High-activity coordination compound for catalyzing polymerization of 4-methyl-1-pentene and preparation method of high-activity coordination compound
A complex, trimethylaluminum technology, applied in the direction of palladium organic compounds, platinum group organic compounds, chemical instruments and methods, etc., can solve the problem of deactivation of active centers, inability to copolymerize olefins, and promote high activity catalyst methyl aluminoxane Expensive dosage and other issues, to achieve the effect of enhancing power supply and improving catalytic activity
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Embodiment 1
[0032] This embodiment provides a diimine ligand, and its synthesis method is as follows.
[0033] Under nitrogen atmosphere and room temperature, add 20mL of toluene and 2,6-dipropyl-4-methoxyaniline (12mmol) to a 100mL branch bottle successively, then slowly add 12mL of trimethylaluminum (1.0M, 12mmol ); the reaction temperature was raised to 110° C., and after 2 hours of reaction, the reaction temperature was down to room temperature, and then acenaphthylquinone (5 mmol) was added; at this moment, the reaction system was changed from colorless to deep red, and a large amount of heat was released; at 110° C. The reaction was continued for 6 hours at low temperature, and then cooled to 0 ° C. The reaction system was terminated with 5% sodium hydroxide ice solution; the organic phase was extracted with ethyl acetate, and then anhydrous MgSO 4 Dry and spin the solvent under reduced pressure to obtain an orange oil; the product is separated through a silica gel column, and the e...
Embodiment 2
[0035] This example provides a diimine palladium complex, the synthesis method of which is as follows.
[0036] Under the protection of nitrogen, add diimine ligand (0.5mmol), (COD)PdMeCl (0.6mmol) and dichloromethane 20mL respectively in the Schlenk bottle with a branch, stir the reaction at room temperature for 12 hours, and then The solvent was evaporated under reduced pressure to about 5ml, and 20ml of n-hexane was added, at which time a large amount of precipitation occurred. Filter with G4 filter ball, wash the precipitate with 3×10 mL of n-hexane, and then vacuum-dry to obtain a yellow solid powder diimide palladium complex with a yield of 73.4%.
Embodiment 3
[0038] This embodiment provides a poly(4-methyl-1-pentene), the preparation method of which is as follows.
[0039] All the glass instruments and magnets used for stirring were dried in an oven (120°C), and all polymerization experiments were carried out under anhydrous and oxygen-free conditions. Under continuous vacuuming, bake a 250mL branched-mouthed round-bottom flask under an infrared lamp at 150°C for more than 1 hour to remove all moisture and air; replace it with nitrogen twice and then fill it with nitrogen to normal pressure; keep the water bath at 30 ℃, add metered amount of chlorobenzene, stir to dissolve and inject 2M monomer and 10 μmol diimine palladium complex dissolved in 2 mL of dichloromethane. Stop the reaction after polymerizing to 2h, use Et 3 After SiH terminated, it was precipitated in methanol. The precipitated polymer was dissolved in petroleum ether, separated by silica gel column, concentrated, and precipitated in methanol. The obtained polymer wa...
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