Reaktion #467241

ord-d0add749c4bf4936a34587fb91347e76

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeequipped with stirring blades
  2. 2
    SonstigeOn the other hand, the polymerization solution was continuously withdrawn from an upper site so that the polymerization solution in the polymerization vessel
  3. 3
    SonstigeThe co-polymerization reaction
  4. 4
    Sonstigewas effected at 89° C.
  5. 5
    SonstigeThe polymerization solution withdrawn from the polymerization vessel
  6. 6
    workup.ADDITIONwas treated with a small amount of ethanol
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    Sonstigeto quench
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    Sonstigethe polymerization reaction
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    Waschenwashed with water
  10. 10
    SonstigeThen the solvent was removed
  11. 11
    workup.ADDITIONby treating with steam in a large amount of water
  12. 12
    Sonstigeto separate a copolymer, which
  13. 13
    Sonstigewas dried at 80° C. for a day and night under reduced pressure

Vorschrift

Ethylene, propylene, 5-ethylidene-2-norbornene and dicyclopentadiene were continuously co-polymerized in a 100-liter polymerization vessel, made of stainless steel, equipped with stirring blades. Briefly, hexane was continuously fed as a solvent for polymerization to a lower site of the polymerization vessel at a rate of 83 liters/hour. On the other hand, the polymerization solution was continuously withdrawn from an upper site so that the polymerization solution in the polymerization vessel was 100 liters. Ethylene, propylene, 5-ethylidene-2-norbornene and dicyclopentadiene were continuously fed as monomers at the lower site of the polymerization vessel at rates of 3.00 kg/hour, 2.00 kg/hour, 0.60 kg/hour and 0.03 kg/hour, respectively, into the polymerization vessel. Dimethylsilyl (tetramethylcyclopentadienyl) (3-tert-butyl-5-methyl-2-phenoxy) titanium dichloride, triphenylmethyl tetrakis(pentafluorophenyl)borate and triisobutyl aluminum were continuously fed as catalysts at the lower site of the polymerization vessel at rates of 0.045 g/hour, 1.378 g/hour and 2.640 g/hour, respectively, into the polymerization vessel. The molecular weight was adjusted with hydrogen. The co-polymerization reaction was effected at 89° C. by feeding low-pressure steam into a jacket attached outside the polymerization vessel. The polymerization solution withdrawn from the polymerization vessel was treated with a small amount of ethanol to quench the polymerization reaction, stripped of the monomers and washed with water. Then the solvent was removed by treating with steam in a large amount of water to separate a copolymer, which was dried at 80° C. for a day and night under reduced pressure. By the above procedure, ethylene/propylene/5-ethylidene-2-norbornene/dicyclopentadiene copolymer was produced at a rate of 3.6 kg/hour. Detailed results are shown in Table 1.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06300447B1uspto-grants-2001_10