تفاعل #331450

ord-f2758879c9dc4ea1bb005ab901567eac

المذيبات

ظروف التفاعل

درجة الحرارة
-70°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىIn a 2 L reaction vessel
  2. 2
    أخرىequipped with a stirrer
  3. 3
    أخرىpolymerization
  4. 4
    أخرىthe solution was reacted for 2.0 hours
  5. 5
    أخرىthe reaction was terminated
  6. 6
    workup.ADDITIONby adding a large amount of methanol
  7. 7
    أخرىAfter removing the solvent
  8. 8
    workup.DISSOLUTIONthe like from the reaction solution, a polymer was dissolved in toluene
  9. 9
    غسيلwashed twice with water
  10. 10
    workup.ADDITIONThis toluene solution was added to the methanol mixture
  11. 11
    أخرىprecipitating a polymer
  12. 12
    تجفيفthe resultant polymer was dried at 60° C. for 24 hours

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08656973B2uspto-grants-2014_02