Styrene → Isobutylene styrene

Temperatur

-70 °C

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 charged. After cooling the reaction vessel to −70° C., 0.35 mL of α-picoline (2-methylpyridine) and 179 mL of isobutylene were added. Further, 9.4 mL of titanium tetrachloride was added to start polymerization, and then the solution was reacted for 2.0 hours while being stirred at −0.70° C. Next, 59 mL of styrene was added into 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 and the like 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.

1. customIn a 2 L reaction vessel
2. customequipped with a stirrer
3. custompolymerization
4. customthe solution was reacted for 2.0 hours
5. customthe reaction was terminated
6. additionby adding a large amount of methanol
7. customAfter removing the solvent
8. dissolutionthe like from the reaction solution, a polymer was dissolved in toluene
9. washwashed twice with water
10. additionThis toluene solution was added to the methanol mixture
11. customprecipitating a polymer
12. dry with materialthe resultant polymer was dried at 60° C. for 24 hours

ORD-Eintrag

ord-f2758879c9dc4ea1bb005ab901567eac

Quelldatensatz

uspto-grants-2014_02

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08656973B2