Vinylidene acenaphthylene α-diimine nickel olefin catalyst and its preparation method and application
A technology of nickel catalyst and diimine, which is applied in the field of vinylidene acenaphthylene asymmetric α-diimine nickel catalyst and its preparation, which can solve the problems of low ligand yield, large steric hindrance, and low polymerization activity of the catalyst , to achieve good polymerization activity, good thermal stability and the effect of
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Embodiment 1
[0042] Embodiment 1, preparation A1:
[0043] 1) Preparation of B2:
[0044] B1 (5g, 24mmol) was dissolved in 250mL carbon tetrachloride, under N 2 Under atmosphere, reflux at 85°C for 30min, add 13g (75mmol) N-bromosuccinimide (NBS) and 1g benzoyl peroxide to the solution, and continue to reflux at 85°C for 5h. After the reaction is over, filter while hot, and use 200mL hot CCl 4 After washing, the mixture obtained by washing was subjected to rotary evaporation, and the solvent carbon tetrachloride was removed to obtain a yellow solid, which was a mixture of product B2 and NBS. Purified by column chromatography with dichloromethane as the eluent, the total mass of product B2 was 5.53 g, and the yield was 63%.
[0045] 2) Preparation of B3:
[0046] B2 (5.5g, 15mmol) in N 2 Dissolve in 100mL acetone under atmosphere, then add 22.5g (1.38mol) anhydrous potassium iodide to the solution, and reflux at 60°C for 4h. After the reaction, the mixture was cooled and poured into a...
Embodiment 2
[0049] Example 2, Preparation A2: In 2,4-bis(benzhydryl)-6-methylaniline (8.8g, 20mmol) and vinylidene acenaphthylquinone (3.7g, 18mmol) in toluene (150mL) solution Add p-toluenesulfonic acid (0.34g, 2mmol) and reflux for 6h. The solvent was removed, and the residue was subjected to silica gel column chromatography with a mixed solvent of dichloromethane and petroleum ether at a volume ratio of 2:1 to obtain A2 with a mass of 4.4 g and a yield of 39%.
Embodiment 3
[0050] Example 3, Preparation A3: In 2,4-bis(bis(4-fluorophenyl)methyl)-6-methylaniline (10.2g, 20mmol) and vinylidene acenaphthylquinone (3.7g, 18mmol) P-toluenesulfonic acid (0.34 g, 2 mmol) was added to the toluene (150 mL) solution, and the reaction was refluxed for 10 h. The solvent was removed, and the residue was subjected to silica gel column chromatography with a mixed solvent of dichloromethane and petroleum ether at a volume ratio of 2:1 to obtain A3 with a mass of 4.9 g and a yield of 39%.
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