Reaktion #1826716

ord-f8b1f8510e1640ab9840d2bebc13ca06

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONA two-liter Parr reactor is charged with approximately 360 g of Isopar-E™
  2. 2
    Sonstigeto give a 1
  3. 3
    workup.ADDITION) After the desired premix time
  4. 4
    workup.ADDITIONthe solution is transferred to a catalyst addition tank
  5. 5
    SonstigeThe polymerization conditions
  6. 6
    workup.ADDITIONAdditional quantities of premixed catalyst are added periodically
  7. 7
    SonstigeThe resulting solution is removed from the reactor
  8. 8
    Sonstigequenched with isopropyl alcohol
  9. 9
    workup.ADDITIONa hindered phenol antioxidant (Irganox™ 1010 from Ciba Geigy Corporation) is added to the resulting solution
  10. 10
    SonstigePolymers formed
  11. 11
    Sonstigeare dried in a vacuum oven
  12. 12
    SonstigeResults

Vorschrift

A two-liter Parr reactor is charged with approximately 360 g of Isopar-E™ mixed alkanes solvent (available from Exxon Chemicals Inc.) and about 460 g of styrene comonomer. Hydrogen is added as a molecular weight control agent by differential pressure expansion from a 75 mL addition tank at 25 psid (2070 kPa). The reactor is heated to 90° C. and saturated with ethylene at 200 psig (1.4 MPa). The appropriate amount of catalyst and cocatalyst (trispentafluorophenylborane) as 0.005 M solutions in toluene (approximately 2 μmole) are premixed in the drybox to give a 1:1 molar ratio of catalyst and cocatalyst. (Excepting for run 3 where the cocatalyst was methylalumoxane in a ratio Al:Ti of 1000:1.) After the desired premix time, the solution is transferred to a catalyst addition tank and injected into the reactor. The polymerization conditions are maintained for 30 minutes with ethylene on demand. Additional quantities of premixed catalyst are added periodically. The resulting solution is removed from the reactor, quenched with isopropyl alcohol and a hindered phenol antioxidant (Irganox™ 1010 from Ciba Geigy Corporation) is added to the resulting solution. Polymers formed are dried in a vacuum oven set at 135° C. for about 20 hours. Results using the catalysts of the invention are shown in Table 1.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05965756uspto-grants-1999_10