Novel ethidene bridged linkage substituted indene fluorene zirconium compound, method for preparing same and application thereof

A zirconium compound, bisindenyl fluorene technology, applied in the field of preparation and its application in olefin homopolymerization, can solve the problem that the dimerization selectivity of metallocene complexes is not very good, and bridged metallocene complexes have not yet been seen and other problems, to achieve the effect of wide application prospects, stable properties and high catalytic activity

Inactive Publication Date: 2010-07-21
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the dimerization selectivity of metallocene complexes is not very good, and there is no report on the use of bridged metallocene complexes for propylene dimerization.

Method used

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  • Novel ethidene bridged linkage substituted indene fluorene zirconium compound, method for preparing same and application thereof
  • Novel ethidene bridged linkage substituted indene fluorene zirconium compound, method for preparing same and application thereof
  • Novel ethidene bridged linkage substituted indene fluorene zirconium compound, method for preparing same and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Synthesis of Ligand Compound L1

[0036]

[0037] Add 3.46g of 3-(1-methyl-1-phenyl-ethyl)indene into the reaction flask, add 30mL of petroleum ether, add dropwise 7.0mL (2.15mol / L) of n-butyl lithium solution, dropwise, After stirring for 2 hours, an off-white powdery solid was obtained, which was dissolved by adding 30 mL of diethyl ether. Add dropwise a mixed solution of 3.46g 9-(2-bromo-ethyl)-fluorene and 20mL diethyl ether, stir for 4h, then add 40mL saturated ammonium chloride aqueous solution to stop the reaction, then extract with 100mL diethyl ether, the obtained yellow liquid is washed with anhydrous magnesium sulfate dry. After filtration and recrystallization, 14.40 g of yellow solid L was obtained, with a yield of 81.6%.

[0038] 1 H NMR (400MHz, 298K, CDCl 3 ): δ7.72(d, J=7.6Hz, 2H, Flu-H), 7.48(d, J=7.6Hz, 1H, Ar-H), 7.41(d, J=7.6Hz, 1H, Ar-H ), 7.33(t, J=7.6Hz, 2H, Ar-H), 7.30-7.26(m, 4H, Ar-H), 7.23-7.18(m, 3H, Ar-H), 7.13(d, J= 6.8Hz, 1H, Ar-...

Embodiment 2

[0040] Synthetic Ligand Compound L2

[0041]

[0042] Add 3.25g of 3-[1-methyl-1-(2-methyl-phenyl)-ethyl]indene into the reaction flask, add 30mL of petroleum ether, and dropwise add 7.0mL (2.15mol / L) of n-butyl Lithium solution, dropwise, stirred for 2h, and the powdery solid was dissolved with 30mL ether. Add dropwise a mixed solution of 3.00g 9-(2-bromo-ethyl)-fluorene and 20mL diethyl ether, stir for 4h, then add 40mL saturated ammonium chloride aqueous solution to stop the reaction, then extract with 100mL diethyl ether, and the obtained yellow liquid is washed with anhydrous magnesium sulfate dry. After filtration and recrystallization, 23.04 g of a yellow solid was obtained, with a yield of 62.8%.

[0043] 1 H NMR (400MHz, 298K, CDCl 3 ): δ7.77 (dd, J=7.6, 3.6Hz, 2H, Flu-H), 7.60 (d, J=7.6Hz, 1H, Ar-H), 7.54 (d, J=7.2Hz, 1H, Ar -H), 7.45(d, J=7.2Hz, 1H, Ar-H), 7.41-7.32(m, 5H, Ar-H), 7.21(d, J=7.2Hz, 1H, Ar-H), 7.15 (t, J=7.2Hz, 1H, Ar-H), 7.04(t, J=7.4Hz, 1H, ...

Embodiment 3

[0045] Synthetic Ligand Compound L3

[0046]

[0047] Add 1.70g of 3-[1-methyl-1-(2-methoxy-phenyl)-ethyl]indene to the reaction flask, add 30mL petroleum ether, drop 3.5mL (2.15mol / L) n-butyl Lithium solution, dropwise, stirred for 2h, filtered, and the powdery solid was dissolved in 30mL ether. Add dropwise a mixed solution of 1.75g ​​9-(2-bromo-ethyl)-fluorene and 20mL diethyl ether, stir for 4h, then add 40mL saturated ammonium chloride aqueous solution to stop the reaction, then extract with 100mL diethyl ether, and the obtained yellow liquid is washed with anhydrous magnesium sulfate dry. After filtration and recrystallization, 1.24 g of yellow solid L was obtained, with a yield of 42.1%.

[0048] 1 H NMR (400MHz, 298K, CDCl 3 ): δ7.78 (d, J=7.2Hz, 2H, Flu-H), 7.54 (d, J=7.6Hz, 1H, Ar-H), 7.49 (d, J=7.4Hz, 1H, Ar-H ), 7.43-7.37(m, 3H, Ar-H), 7.33(dt, J=7.4, 1.2Hz, 2H, Ar-H), 7.24-7.20(m, 2H, Ar-H), 7.03(dt, J=7.4, 0.9Hz, 1H, Ar-H), 6.98-6.93(m, 2H, Ar-H), 6.76(d...

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Abstract

The invention discloses a novel C1-symetrical ethidene bridged linkage indene fluorene zirconium compound, a method for preparing the same and application thereof in alpha-olefinic polymerization and oligomerization. The C1-symetrical zirconium compound has the characteristics that: at least one of indene 3-position substituents R1, R2 and R3 is an aryl group; the compound is a high-efficiency catalyst, can be used for catalyzing ethane polymerization and has moderate catalytic activity, and the obtained polyethylene has higher molecular weight and broader molecular weight distribution; when the compound is used for catalyzing the ethane polymerization, the propylene dimerization products can be exclusively obtained, and 2-methyl-2-amylene is obtained in high selectivity. The structure of the compound can be represented by a general expression below.

Description

technical field [0001] The invention relates to a class of metallocene compounds and a preparation method thereof, in particular to the preparation of bridged metallocene complexes and their application in olefin homopolymerization. Background technique [0002] In the early 1950s, Ziegler-Natta catalyst (J.Am.Chem.Soc., 1957, 79, 2975) was successfully applied to olefin polymerization, which led to the rapid development of metal organic compound chemistry. In the early 1980s, Sinn (Angew.Chem.Int.Ed.Engl., 1980, 92, 396) and Kaminsky (Macromol.Chem., Rapid Commun., 1983, 4, 417) and others discovered metallocene complexes The homogeneous catalytic olefin polymerization system composed of MAO, compared with the traditional Ziegler-Natta catalyst, the electronegativity and space environment of the active center of the metallocene catalyst can have a large change, which makes the composition of the polymer chain generated and highly controllable structures. Even small change...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F19/00B01J31/22C08F110/02C08F110/06C08F4/6592
Inventor 黄吉玲黄文忠郝超马海燕
Owner EAST CHINA UNIV OF SCI & TECH
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