Preparation method of olefin-unsaturated carboxylic acid copolymer
A carboxylic acid copolymer, unsaturated technology, applied in the field of high molecular polymer preparation, can solve the problems of polymer transportation solvent removal, difficult granulation, scaling, etc.
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Embodiment 1
[0132] 1) Preparation of Ligand L1:
[0133] 1.5ml 2,6-dimethylaniline (12mmol) was reacted with 57ml 1M trimethylaluminum in toluene, after reflux for 3h, camphorquinone (1.05g, 5mmol) was added, and the reaction was reflux for 8 hours. The reaction was terminated with sodium / ice water, extracted with ethyl acetate, the organic phases were combined, and dried over anhydrous magnesium sulfate. The product was separated by petroleum ether / ethyl acetate column chromatography to obtain a colorless crystal ligand L1 with a yield of 70.2%. 1 HNMRδ(ppm)7.00-6.89(m,6H,Ar-H),3.57(s,1H,NH),2.18(s,6H,CAr-CH 3 ),2.05(s,6H,CH 3 ),1.74(m,4H,CH 2 ),1.44(s,3H,CH 3 ),1.35(m,1H),1.21(s,3H,CH 3 ),1.01(s,3H,CH 3 ),0.87(s,3H,CH 3 ).
[0134] 2) Preparation of complex Ni1:
[0135] 10ml (DME)NiBr 2 (277mg, 0.9mmol) ethanol solution was added dropwise to 10ml of ligand L1 (223mg, 0.6mmol) in dichloromethane solution, stirred at room temperature for 6 hours, a precipitate precipitated, filt...
Embodiment 2
[0139] 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 (5.10 g) of 2,2-dimethyl-7-octenoic acid, and 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
[0141] 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 (5.10 g) of 2,2-dimethyl-7-octenoic acid, and 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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