Non-bridging zwitterionic half-metallocene complex and application thereof
A zwitterion, single metallocene technology, applied in the field of olefin polymerization catalysts, to achieve the effect of low catalytic cost
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Embodiment 1
[0022] Embodiment 1 Synthesis of non-bridging zwitterionic single metallocene complexes
[0023]
[0024] At room temperature and under a nitrogen atmosphere, 2.05 mmol of NaH powder was slowly mixed with 20 mL of a THF solution containing 2.00 mmol of protonated organoborate ligands (one of HL1-HL10), and the reaction mixture was stirred at room temperature for 10 hours, and then The reaction solution was cooled to -20°C and filtered to remove insoluble matter. The resulting filtrate was added at -20°C to a solution containing an equivalent amount of monometallocene complex Cp'MX 2 (2.00 mmol) in THF (20 mL), stirred overnight at room temperature. The solvent was distilled off under reduced pressure, and the crude product was washed with CHCl 3 / n-Hexane mixed solvent recrystallization to obtain a blue-green product. Experimental results: complex I1, yield 0.542g, yield 50%, elemental analysis C 70.88, H 5.69, N 5.24; complex I2, yield 0.504g, yield 44%, elemental analys...
Embodiment 2
[0025] Embodiment 2 catalytic ethylene polymerization reaction
[0026] The polymerization reaction was carried out in a 250 mL autoclave, using the non-bridged zwitterionic monometallocene complexes I1-I9 and II1-II11 prepared in Example 1 above as main catalysts, and aluminum alkyls as co-catalysts. Before the polymerization reaction, the reactor was baked at 120° C. for 1 hour under vacuum, and filled with ethylene gas at an atmospheric pressure. Under an ethylene atmosphere, first 70mL of toluene solution containing the procatalyst (Al / M in Table 1 represents the molar ratio of the aluminum in the procatalyst to the metal in the procatalyst) was added to the reactor, and then 10mL of the procatalyst ( 2umol) of toluene solution was added to the reactor, the ethylene pressure was raised to 5 atmospheres, and the timing was started. After the polymerization reaction was carried out for 30 minutes, the ethylene gas in the reactor was vented, and the polymerization reaction w...
Embodiment 3
[0030] Embodiment 3 catalytic ethylene / norbornene copolymerization reaction
[0031] The polymerization reaction was carried out in a 250mL autoclave, using the non-bridged zwitterionic monometallocene complexes I1~I9 and II1~II11 prepared in the above Example 1 as the main catalyst, and the alkylaluminum or haloalkylaluminum as the cocatalyst . Before the polymerization reaction, the reactor was baked at 120° C. for 1 hour under vacuum, and filled with ethylene gas at an atmospheric pressure. Under an ethylene atmosphere, first add 70 mL of toluene solution containing cocatalyst and norbornene (NBE) into the reactor, then add 10 mL of toluene solution containing main catalyst (2 μmol) into the reactor, and raise the ethylene pressure to 5 atmospheric pressure and start the timer. After the polymerization reaction was carried out for 30 minutes, the ethylene gas in the reactor was vented, and the polymerization reaction was terminated with HCI / methanol solution. The polymer...
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