Supported metallocene catalyst as well as preparation method and application thereof
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[0114] The preparation method of supported metallocene catalyst of the present invention comprises the steps:
[0115] Step 1, dissolving the carrier modifier in the first solvent, then adding the carrier, controlling the temperature of the mixed liquid at 50-100°C, and stirring at constant temperature for 1-40 hours; and
[0116] Step 2, dissolving the pyrrocene heterocyclic compound in the second solvent, and adding it dropwise to the mixed solution prepared in step 1 after dissolving, controlling the temperature at -50°C to 50°C, stirring at constant temperature for 2 to 20 hours, and post-processing to obtain Supported metallocene catalysts.
[0117] Wherein, the preparation method of pyrrolene heterocyclic compound comprises the following steps:
[0118] Step a, reacting formula II 2-pyrrole carboxaldehyde or its derivatives with indene to prepare formula III nitrogen-containing fulvene, R 1 , R 2 and R 3 independently selected from H, CH 3 - and saturated or double ...
Embodiment 1
[0140] 3-CH 3 - 2-pyrrole formaldehyde and indene are cooled to 0°C, tetrahydropyrrole is added dropwise, the ratio of the three substances is 1:1:5, and then raised to room temperature and stirred for 0.5 hours to obtain nitrogen-containing fulvene; 2°C, add lithium aluminum hydride dropwise, the molar ratio of nitrogen-containing fulvene to lithium aluminum hydride is 1:1; heat up to 65°C, stir for 30 hours to obtain a ligand containing pyrrole N heterocycle; cool down to 0°C, Zr(NMe 2 ) 4 , heated up to 80°C, and stirred for 10h to obtain the metallocene catalyst [(η 5 -C 9 h 6 )CH 2 (2-(3-CH 3 -C 4 h 2 N))]Zr(NMe 2 ) 2 .
[0141] The carrier modifier is methyl aluminoxane, and the inorganic carrier is silica. The preparation method is as follows: step 1, dissolve the carrier modifier methyl aluminoxane in toluene, add the carrier and control the temperature of the mixed solution to 80°C, Stir at constant temperature for 15 hours; step 2, dissolve the pyrrocene ...
Embodiment 2
[0144] 4-CH 3 - 2-pyrrole formaldehyde and indene are cooled to 5°C, tetrahydropyrrole is added dropwise, the ratio of the three substances is 1:2:4, and then raised to room temperature and stirred for 20 hours to obtain nitrogen-containing fulvene; -10°C, add lithium aluminum hydride dropwise, the molar ratio of nitrogen-containing fulvene to lithium aluminum hydride is 1:2, heat up to 50°C, stir for 50 hours to obtain a ligand containing pyrrole N heterocycle; cool down to 5°C , dropwise added Zr(NEt 2 ) 4 , heated up to 90°C, and stirred for 20h to obtain the metallocene catalyst [(η 5 -C 9 h 6 )CH 2 (2-(4-CH 3 -C 4 h 2 N))]Zr(NEt 2 ) 2 .
[0145] The carrier modifier is trimethylaluminum, and the inorganic carrier is silicon dioxide. The preparation method is as follows: step 1, dissolve the carrier modifier in toluene, add the carrier, control the temperature of the mixed solution at 60°C, and stir at a constant temperature for 10 hours; step 2. Dissolve the p...
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