Preparation method of copolymer of olefin and unsaturated carboxylic acid
An unsaturated, copolymer technology, applied in the field of polymer preparation, can solve the problems of expensive equipment, high temperature and high pressure conditions, and high energy consumption, and achieve the effect of improving the effect of balling
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Embodiment 1
[0111] 1) Ligand L 1 Preparation of:
[0112] The preparation of complex (R in structural formula III 1 , R 3 is ethyl, R 2 , R 4 -R 7 , R 10 for hydrogen, R 8 , R 9 and R 11 is methyl, R 12 is ethyl, M is nickel, Y is O, X is Br)
[0113] Under the protection of nitrogen, 2,6-diethylaniline (2.0ml, 12mmol) was dissolved in 20ml of toluene, and 12ml of trimethylaluminum (1.0M, 12mmol) was added dropwise at room temperature, and the reaction was refluxed for 2 hours, and the system was cooled to room temperature. Camphorquinone (0.831g, 5mmol) was added, and the system was refluxed for 6h. The reaction product was neutralized by aqueous sodium hydroxide solution, extracted and dried with dichloromethane, and the yellow ligand L was obtained by column chromatography. 1 , the yield was 69.2%. 1 H-NMR (CDCl 3 ):δ6.94-6.92(m,6H,C Ar -CH 3 ),2.56-2.51(m,4H,C Ar -CH 3 ),2.36-2.31(m,4H,C Ar -CH 3 ),1.82-1.78(m,4H,CH 2 ),1.54(m,1H),1.24-1.18(m,12H),1.09(s,3H,CH 3 ...
Embodiment 2
[0119] 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 Gas replacement 3 times. Inject 500 mL of hexane into the polymerization system, and simultaneously add 8.0 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
[0121] 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 Gas replacement 3 times. Inject 500 mL of hexane into the polymerization system, and simultaneously add 8.0 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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