반응 #163425

반응 방정식

methylcyclohexane

cumyl chloride

isobutylene

styrene

→

styrene isobutylene

용매

n-butyl chloride

반응 조건

후처리

1. 1
   기타In a 2 L reaction vessel
2. 2
   기타equipped with a stirrer
3. 3
   기타the solution was reacted for 2.0 hours
4. 4
   기타the reaction was terminated
5. 5
   workup.ADDITIONby adding a large amount of methanol
6. 6
   기타After removing the solvent from the reaction solution
7. 7
   workup.DISSOLUTIONa polymer was dissolved in toluene
8. 8
   세척washed twice with water
9. 9
   workup.ADDITIONThis toluene solution was added to the methanol mixture
10. 10
    기타precipitating a polymer
11. 11
    건조the resultant polymer was dried at 60° C. for 24 hours

실험 절차

In a 2 L reaction vessel equipped with a stirrer, 589 mL of methylcyclohexane (dried over molecular sieves), 613 mL of n-butyl chloride (dried over molecular sieves) and 0.550 g of cumyl chloride were added. After cooling the reaction vessel to −70° C., 0.35 mL of α-picoline(2-methylpyridine) and 179 mL of isobutylene were added. Furthermore, 9.4 mL of titanium tetrachloride was added and the polymerization was initiated, and then the solution was reacted for 2.0 hours while stirring at −70° C. Next, 59 mL of styrene was added to the reaction vessel and the reaction was continued for 60 minutes, and then the reaction was terminated by adding a large amount of methanol. After removing the solvent from the reaction solution, a polymer was dissolved in toluene and washed twice with water. This toluene solution was added to the methanol mixture, thereby precipitating a polymer, and the resultant polymer was dried at 60° C. for 24 hours to obtain a styrene-isobutylene diblock copolymer.

출처