Reaktion #79447

ord-b94393dbe5344009b8ce3300b994e782

Reaktionsgleichung

CCO
ethanol
CC(C)[CH2][Al]([CH2]C(C)C)[CH2]C(C)C
triisobutylaluminum
C=C
ethylene
CO
methanol
C=C
ethylene
C=C.C=CCCCCCC
ethylene/1-octene

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeTo 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
    Sonstigewas elevated to 60° C
  4. 4
    Sonstigepolymerization
  5. 5
    Temperaturto maintain the total pressure at 3.0 Kg/cm2-G
  6. 6
    Sonstigeto terminate
  7. 7
    Sonstigethe polymerization
  8. 8
    Sonstigethe unreacted ethylene was purged out
  9. 9
    SonstigeThe resulting reaction solution
  10. 10
    Sonstigeto precipitate a polymer
  11. 11
    SonstigeThe polymer was separated by filtration
  12. 12
    Sonstigedried overnight under reduced pressure

Vorschrift

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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06713562B2uspto-grants-2004_03