A kind of method for preparing olefin-olefin alcohol copolymer
A technology of olefinic alcohols and copolymers, which is applied in the field of high molecular polymer preparation, and can solve problems such as scaling, removal of polymer transport solvents, and difficulties in granulation, and achieve the effect of not easy to scale and convenient transportation
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Embodiment 1
[0125]
[0126] Preparation of complex Ni1
[0127] 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 Br 6 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.
[0128] 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, 15 mmol (2.5 mL)...
Embodiment 2
[0130] 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, 30 mmol (5.1 mL) of 2-methyl-2-hydroxyl-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.
[0131] figure 1 Photographs of spherical and / or spherical-like polymers prepared in this example are shown.
Embodiment 3
[0133] 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, 30 mmol (5.1 mL) of 2-methyl-2-hydroxyl-7-octene, 30 mL of AlEt 3(1.0mol / L hexane solution), 6.5mL MAO (1.53mol / L toluene solution), at 60°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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