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Binuclear metallocene compound and its preparation and application in olefinic polymerization

A technology of metallocene compounds and compounds, applied in the field of binuclear metallocene compounds, can solve problems such as poor processability, narrow polyolefin molecular weight distribution, and increased processing difficulty

Inactive Publication Date: 2003-07-09
CHINA PETROLEUM & CHEM CORP +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the narrow molecular weight distribution of polyolefins produced by metallocene catalysts, the processing performance is poor, which increases the processing difficulty in the process.

Method used

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  • Binuclear metallocene compound and its preparation and application in olefinic polymerization

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preparation example Construction

[0016] The preparation method of compound (I) can refer to T Ushioda, et al, J. Organomet. Chem, 518 (1996) 155-166. The detailed preparation steps are as follows: the structural expression is The silane compound ligand is dissolved in n-hexane, and n-butyllithium is added dropwise at a temperature of -30 to 20°C, preferably -10 to 0°C. The molar ratio to n-butyllithium is 1:2.0-2.5. After the dropwise addition is completed, it is naturally raised to room temperature and reacted for 8-15 hours. The solvent was removed by filtration, and the solvent was sucked dry under reduced pressure. This gives the compound of formula (II) as the lithium salt of the Si-bridged biscyclopentadienyl ligand. Toluene was added to the solid lithium salt to obtain a white turbid liquid, namely the suspension of the above lithium salt. Add CpM at room temperature 1 Cl 3 DME, wherein DME is ethylene glycol dimethyl ether, Cp is cyclopentadienyl, M 1 for zirconium. CpM 1 Cl 3 ·The molar ra...

example 1

[0021] The preparation formula is Ligand Compound A.

[0022] Will 5 grams (0.0266mol) was dissolved in 80 ml of n-hexane, and 0.0532mol of n-butyllithium was added dropwise in an ice-water bath. After the dropwise addition, the ice bath was removed, and the mixture was naturally raised to room temperature and reacted overnight. The solvent was removed by filtration and dried under vacuum. 150 ml of toluene was added to obtain a white cloudy liquid. Add 9.36 g of cyclopentadienyl zirconium trichloride ethylene glycol dimethyl ether (CpZrCl 3 ·DME), stirred at 25°C for 24 hours. After centrifugation, the residue was extracted twice with 50 ml of dichloroethane, the centrifuged liquid and the extract were combined, concentrated until a solid appeared, and left standing at -20°C for 24 hours to obtain 1.933 g of pale yellow needle-like crystals, which was compound A. Yield 19.2 wt%.

example 2

[0024] The preparation formula is Ligand compound B

[0025] Will 5 grams (0.0266 mol) was dissolved in 80 ml of n-hexane, and 0.0532 mol of n-butyllithium was added dropwise under an ice-water bath. After the dropwise addition, the ice bath was removed, and the mixture was naturally raised to room temperature, and reacted overnight. The solvent was removed by filtration and dried under vacuum. 5.30 g of a white powdery solid was obtained, which was compound B, and the yield was 99.6% by weight.

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Abstract

The present invention relates to a binuclear metallocene compound, its preparation method and its application in olefinic polymerization. Said invention provides its structure expression formula, said compound can be matched with cocatalyst alkyl aluminoxane, and used for olefinic polymerization. It possesses high polymerization reaction activity, and can obtain olefinic polymerization product with high molecular weight and wide molecular weight distribution.

Description

technical field [0001] The invention relates to a class of dinuclear metallocene compound and its preparation and application of the compound as a catalyst in olefin polymerization. Background technique [0002] Since the 1950s, metallocene catalysts have been a research hotspot in catalytic olefin polymerization. In the early 1980s, the discovery of Kaminsky cocatalyst methylaluminoxane pushed the catalytic polymerization of olefins into a new research climax. Compared with the traditional Ziegler-Natta catalytic system, metallocene catalysts have the outstanding advantages of being able to control the molecular weight, molecular weight distribution, comonomer content and stereoregularity of polymers. However, because the molecular weight distribution of polyolefins produced by metallocene catalysts is too narrow, the processability is poor, which increases the processing difficulty in the process. At present, the focus of some work has shifted to the synthesis and perform...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F4/642C08F10/00
Inventor 钱延龙冯作峰黄吉玲王红陈伟郑刚孙俊全
Owner CHINA PETROLEUM & CHEM CORP
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