A kind of preparation method of ethylene copolymer
A technology of ethylene copolymer and ethylene, which is applied in the field of preparation of ethylene copolymer, can solve the problems of low yield of nickel disalicylaldimine complex and low activity of ethylene polymerization, and achieve low cost, simple preparation method and good repeatability Effect
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[0015] The invention provides a preparation method of ethylene copolymer, which comprises the step of polymerizing ethylene and α-olefin in a solvent in the presence of an olefin polymerization catalyst, wherein the olefin polymerization catalyst contains the formula (I) The bimetallic catalyst precursor and alkylaluminoxane of the shown structure,
[0016] Formula (Ⅰ),
[0017] Among them, R 1 , R 2 , R 3 , R 4 , R 1 ’, R 2 ’, R 3 ’ and R 4 ' same or different, and each independently hydrogen, phenyl or C 1 -C 20 the alkyl group; R 5 and R 5 ’ same or different, and each independently hydrogen or C 1 -C 20 Alkyl group; M 1 and M 2 The same or different, and each independently being one of titanium, zirconium and hafnium.
[0018] According to the present invention, M in different bimetallic catalyst precursors 1 and M 2 may be the same or different, and each independently is one of titanium, zirconium and hafnium. Preferably, M 1 and M 2 Both are titani...
preparation example 1
[0048] This preparation example is used to illustrate the preparation of the bimetallic catalyst precursor having the structure represented by formula (II).
[0049] 6,6'-(1E,1'E)-(4,4'-methylenebis(4,1-phenylene)bis(imine-1-substituted-1-ylidene))bis(form Base-1-substituted-1-ylidene)bis(2-tert-butylphenol) (prepared according to the preparation method recorded in Eur.Polym.J.2012,48,191-199, the same below) (1.77g, 3.41mmol ) was dissolved in dichloromethane solvent (the amount of dichloromethane was 30mL), and the solution was added to the dichloromethane solution containing tetrachlorobis(tetrahydrofuran)titanium (2.28g, 6.82mmol) at -78°C ( The amount of dichloromethane used is 30 mL), reacted at low temperature for 1 hour, returned to room temperature 25°C, and continued to react for 16 hours. After the reaction was finished, the solvent was removed with a vacuum line, the residue was washed with dichloromethane and filtered through diatomaceous earth, the filtrate was ...
preparation example 2
[0052] This preparation example is used to illustrate the preparation of the bimetallic catalyst precursor having the structure represented by formula (II).
[0053] 6,6'-(1E,1'E)-(4,4'-methylenebis(4,1-phenylene)bis(imine-1-substituted-1-ylidene))bis(form Base-1-substituted-1-ylidene)bis(2-tert-butylphenol)(0.24g, 0.46mmol) was dissolved in dichloromethane solvent (the amount of dichloromethane used was 30mL), and the This solution was added to a dichloromethane solution containing tetrachlorobis(tetrahydrofuran)titanium (0.32g, 0.96mmol) (the amount of dichloromethane used was 30mL), reacted at low temperature for 1 hour, returned to room temperature and heated to 40°C , continue to react for 12 hours. After the reaction was finished, the solvent was removed with a vacuum line, the residue was washed with dichloromethane and filtered through diatomaceous earth, the filtrate was sucked dry, and the crude product was recrystallized with dichloromethane / n-hexane to obtain 0.41...
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