Polyolefin block copolymers
A technology of block copolymer and ethylene, applied in the field of block copolymer
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Embodiment A
[0039] Catalyst 1: Preparation of bis(2-chloro-5-phenyl-5,10-dihydroindeno[1,2-b]indolyl) zirconium dichloride
[0040] In a 100 mL round bottom flask, mix 50 mL ethanol, 4 mL H 2 SO 4 , 5.09 grams of 5-chloro-dihydro-1-indanone (0.0306 moles) and 6.74 grams of N, N-diphenylhydrazine hydrochloride (0.0306 moles), and heated to reflux for 4 hours. A brown solid isolated when the reaction mixture was cooled, and recrystallized from ethanol afforded 7.55 g of the indenoindole product (72% yield).
[0041] Slurry 2.37 g (0.0075 mol) of 2-chloro-5-phenyl-5,10-dihydroindeno[1,2-b]indole in 40 mL of hexane under a dry nitrogen atmosphere . To the slurry was added 5.6 mL of a 2.0 M solution of n-butyllithium in cyclohexane. The mixture was stirred at room temperature under nitrogen atmosphere for 67 hours. The resulting yellow solid was filtered, washed with hexane and dried under vacuum (1.8 g of product, 67% yield).
[0042] The above lithium salt (0.9 g, 0.0028 mol) was disso...
Embodiment B
[0044] In an inert atmosphere of a dry box, 5 mg of the catalyst 1 prepared in Example A was mixed with 1.9 ml of 10% by weight MAO toluene solution and 3 ml of toluene to prepare a catalyst and activator solution. The solution was allowed to stand for 30 minutes before being added to the polymerization reactor.
Embodiment C
[0046] In an inert atmosphere of a dry box, 5 mg of catalyst 1 prepared in Example A was mixed with 12 mg of tetrakis(pentafluorophenyl)trityl borate, 1.5 ml of triisobutylaluminum (25% by weight in heptane) and 3.5 ml of toluene were mixed to make a catalyst and activator solution. The solution was allowed to stand for 30 minutes before being added to the polymerization reactor.
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