Reaktion #1448756

ord-a1ae9d76ada7409ca8f72a29602a4850

Lösungsmittel

Reaktionsbedingungen

Temperatur
40°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeTo a 4000 ml polymerization apparatus
  2. 2
    Sonstigedried under reduced pressure
  3. 3
    workup.ADDITIONwere charged at normal temperature
  4. 4
    Sonstigewas elevated to 40° C.
  5. 5
    workup.ADDITIONwas added to the polymerization vessel, and polymerization
  6. 6
    Sonstigea polymer was precipitated out of the polymerization solution in 2 L of methanol
  7. 7
    Sonstigewas dried in a vacuum at 130° C. for 12 hours

Vorschrift

To a 4000 ml polymerization apparatus dried under reduced pressure and thoroughly purged with nitrogen, 1670 ml of dry hexane, 73.3 g of 1-butene and triisobutylaluminum (1.0 mmol) were charged at normal temperature, then the temperature inside the polymerization apparatus was elevated to 40° C., and the polymerization apparatus was pressurized with propylene to 0.30 MPa and subsequently pressurized with ethylene to 0.40 MPa. Thereafter, a toluene solution in which 0.002 mmol of rac-dimethylsilylenebis(2-methyl-4-phenyl-indenyl)zirconium dichloride and methylaluminoxane (manufactured by Tosoh Finechem Corp.) in terms of 0.6 mmol of aluminum were contacted, was added to the polymerization vessel, and polymerization was conducted for 20 minutes while maintaining the internal temperature at 40° C. and the total pressure at 0.80 MPa by continuously supplying ethylene. The polymerization was stopped by adding 20 ml of methanol. After depressurizing, a polymer was precipitated out of the polymerization solution in 2 L of methanol, and was dried in a vacuum at 130° C. for 12 hours. The obtained polymer was 158.0 g and the polymerization activity was 237.0 kg/mmol-cat hr. The polymer had a composition of 57.3 mol % of propylene content, 20.8 mol % of ethylene content and 21.9 mol % of 1-butene content, and had an intrinsic viscosity [η] of 2.08 dl/g.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07879960B2uspto-grants-2011_02