Method for preparing supported hybrid metallocene catalyst and supported hybrid metallocene catalyst prepared by using the method
A technology of metallocene catalysts and metallocene compounds, applied in catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as scaling and limitations
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preparation Embodiment 1
[0138] Preparation Example 1: Precursor A
[0139]
[0140] 1-1 Synthesis of Ligand Compounds
[0141]4.05 g (20 mmol) of ((1H-inden-3-yl)methyl)trimethylsilane were placed in a dry 250 mL Schlenk bottle and dissolved in 40 mL of diethyl ether under argon. After the solution was cooled to 0 °C, 1.2 equivalents (9.6 mL, 24 mmol) of 2.5M n-BuLi in hexane (hexane solution) were slowly added dropwise. The reaction mixture was slowly warmed to room temperature and stirred for 24 hours. In another 250ml Schlenk bottle, prepare a solution of 2.713g (10mmol) of silicone tether in 30ml of hexane, cool to -78°C, and slowly add the above-prepared mixture dropwise therein . After the dropwise addition, the mixture was slowly warmed to room temperature and stirred for 24 hours. 50 mL of water was added thereto, and the organic layer was extracted three times with 50 mL of diethyl ether. Add appropriate amount of MgSO to the extracted organic layer 4 and stir for a while. Then...
preparation Embodiment 2
[0152] Preparation Example 2: Precursor B
[0153]
[0154] As a metallocene compound precursor, dichloro[rac-ethylenebis(4,5,6,7-tetrahydro-1-indenyl)]zirconium(IV) was obtained (purchased from Sigma Aldrich ( Sigma-Aldrich), Cas No. 100163-29-9). 2.13 g (5 mmol) of the metallocene compound precursor was added to a 250 mL Schlenk bottle dried in an oven. Under an argon atmosphere, 1.02 g (10 mmol) of pivalic acid was added thereto, and dissolved in 50 mL of dichloromethane. The reaction mixture was cooled to 0°C, and then 1.4 mL (10 mmol) of triethylamine was slowly injected thereinto. The bath was removed and the reaction mixture was gradually warmed to room temperature. Within 30 minutes, the yellow color disappeared and it turned white. After about 1 hour, the reaction solvent was completely removed under reduced pressure, and 100 mL of diethyl ether was added to completely dissolve the white solid by sonication. The mixture in the flask was filtered under argon ...
preparation Embodiment 3
[0156] Preparation Example 3: Precursor C
[0157]
[0158] As a metallocene compound precursor, [rac-ethylenebis(indenyl)]zirconium(IV) dichloride (available from Sigma-Aldrich, CAS No. 100080-82-8) was obtained. 2.05 g (5 mmol) of the metallocene compound precursor was added to a 250 mL Schlenk bottle dried in an oven, and then 60 mL of anhydrous toluene was added thereto to prepare a suspension. Under an argon atmosphere, 2.11 g (15 mmol, 3 equivalents) of potassium pivalate was added thereto, and within about 2 hours, the floating matter disappeared and the solution turned into a clear yellow color. The reaction mixture was further stirred for about 3 hours and then passed through a pad of celite under argon atmosphere to remove residual potassium pivalate and inorganic material. The solvent was removed from the resulting filtrate under reduced pressure, and recrystallized with pentane to obtain a pale yellow compound with a yield of 50% to 60%.
[0159] 1 H NMR (5...
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