Binuclear metallocene compound as well as preparation method and application thereof
A technology of metallocene compounds and metals, which is applied in the field of dinuclear metallocene compounds and their preparation, can solve the problems of low glass transition temperature of polymers, low insertion rate of cycloolefin monomers, limit the application range of polymers, etc., and achieve high catalytic performance Activity characteristics, easy availability of raw materials, and the effect of increasing insertion rate
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Embodiment A1
[0055] (1) Preparation of binuclear metallocene compound A-1:
[0056]Under nitrogen atmosphere, 5 mmol of cyclopentadienyl titanium trichloride (CpTiCl 3 ) was dissolved in 50mL of anhydrous toluene, cooled to -30°C and stirred; then 2.5mmol bisphenol A dilithium was added at one time; returned to room temperature and continued to stir for 24h; after the reaction was completed, the reaction solution was filtered anhydrous and oxygen-free, Collect the filtrate; the filtrate is vacuum-dried to precipitate a solid; the solid is dissolved in a small amount of anhydrous toluene, and the crystal is precipitated at -40~-20°C; then the crystal is separated and vacuum-dried to obtain the corresponding binuclear metallocene compound A-1, yield 78%, 1 H NMR (CDCl 3 , δ, ppm): 6.65-6.98 (M, 8H, C 6 h 4 ),6.72(S,10H,C 5 h 5 ),1.59(S,6H,C(CH 3 ) 2 );
[0057]
[0058] (2) Preparation of ethylene / norbornene copolymer: under anhydrous and oxygen-free conditions, add 0.4 mol of no...
Embodiment A2
[0060] (1) Preparation of binuclear metallocene compound A-2:
[0061] The difference from Example A1 is that in the synthetic raw material of the binuclear metallocene compound A-2, indenyl titanium trichloride is used instead of CpTiCl 3 , select tetramethyl bisphenol A dilithium to replace bisphenol A dilithium simultaneously, all the other are consistent with embodiment A1; Productive rate 75%, 1 H NMR (CDCl 3 , δ, ppm): 6.82-7.37 (M, 12H), 6.46 (d, 4H, Ind), 6.18 (t, 2H, Ind), 2.19 (S, 12H, C 6 h 2 (CH 3 ) 2 ),1.58(S,6H,C(CH 3 ) 2 );
[0062]
[0063] (2) Preparation of ethylene / norbornene copolymer: under anhydrous and oxygen-free conditions, add 0.4 mol of norbornene to a 500mL reactor, continue to add toluene until the total volume reaches 250mL, heat up to 80°C, and stir well Then add 4.8mmol of MAO and 1.2μmol of metallocene compound A-2 in turn, quickly fill with ethylene, make the pressure rise to 0.6MPa, and continue the reaction for 10min; After dryin...
Embodiment A3
[0065] (1) Preparation of binuclear metallocene compound A-3:
[0066] The difference from Example A1 is that in the synthetic raw material of the binuclear metallocene compound A-3, pentamethylcyclopentadienyl titanium trichloride is selected to replace CpTiCl 3 , while selecting 4,4'-dibenzylidene bisphenol dilithium to replace bisphenol A dilithium, and the rest are consistent with Example A1; the yield is 68%, 1 H NMR (CDCl 3 , δ, ppm): 7.09-7.26 (M, 10H, C 6 h 5 ),6.65-6.82(M,8H,C 6 h 4 ),1.95(S,30H,C 5 (CH 3 ) 5 );
[0067]
[0068] (2) Preparation of ethylene / norbornene copolymer: under anhydrous and oxygen-free conditions, add 0.4 mol of norbornene into a 500mL reactor, continue to add toluene until the total volume is 250mL, heat up to 90°C, and stir well ; Then add 1.2mmol of MAO and 1.2μmol of metallocene compound A-3 in turn, quickly fill with ethylene, raise the pressure to 3MPa, and continue the reaction for 10min; After that, the ethylene / norbornene...
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