反応 #79447

ord-b94393dbe5344009b8ce3300b994e782

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他To 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
    その他was elevated to 60° C
  4. 4
    その他polymerization
  5. 5
    温度to maintain the total pressure at 3.0 Kg/cm2-G
  6. 6
    その他to terminate
  7. 7
    その他the polymerization
  8. 8
    その他the unreacted ethylene was purged out
  9. 9
    その他The resulting reaction solution
  10. 10
    その他to precipitate a polymer
  11. 11
    その他The polymer was separated by filtration
  12. 12
    その他dried overnight under reduced pressure

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06713562B2uspto-grants-2004_03