Preparation method of olefin copolymer with carboxyl group
An olefin copolymer and olefin technology, which is applied in the field of polymer polymer preparation, can solve the problems of expensive equipment, high temperature and high pressure conditions, and high energy consumption, and achieve the effects of not easy scaling and convenient transportation.
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Embodiment 1
[0135] Complex Ni 1 preparation of
[0136]
[0137] Will contain 0.277g (0.9mmol) (DME) NiBr 2 The ethanol solution (10mL) was slowly added dropwise to the ligand L containing 0.233g (0.6mmol) 1 dichloromethane solution (10 mL). The color of the solution immediately turned dark red, and a large amount of precipitate formed. Stir at room temperature for 6 h, add anhydrous ether to precipitate. The filter cake was obtained by filtration, washed with anhydrous ether, and vacuum-dried to obtain a brownish-red powdery solid Ni 1 . Yield: 78.2%. Elemental analysis (C 60 h 58 Br6 N 4 Ni 3 o 2 ): C, 47.33; H, 3.84; N, 3.68; found (%): C, 47.38; H, 4.00; N, 3.46.
[0138] 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 7.6 mg (5 μmol) of the complex Ni1, 10 mL of dichlor...
Embodiment 2
[0140] 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 7.6 mg (5 μmol) of the complex Ni 1 , 50mL dichloromethane, 30mmol (5.10g) 2,2-dimethyl-7-octenoic acid, 30mL 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
[0142] 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 7.6 mg (5 μmol) of the complex Ni 1 , 100mL dichloromethane, 30mmol (5.10g) 2,2-dimethyl-7-octenoic acid, 30mL 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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