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Multinuclear metallocene complex and application thereof

A metallocene complex and multi-nuclear technology, applied in the field of multi-nuclear metallocene complexes, can solve the problems of narrow molecular weight distribution, damage, and increased cost of polymers

Inactive Publication Date: 2007-08-15
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Metallocene catalysts have the advantages of a single active center and controllable polymer structure and molecular weight, so they have become a class of olefin polymerization catalysts with excellent performance after Ziegler-Natta catalysts. However, due to the narrow molecular weight distribution of the obtained polymers, processing Difficulty has become one of the important reasons hindering the industrialization process. In order to solve this problem, people mix different metallocene compounds to make composite catalysts to catalyze the polymerization of olefins or to mix polymers obtained by metallocene-catalyzed olefin polymerization to broaden the The molecular weight distribution of the polymer, but this method often destroys the characteristics of the metallocene catalyst itself and increases the cost
Therefore, in recent years, the design and synthesis of dinuclear or multinuclear metallocene compounds has become a major research focus in the field of metallocene-catalyzed olefin polymerization. Since there are multiple metal centers in the catalyst molecule, more than one active center can be formed during the polymerization process. , so that polyolefins with wide molecular weight distribution or bimodal distribution can be obtained. So far, there are many reports on the synthesis of binuclear metallocene compounds and their application in olefin polymerization, but the synthesis of multi-nuclear metallocene compounds and their application in olefin polymerization There is very little applied research

Method used

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  • Multinuclear metallocene complex and application thereof
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  • Multinuclear metallocene complex and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] 1,3,5-Tris(cyclopentadienylmethylene)benzene C 6 h 3 (CH 2 C 5 h 5 ) 3 Synthesis of -1,3,5(1)

[0051]

[0052] Under the protection of argon, at -78°C, a 40 mL tetrahydrofuran solution containing 1.79 g (5 mmol) of 1,3,5-tris(bromomethyl)benzene [1,3,5-tris(bromomethyl)benzene] was dropped Add it to 30 mL of tetrahydrofuran solution containing 15 mmol of cyclopentadienyl sodium salt, stir while adding, and naturally raise the temperature to 0°C after the addition, and continue to stir and react at 0°C for two hours. Remove the solvent in vacuo, add 30ml of distilled water and 30ml of diethyl ether to the residue, separate the layers, extract the water phase with 30ml of diethyl ether twice, combine the diethyl ether phases, and dry with anhydrous magnesium sulfate or calcium hydride. The solvent was removed in vacuo to obtain 1.49 g of light yellow oily ligand 1,3,5-tris(cyclopentadienylmethylene)benzene (1), with a yield of 95.5%.

[0053] 1 H NMR (CDCl 3 ...

Embodiment 2

[0055] 1,2,4,5-Tetrakis(cyclopentadienylmethylene)benzene C 6 h 2 (CH 2 C 5 h 5 ) 4 Synthesis of -1, 2, 4, 5(2)

[0056]

[0057] Under argon protection, at -78°C, 1.69g (3.75mmol) of 1,2,4,5-tetrakis(bromomethyl)benzene[1,2,4,5-tetrakis(bromomethyl)benzene] Add 40mL of THF solution to 30mL THF solution containing 15mmol of cyclopentadienyl sodium salt dropwise, and stir while adding. After the addition, the temperature is naturally raised to 0°C, and the stirring reaction is continued at 0°C for two hours. Remove the solvent in vacuo, add 30ml of distilled water and 30ml of diethyl ether to the residue, separate the layers, extract the water phase with 30ml of diethyl ether twice, combine the diethyl ether phases, and dry with anhydrous magnesium sulfate or calcium hydride. The solvent was removed in vacuo to obtain 1.38 g of light yellow oily ligand 1,2,4,5-tetrakis(cyclopentadienylmethylene)benzene (2), with a yield of 94.5%.

[0058] 1 H NMR (CDCl 3 , δ, ppm): ...

Embodiment 3

[0060] Bridged trinuclear titanocene C 6 h 3 [CH 2 C 5 h 4 Ti(C 5 h 5 )Cl 2 ] 3 Synthesis of -1,3,5(3)

[0061]

[0062] Under argon protection at 0°C, 5.6ml (9mmol, butyllithium concentration of 1.6mol / l) n-hexane solution of butyllithium was added dropwise to 0.94g (3mmol) 1,3,5-tri( Cyclopentadienyl methylene) benzene [C 6 h 3 (CH 2 C 5 h 5 ) 3 -1, 3, 5] (1) In 50ml ether solution, stir while adding, naturally warm up to room temperature after addition, stir overnight, filter, wash the solid three times with 20ml ether respectively, and vacuum dry to obtain light yellow powder Lithium salt. At 0°C, slowly add the powder to 60ml of toluene solution containing 1.97g (9mmol) of mono-titanocene, stir while adding, after the addition, naturally warm to room temperature, stir overnight, filter, and the solids are respectively washed with 40ml of two Extracted 4 times with methyl chloride, combined the extracts, concentrated in vacuo, and placed the concentrated...

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Abstract

The invention discloses a new polynuclear metallocene complex and application in the catalytic polymeric ethylene, whose general molecular formula is Ar-bR, wherein Ar is non-substituted or substituted phenyl; R is substituted radical on Ar directly; b is the quantity of substituted radical R on Ar, which is integral between 2 and 6; when R is multiple, it can be different metallocene complexes mutually; Ar is core of multiple substituted radical R.

Description

technical field [0001] The invention relates to a new multinuclear metallocene complex and the application of the multinuclear metallocene complex in olefin polymerization. Background technique [0002] Metallocene catalysts have the advantages of a single active center and controllable polymer structure and molecular weight, so they have become a class of olefin polymerization catalysts with excellent performance after Ziegler-Natta catalysts. However, due to the narrow molecular weight distribution of the obtained polymers, processing Difficulty has become one of the important reasons hindering the industrialization process. In order to solve this problem, people mix different metallocene compounds to make composite catalysts to catalyze the polymerization of olefins or to mix polymers obtained by metallocene-catalyzed olefin polymerization to broaden the The molecular weight distribution of the polymer, but this method often destroys the characteristics of the metallocene...

Claims

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Application Information

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IPC IPC(8): C07F17/00C08F4/76C08F10/02
Inventor 肖孝辉孙俊全林峰聂玉静刘希杰
Owner ZHEJIANG UNIV
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