Diimine metal complex and preparation method and application thereof
A technology of metal complexes and diimines, applied in nickel organic compounds, chemical instruments and methods, compounds containing elements of Group 8/9/10/18 of the periodic table, etc., can solve the problem that late transition metal catalysts cannot meet the requirements And other issues
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Embodiment 1
[0071]
[0072] Complex Ni 1 preparation of
[0073] Will contain 0.277g (0.9mmol) (DME) NiBr 2 The ethanol solution (10mL) was slowly added dropwise to the ligand L containing 0.175g (0.6mmol) 1 dichloromethane solution (10 mL), stirred at room temperature for 6 h, and added anhydrous ether to precipitate. Filtration left the filter cake, washed the filter cake with anhydrous ether, and obtained yellow powdery solid Ni after vacuum drying. 1 . Yield: 70.2%. Elemental analysis (C 44 h 58 Br 6 N 4 Ni 3 o 2 ): C, 39.72; H, 4.39; N, 4.21; Experimental values (%): C, 39.38; H, 4.60; N, 3.96.
[0074] The 1L stainless steel polymerization kettle equipped with mechanical stirring was continuously dried at 130°C for 6hrs, vacuumized while hot and heated with N 2 Air replacement 3 times. Inject 500ml of hexane, then add 5.0ml methylaluminoxane (MAO) (1.53mol / l toluene solution), add 3.3mg (2.5μmol) complex Ni 1 . At 60°C, the ethylene pressure was maintained at 10 ...
Embodiment 2
[0076] The 1L stainless steel polymerization kettle equipped with mechanical stirring was continuously dried at 130°C for 6hrs, vacuumized while hot and heated with N 2 Air replacement 3 times. Inject 500ml of hexane, then add 5.0ml methylaluminoxane (MAO) (1.53mol / l toluene solution), add 3.3mg (2.5μmol) complex Ni 1 . At 80°C, the ethylene pressure was maintained at 10 atm, and the reaction was vigorously stirred for 30 min. Neutralized with ethanol solution acidified with 10 wt% hydrochloric acid to obtain polyethylene, the results are shown in Table 1.
Embodiment 3
[0078] The 1L stainless steel polymerization kettle equipped with mechanical stirring was continuously dried at 130°C for 6hrs, vacuumized while hot and heated with N 2 Air replacement 3 times. Inject 500ml of hexane, 10ml of 1-hexene, then add 5.0ml of methylaluminoxane (MAO) (1.53mol / l toluene solution), add 3.3mg (2.5μmol) of the complex Ni 1 . At 80°C, the ethylene pressure was maintained at 10 atm, and the reaction was vigorously stirred for 30 min. Neutralized with ethanol solution acidified with 10 wt% hydrochloric acid to obtain polyethylene, the results are shown in Table 1.
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