Synthetic method of metallocene catalyst aid and application of metallocene catalyst aid in 1-decene polymerization process
A metallocene catalyst and technology for synthesis methods, which are applied in chemical instruments and methods, compounds containing elements of Group 3/13 of the periodic table, organic chemistry, etc. The effect of high yield and simple reaction process
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Embodiment 1
[0032] In a 2L reaction kettle, add 170g of tetrapentafluorophenyl borate and 1120g of dichloromethane, and stir for 30min at room temperature (25°C). 69 g of trityl chloride was added, and the reaction was stirred for 2 hours at a temperature of 25-30° C. in the kettle. Stop the reaction, add 17g of diatomaceous earth, and stir for 10min. After vacuum filtration to remove insoluble solids, the organic phase filtrate was distilled off under reduced pressure to remove most of the solvent dichloromethane. Add 380g of n-heptane, and continue vacuum distillation to remove low-boiling dichloromethane. Vacuum filtration afforded a crude solid. The crude product was vacuum-dried at 50° C. for 10 hours to obtain 200 g of triphenylcarba(pentafluorophenyl) borate as a white powder solid (99% purity, 91.6% molar yield).
Embodiment 2
[0034] In a 2L reaction kettle, add 170g of tetrapentafluorophenyl borate and 1120g of dichloromethane, and stir for 30min at room temperature (25°C). 76.5 g of trityl chloride was added, and the reaction was stirred for 2 hours under the condition that the temperature in the kettle was 25-30°C. Stop the reaction, add 17g of diatomaceous earth, and stir for 10min. After vacuum filtration to remove insoluble solids, the organic phase filtrate was distilled off under reduced pressure to remove most of the solvent dichloromethane. Add 380g of n-heptane, and continue vacuum distillation to remove low-boiling dichloromethane. Vacuum filtration afforded a crude solid. The crude product was vacuum-dried at 50° C. for 10 hours to obtain 208 g of triphenylcarba(pentafluorophenyl) borate as a white powder solid (purity 99%, molar yield 95.3%).
Embodiment 3
[0036] In a 2L reaction kettle, add 170g of tetrapentafluorophenyl borate and 1120g of dichloromethane, and stir for 30min at room temperature (25°C). 51.8 g of N,N-dimethylaniline hydrochloride was added, and the reaction was stirred for 2 hours under the condition that the temperature in the kettle was 25-30°C. Stop the reaction, add 17g of diatomaceous earth, and stir for 10min. After vacuum filtration to remove insoluble solids, the organic phase filtrate was distilled off under reduced pressure to remove most of the solvent dichloromethane. Add 380g of n-heptane, and continue vacuum distillation to remove low-boiling dichloromethane. Vacuum filtration afforded a crude solid. The crude product was vacuum-dried at 50° C. for 10 hours to obtain 178 g of white powder solid N,N-dimethylanilinium tetrakis(pentafluorophenyl) borate (purity 99%, molar yield 93.8%).
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