3-sulfur five-atom bridged dinuclear metallocene complexes and uses thereof
A metallocene complex and atomic bridge technology, applied in the field of dinuclear metallocene complexes, can solve the problems of poor processing performance and unfavorable industrialized production.
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Embodiment 1
[0028] Embodiment 1 [(CpTiCl 2 ) 2 (η5-η5-C 5 h 4 (CH 2 ) 2 S(CH 2 ) 2 C 5 h 4 )] (1) synthesis
[0029]
[0030]
[0031] At 0°C, the C 5 h 5 Na (30.8ml, 0.54mol / L) was slowly dropped into Cl(CH 2 ) 2 S(CH 2 ) 2 Cl (1.32g, 8.31mmol) in THF (50.0ml). After naturally rising to room temperature (25° C.), a white precipitate slowly appeared, and the mixture was stirred for 5 hr. Add saturated NH 4 Cl aqueous solution, ether extraction separation, organic phase solution with anhydrous MgSO 4 dry. The solvent was drained to obtain light yellow transparent liquid L1. At -76°C, under the protection of Ar gas, the diethyl ether solution of L1 was added dropwise to the petroleum ether solution of n-BuLi (0.72mol / L, 23.1ml), white solid particles were precipitated, and the dropwise addition was completed in about 1 hr. After reacting overnight, the supernatant was removed by centrifugation, washed with petroleum ether (20ml×2), and dried to obtain 0.96g of lig...
Embodiment 2
[0033] Embodiment 2 [(CpZrCl 2 ) 2 (η5-η5-C 5 h 4 (CH 2 ) 2 S(CH 2 ) 2 C 5 h 4 )] (2) synthesis
[0034]
[0035]
[0036] At 0°C, the C 5 h 5 Na (30.8ml, 0.54mol / L) was slowly dropped into Cl(CH 2 ) 2 S(CH 2 )2 Cl (1.32g, 8.31mmol) in THF (50.0ml). After naturally rising to room temperature (25° C.), a white precipitate slowly appeared, and the mixture was stirred for 5 hr. Add saturated NH4Cl aqueous solution, extract and separate with ether, and dry the organic phase solution with anhydrous MgSO4. The solvent was drained to obtain light yellow transparent liquid L1. At -76°C, under the protection of Ar gas, the diethyl ether solution of L1 was added dropwise to the petroleum ether solution of n-BuLi (0.72mol / L, 23.1ml), white solid particles were precipitated, and the dropwise addition was completed in about 1 hr. After reacting overnight, the supernatant was removed by centrifugation, washed with petroleum ether (20ml×2), and dried to obtain light ye...
Embodiment 3
[0038] Embodiment 3 catalytic ethylene polymerization reaction
[0039] In a 50mL polymerization reaction bottle, add toluene (amount of 23mL) and 1mL of toluene solution of 10% methylaluminoxane (MAO) in sequence, feed ethylene gas, the total volume of the added liquid is 25ml, and feed the pressure of ethylene Is 1 atmosphere of pressure (ie 1bar). Add 31 mL of toluene solution ([cat]=0.4 μmol / mL) of the 3-sulfur pentaatom-bridged dinuclear metallocene compound obtained in Example 1 to initiate ethylene polymerization, and polymerize at 0° C. for 20 min. After the reaction reaches the set time, a mixed solution of 150ml ethanol and 10ml hydrochloric acid is added to terminate the reaction, and white polyethylene precipitates are formed immediately. After filtration, the polyethylene was repeatedly washed with ethanol and distilled water to remove the participating catalysts and acids, and dried in a vacuum oven at 60°C to constant weight.
[0040] Obtain polyethylene 0.30g...
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