Preparation of metallocene catalyst
A metallocene catalyst and metallocene technology, applied in the direction of metallocene, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of reducing polymer crystallinity, reducing syndiotacticity, etc., to achieve excellent activity, avoid The effect of the fouling phenomenon
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[0085] Preparation of silica loaded with methylaluminoxane
[0086] Silica gel (Fuji Silysia, P-10) was dried in an oven at 150° C. for 18 hours, and then transferred into a glove box for storage. In a glove box, 15 g of dry silica was charged to a 1 L three-neck round bottom flask equipped with a condenser. The flask was sealed and removed from the glove box and loaded onto a Schlenk manifold under a slight positive pressure of nitrogen. To this was added 150 mL of dry deoxygenated toluene, the slurry was stirred briefly, and 41 mL of a 30% by weight solution of MAO in toluene was added. The reaction mixture was heated to 115° C. and refluxed for 4 hours under magnetic stirring. The slurry was cooled to room temperature and precipitated. Remove the upper layer of toluene with a cannula, wash the wet product three times sequentially with 150 mL of toluene, and then wash three times with 150 mL of dry deoxygenated hexane. Next, the MAO on silica was dried in vacuo to obtain...
Embodiment 1
[0087] The preparation of embodiment 1 miPP catalyst
[0088] 5 g of MAO on P-10 silica was added to a 100 mL round bottom flask containing 30 mL of toluene and the flask was allowed to cool to 15°C. In a 20mL Wheaton bottle, the rac-Me 2 Si(2-Me-4-PhInd) 2 ZrCl 2 (65 mg) was slurried with 10 mL of toluene. This metallocene slurry was applied to a stirred dispersion of MAO on silica. The transfer of the metallocene was accomplished with a second 10 mL portion of toluene. The metallocene was reacted with MAO / silica at 15°C for 1 hour. After the solids had settled, the supernatant was removed with a cannula. Wash the loaded wet catalyst with 50 mL of toluene, let the solid settle, and take out the upper liquid with a cannula. Then, the supported wet catalyst was washed with 3 portions of 50 mL of hexane at 0° C. for 3 times. After the third hexane decantation, the wet catalyst slurry was diluted with 45 g of mineral oil. The miPP supported catalyst was obtained as a slu...
Embodiment 2
[0089] The preparation of embodiment 2 miPP catalyst
[0090] 4 g of MAO on P-10 silica was added to a 100 mL round bottom flask containing 30 mL of toluene and the flask was cooled to 0°C. In a 20mL Wheaton bottle, the rac-Me 2 Si(2-Me-4, 5-BzInd) 2 ZrCl 2 (60 mg) was slurried with 10 mL of toluene. This metallocene slurry was applied to a stirred dispersion of MA0 on silica. The transfer of the metallocene was accomplished with a second 10 mL portion of toluene. The metallocene was reacted with MAO / silica at 0 °C for 1 hour. After the solids had settled, the supernatant was removed with a cannula. The supported wet catalyst was washed three times with 3 portions of 50 mL of hexane in sequence. After the third hexane decantation, the wet catalyst slurry was diluted with 45 g of mineral oil. A 7.0% solids slurry of the miPP supported catalyst was obtained.
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