution was diluted with 200 ml of water, and then neutralized with hydrochloric acid to cause the precipitation of a white resin. The resin thus obtained was collected by filtration, washed with water, and dried. The resin thus obtained was dissolved in 200 ml of tetrahydrofuran, and added dropwise to 5 liters of ultrapure water with vigorous stirring to reprecipitate. The reprecipitation procedure was then repeated three times. The resin thus obtained was dried at a temperature of 120° C. in a vacuum drier for 12 hours to obtain a poly(p-hydroxystyrene) alkali-soluble resin R-1.

출처