Copolymer containing polar group and preparation method and application thereof
A technology of polar groups and copolymers, applied in the field of high molecular polymer preparation, to achieve the effect of improving the effect of ball formation and simple preparation process
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Embodiment 1
[0173] 1) Ligand L1 preparation:
[0174] ɑ-diimine compound A1 3.52g (8mmol), add 30ml toluene, 1M trimethylaluminum (16ml, 16mmol) successively, reflux reaction for 8 hours, stop the reaction with sodium hydroxide / ice water, extract with ethyl acetate, combine The organic phase was dried with anhydrous magnesium sulfate, and the product was separated by petroleum ether / ethyl acetate column chromatography to obtain a colorless crystal ligand L1 with a yield of 85.2%. 1 HNMRδ(ppm)7.23-6.88(m,14H),4.84(s,1H),4.73(s,1H),3.85(s,1H,NH),2.02(s,3H,CH 3 ),1.87(s,6H,CH 3 ),1.75(s,6H,CH 3 ).
[0175] 2) Preparation of complex Ni1: 10ml (DME) NiBr 2 (277mg, 0.9mmol) ethanol solution was added dropwise to 10ml of ligand L1 (274mg, 0.6mmol) in dichloromethane solution, stirred at room temperature for 6 hours, precipitated, filtered and washed with ether and dried to obtain a red powder solid, the yield was 74%. Elemental analysis (C 70 h 74 Br 6 N 4 Ni 3 o 2 ): C, 50.68; H, 4....
Embodiment 2
[0178] Dry the 1L stainless steel polymerization kettle equipped with mechanical stirring at 130 ° C for 6 hours, vacuumize while it is hot and use N 2Air replacement 3 times. Inject 500 mL of hexane into the polymerization system, and simultaneously add 8.3 mg (5 μmol) of the complex Ni1, 50 mL of dichloromethane, 30 mmol (5.1 mL) of 2-methyl-2-hydroxy-7-octene, 30 mL of AlEt 3 (1.0mol / L hexane solution), 6.5mL MAO (1.53mol / L toluene solution), at 30°C, keep 10atm ethylene pressure, and stir for 30min. Finally, it was neutralized with an ethanol solution acidified with 10 wt% hydrochloric acid to obtain a polymer. The polymerization activity and the performance parameters of the polymer are shown in Table 1.
Embodiment 3
[0180] Dry the 1L stainless steel polymerization kettle equipped with mechanical stirring at 130 ° C for 6 hours, vacuumize while it is hot and use N 2 Air replacement 3 times. Inject 500 mL of hexane into the polymerization system, and simultaneously add 8.3 mg (5 μmol) of the complex Ni1, 100 mL of dichloromethane, 30 mmol (5.1 mL) of 2-methyl-2-hydroxy-7-octene, 30 mL of AlEt 3 (1.0mol / L hexane solution), 6.5mL MAO (1.53mol / L toluene solution), at 30°C, keep 10atm ethylene pressure, and stir for 30min. Finally, it was neutralized with an ethanol solution acidified with 10 wt% hydrochloric acid to obtain a polymer. The polymerization activity and the performance parameters of the polymer are shown in Table 1.
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