Propylene → Vinylcyclohexane Propylene

関与物質

反応手順

To 100 ml of dehydrated pure n-heptane was added 1.95 g of triethyl aluminium, 675 mg of ethyl p-anisate and 6.0 g of titanium compound catalyst prepared according to Example 1 of Published Unexamined Japanese Patent Application No. 57-59916 in this order, and the temperature of the mixture was elevated to 50° C. Subsequently, 50 g of vinylcyclohexane was added to the mixture and polymerization of vinylcyclohexane wa continued for 15 minutes. The resulting polymer slurry was washed with 200 ml of n-heptane four times to remove unused vinylcyclohexane, triethylaluminium as a cocatalyst and ethyl p-anisate. Then, n-heptane was removed from the washed acitve slurry by distillation under reduced pressure to obtain 7.8 g of powder of polyvinylcyclohexane containing acitve catalyst. The amount of polyvinylcyclohexane polymerized is 0.30 g per g of the charged titanium compound catalyst In a stainless steel autocave (inner volume: 5l) was performed polymerization of propylene using 1.06 g of the above-described vinylcyclohexane polymerization catalyst, 0.75 g of triethyl aluminium, 0.237 g of methyl p-toluylate and 1,500 ml of n-heptane under the conditions of a pressure of 6 kg/cm2 guage and a temperature of 70° C. and a hydrogen concentration of 1.5% by volume for 40 minute. After completion of the polymerization, 50 ml of n-butanol was added to stop the polymerization and the resulting polymer slurry was taken out followed by the separation of polymer powder and solvent by filtration. After washing the polymer powder with 500 ml of 1N hydrochloric acid, further washing was performed with methanol until the washings became neutral.

情報源と証拠