Asymmetric bridged indenocene-based transition metal catalyst, preparation method and application
A technology of indenyl and transition metals, applied in the field of metallocene catalysts, can solve theoretical and technical problems
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
preparation example Construction
[0051] The preparation of the metallocene compound as formula 1:
[0052] Weigh 40mmol of 4-phenyl-2-methylindenyl, dissolve in 200ml Et 2 O, cooled to -78°C, and 40 mmol of 2.4M n-butyllithium in hexane solution was slowly added dropwise thereto, and the dropwise addition was completed over 15 minutes. Return to room temperature naturally under stirring, and stir at room temperature for another 12 h to obtain a solution of indenyllithium compound.
[0053] Weigh 20mmol of Me(PhMeNH 2 CH 2 CH 2 C) SiCl 2 , was dissolved in 100 mL of n-hexane, cooled to -78°C, and the solution of the indenyllithium compound prepared above was slowly added dropwise thereto, and the dropwise addition was completed within 30 minutes. Return to room temperature naturally under stirring, and stir at room temperature for another 12 h. The insolubles are removed by filtration, and the filtrate is passed through a silica gel column to obtain a yellow solution, and the solvent is drained to obtain...
Embodiment 1
[0060] 1. Preparation of catalyst
[0061] Weigh 2 g of silica gel that has been roasted at 600° C., add 10 mL of 10% MAO toluene solution (percentage by weight), and heat to 80° C. Add the toluene solution of the metallocene compound shown in Formula 1 under the condition of uniform stirring, control the Al / Zr ratio to 200:1, and react overnight. The solid was collected by filtration and washed with toluene until the washed solvent was colorless. The solid was dried in vacuum for 24 hours to obtain a solid powder, which was stored in a glove box for future use (this reaction method is used unless otherwise specified below). The catalyst SC-1 with a certain metal content can be obtained by measuring and calculating the amount of feed and the metal content of the washing effluent, wherein the zirconium content is 0.268% (29.4 μmol / g).
[0062]
[0063] 2. Catalytic reaction
[0064] A 300mL autoclave was selected, evacuated in an oil bath at 100°C, and replaced with nitrog...
Embodiment 2 4
[0070] 1. Preparation of catalyst
[0071] Weigh 2 g of silica gel that has been roasted at 600°C, add 10mL of 10% MAO toluene solution (weight percent) and pure toluene solvent, heat to 80°C, stir for 24 hours, filter, collect the solid, and wash it with toluene solvent 3 times, the solid After vacuum drying for 24 hours, MAO-silica gel was obtained as solid powder.
[0072] Weigh a certain amount of MAO-silica gel, add toluene solvent to form a suspension, add the toluene solution of the metallocene zirconium compound under the condition of uniform stirring, and react overnight. The solid was collected by filtration and washed with toluene until the washed solvent was colorless. The solid was dried in vacuum for 24 hours to obtain a solid powder, which was stored in a glove box for future use. A catalyst with a certain zirconium content can be obtained through the measurement and calculation of the feeding amount and the zirconium content of the washing liquid.
[0073] Se...
PUM
| Property | Measurement | Unit |
|---|---|---|
| melting point | aaaaa | aaaaa |
| melting point | aaaaa | aaaaa |
| melting point | aaaaa | aaaaa |
Abstract
Description
Claims
Application Information
Login to View More