Pyridine imine vanadium complex as well as preparation method and application thereof in conjugated olefin polymerization
A technology of pyridinium vanadium and conjugated olefin, which is applied in the field of polyconjugated diene preparation, can solve the problem of low polymer structure selectivity, and achieve the effects of controllable molecular weight, avoiding complexity, and high conversion rate
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specific Embodiment approach 1
[0026] Specific embodiment one: the structure of a kind of pyridineimine vanadium complex of the present embodiment is one of the following structures:
[0027]
[0028] The method for preparing the above-mentioned pyridineimine vanadium complex is carried out according to the following steps:
[0029] Under anhydrous, oxygen-free, room temperature conditions, the VCl 3 (THF) 3 and ligand were dissolved in dichloromethane, and then the dichloromethane solution of the ligand was added dropwise to VCl 3 (THF) 3 In the dichloromethane solution of , after the reaction, concentrated in vacuo, filtered, washed and dried to obtain the pyridineimide vanadium complex.
[0030] Further limited, the ligand is one of the following structures:
[0031]
[0032] Further limited, the concentration of the dichloromethane solution of the ligand is 0.01mol / L~10mol / L, the VCl 3 (THF) 3 The concentration of the dichloromethane solution is 0.01mol / L~10mol / L.
specific Embodiment approach 2
[0033] Specific embodiment two: the application of a kind of pyridine imine vanadium complex of the present embodiment in conjugated olefin polymerization, the concrete process is as follows:
[0034] Under anhydrous and oxygen-free conditions, the pyridineimine vanadium complexes represented by formulas I to IV are dissolved in an organic solvent, then cocatalysts and conjugated olefin monomers are added in sequence, and the polymerization reaction is carried out at 0 to 100 ° C for 1 min to 5 h. , to obtain polyconjugated olefins.
[0035] Further limited, the cocatalyst is trimethylaluminum, triethylaluminum, triisobutylaluminum, methylaluminoxane, drained methylaluminoxane, diethylaluminum monochloride, dichloromonoethylaluminum A kind of base aluminum, dimethyl aluminum monochloride, monomethyl aluminum dichloride, sesquimethyl aluminum chloride, sesquiethyl aluminum chloride, and the conjugated olefin monomer is butadiene Or isoprene, and the organic solvent is one of t...
Embodiment 1
[0040] Embodiment 1: the preparation method of the pyridine imine vanadium complex shown in formula I is carried out according to the following steps:
[0041] Under nitrogen atmosphere and room temperature, put VCl in a dry Shrek tube.3 (THF) 3 (200 mg, 0.5 mmol) was dissolved in 10 mL of redistilled dichloromethane, pyridylbenzylimine ligand A (102 mg, 0.5 mmol) was dissolved in 5 mL of dichloromethane, and the dichloromethane solution of the ligand was added dropwise at room temperature to VCl 3 (THF) 3 In the dichloromethane solution of 0.1%, stirred overnight, concentrated the reaction solution to 3mL, added 5mL of n-hexane to separate out a large amount of solid, filtered, and vacuum-dried the filter residue to constant weight to obtain 0.17g of yellow solid, which was the pyridineimide vanadium shown in formula I Complex, yield 77%.
[0042] Elemental analysis: Theoretical value: C 13 H 12 Cl 3 N 2 V 1 / 2 (CH 2 Cl 2 ): C, 40.94; H, 3.31; N, 7.07; found: C, 40.59...
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