Ethylene → Ethene;oct-1-ene

Temperature

140.10000610351562 °C

Under a nitrogen atmosphere, a 500 mL autoclave was charged with hexane (250 mL), triisobutylaluminum (0.2 mL of a 25.2 wt % solution in heptane diluted with toluene (5 mL)) and 1-octene (18 mL, 115 mmol). The autoclave was stirred at ca. 1500 rpm, heated to 140.1° C. (P=75.7 psig) then pressurized with ethylene to 265.6±1 psig. Ethylene flow into the reactor was allowed during the copolymerization. A solution of precatalyst (40-50 μmol), PhNMe2H+ B(C6F5)4− (1 equiv.) and toluene (100 mL) was added to the stirred mixture over 30 min. at a variable rate sufficient to obtain 12-15 g isolated copolymer with an exotherm of less than 1.5° C., typically less than 1° C. The polymer was precipitated with 2-propanol (1.5 L), isolated, then dried under vacuum at 80° C. See Table below.

1. customto obtain 12-15 g
2. customisolated copolymer with an exotherm of less than 1.5° C., typically less than 1° C
3. customThe polymer was precipitated with 2-propanol (1.5 L)
4. customisolated
5. customdried under vacuum at 80° C

ORD record

ord-70a249b291a34c13bfc5875827b46607

Source dataset

uspto-grants-2003_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06528670B1