Ethylene → Ethene propene 1-butene

Temperature

65 °C

To a 2000 ml polymerization apparatus dried under reduced pressure and thoroughly purged with nitrogen, 817 ml of dry hexane, 50 g of 1-butene and triisobutylaluminum (1.0 mmol) were charged at normal temperature, then the temperature inside the polymerization apparatus was elevated to 65° C., and the polymerization apparatus was pressurized with propylene to 0.70 MPa and subsequently pressurized with ethylene to 0.75 MPa. Thereafter, a toluene solution in which 0.002 mmol of di(m-trifluoromethylphenyl)methylene(3-tert-butyl-5-n-propylcyclopentadienyl)(fluorenyl)zirconium dichloride synthesized by Synthesis Method 9 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 16 minutes while maintaining the internal temperature at 65° C. and the total pressure at 0.75 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 120.7 g and the polymerization activity was 226.2 kg/mmol-cat-hr. The polymer had a composition of 58.5 mol % of propylene content, 32.5 mol % of ethylene content and 9.0 mol % of 1-butene content, and had an intrinsic viscosity [η] of 1.65 dl/g.

1. customTo a 2000 ml polymerization apparatus
2. customdried under reduced pressure
3. additionwere charged at normal temperature
4. customwas elevated to 65° C.
5. additionwas added to the polymerization vessel, and polymerization
6. customa polymer was precipitated out of the polymerization solution in 2 L of methanol
7. customwas dried in a vacuum at 130° C. for 12 hours

ORD record

ord-49ae1ab6c8a8432b9628a4fa4c402498

Source dataset

uspto-grants-2011_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07879960B2