Toluene → Ethylene/Propylene 1,3-Butadiene

Participants

Reaction Conditions

Reaction Steps

Next, 5 g of the obtained polyolefin copolymer and 750 mL of dried toluene were charged into a 2000-mL SUS autoclave thoroughly purged with a nitrogen gas, and then, after the inner temperature of the autoclave was raised to 80° C., the mixture was agitated for 2 hours to dissolve the polyolefin copolymer. Thereafter, the inside of the polymerization vessel was pressurized to 0.8 MPa with ethylene. Then, a toluene solution containing 0.75 mmol of tungsten hexachloride, 7.5 mmol of propyl acetate, and 1.5 mmol of tetramethyl tin was charged into the autoclave, and the reaction was carried out for 60 minutes while maintaining the ethylene pressure at 0.8 MPa and the inner temperature at 80° C. Thereafter, 20 mL of methanol was added to terminate the reaction. After depressurized, the obtained reaction solution was passed through a column packed with 100 g of silica gel, and then the polymer was recovered from the reaction solution by precipitation in 4 L of methanol, and dried at 130° C. for 12 hours under vacuum. The yield of the obtained polyolefin polymer containing vinyl groups at both ends thereof was 3.9 g. In the composition of the polymer, the content of ethylene was 79.8% by mole, the content of propylene was 16.6% by mole, and the content of 1,3-butadiene was 3.6% by mole. The content of 1,3-butadiene contained 0.6% by mole of 1,4-addition structure, 0.5% by mole of 1,2-addition structure, 2.3% by mole of 5-membered ring structure, and 0.2% by mole of 3-membered ring structure. The terminal vinylation ratio of the polymer was 77%, and the intrinsic viscosity [η] was 0.12 dL/g.

Provenance & Evidence