1,2,4-Trichlorobenzene → Ethene propene 1-butene

Temperature

35 °C

In a 2000 ml polymerization apparatus thoroughly purged with nitrogen, 100 ml of dry hexane, 480 g of 1-butene and triisobutylaluminum (1.0 mmol) were placed at ordinary temperature. Then, the internal temperature of the polymerization apparatus was raised to 35° C., and the polymerization apparatus was pressurized to 0.54 MPa with propylene and then pressurized to 0.62 MPa with ethylene. Thereafter, a toluene solution in which 0.005 mmol of diphenylmethylene(cyclopentadienyl)fluorenyl zirconium dichloride and 1.5 mmol (in terms of aluminum) of methylaluminoxane (available from Tosoh Finechem Corporation) had been contacted was introduced into the polymerizer. With maintaining the internal temperature at 35° C. and the ethylene pressure at 0.62 MPa, polymerization was carried out for 5 minutes, and 20 ml of methanol was added to terminate polymerization. After the pressure was released, a polymer was precipitated from the polymer solution in 2 liters of methanol, and the polymer was dried under vacuum at 130° C. for 12 hours. The amount of the polymer obtained was 36.1 g. The polymer had composition of a propylene content of 61.3% by mol, an ethylene content of 10.3% by mol and a 1-butene content of 28.4% by mol, and the polymer had an intrinsic viscosity [η] of 2.67 dl/g and a glass transition temperature Tg of −27.7° C. Further, any melting peak was not present, and the molecular weight distribution as determined by GPC was 2.0. As for the absorptions of methyl groups of propylene units in 13C-NMR of the polymer measured in a 1,2,4-trichlorobenzene solution, the sum total of absorption intensities observed at about 20.0 to 21.0 ppm on the basis of tetramethylsilane was 0.8 of the absorption intensities at about 19.0 to 22.0 ppm assigned to propylene methyl.

1. customIn a 2000 ml polymerization apparatus
2. temperatureWith maintaining the internal temperature at 35° C.
3. customto terminate
4. custompolymerization
5. customa polymer was precipitated from the polymer solution in 2 liters of methanol
6. customthe polymer was dried under vacuum at 130° C. for 12 hours
7. customThe amount of the polymer obtained
8. customthe sum total of absorption intensities
9. custom0.8 of the absorption intensities at about 19.0 to 22.0 ppm

ORD record

ord-ec6f2e75248041d8832340e2c40e4c7d

Source dataset

uspto-grants-2011_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08008401B2