Реакция #79447

ord-b94393dbe5344009b8ce3300b994e782

Реагенты

Нет

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеTo a 2 liter-stainless steel autoclave thoroughly purged with nitrogen, 600 ml of hexane and 300 ml of 1-octene
  2. 2
    workup.ADDITIONwere introduced
  3. 3
    Другоеwas elevated to 60° C
  4. 4
    Другоеpolymerization
  5. 5
    Температураto maintain the total pressure at 3.0 Kg/cm2-G
  6. 6
    Другоеto terminate
  7. 7
    Другоеthe polymerization
  8. 8
    Другоеthe unreacted ethylene was purged out
  9. 9
    ДругоеThe resulting reaction solution
  10. 10
    Другоеto precipitate a polymer
  11. 11
    ДругоеThe polymer was separated by filtration
  12. 12
    Другоеdried overnight under reduced pressure

Методика

To a 2 liter-stainless steel autoclave thoroughly purged with nitrogen, 600 ml of hexane and 300 ml of 1-octene were introduced, and the temperature of the system was elevated to 60° C. Then, 1 mmol of triisobutylaluminum and 0.5 ml (0.001 mmol in terms of Zr) of the catalyst solution prepared above were injected into the autoclave together with ethylene to initiate polymerization. Thereafter, only ethylene was continuously fed to maintain the total pressure at 3.0 Kg/cm2-G, and the polymerization was performed at 70° C. for 60 minutes. Then, a small amount of ethanol was fed to the system to terminate the polymerization, and the unreacted ethylene was purged out. The resulting reaction solution was introduced into a large excess of methanol to precipitate a polymer. The polymer was separated by filtration and dried overnight under reduced pressure, to obtain a long-chain branched ethylene/1-octene random copolymer.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US06713562B2uspto-grants-2004_03