Bis-silicon-bridged dinuclear metallocene compound and preparation and application thereof

A technology of metallocene compound and silicon bridge, which is applied in the field of double-silicon bridge and dinuclear metallocene compound, can solve the problems of olefin polymerization that have not been reported, and achieve the effect of improving catalyst performance and high olefin polymerization activity

Active Publication Date: 2012-08-08
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] No report on olefin polymerization

Method used

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  • Bis-silicon-bridged dinuclear metallocene compound and preparation and application thereof
  • Bis-silicon-bridged dinuclear metallocene compound and preparation and application thereof
  • Bis-silicon-bridged dinuclear metallocene compound and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] [μ,μ-(SiMe 2 ) 2 (n-BuC 5 h 2 )(CH 2 =CHCH 2 -C 5 h 2 )]Synthesis

[0055] Add 50mL (0.42mol) (CH 3 ) 2 SiCl 2 , and then add 100 mL of n-hexane, and stir evenly. Add 260mL (0.84mol) of 1.6M CpNa dropwise at 0°C, react for 6 hours, add 50mL of distilled water to wash, use a pear-shaped separatory funnel to separate liquid to remove the organic phase, wash the water phase with 3×20mL ether, and combine the organic phases , and with anhydrous MgSO 4 Dry, filter and remove solvent in vacuo. Distill under reduced pressure, collect fractions at 40-42°C / 2mmHg to obtain a light yellow liquid product. Take the above light yellow liquid product and add it to a 250mL Schlenk bottle, and dissolve it with 80mL n-hexane. Add about 53mL of 1.8M n-BuLi dropwise at 0°C, stir the reaction for 12 hours, then add 11.6mL (CH 3 ) 2 SiCl 2 and 20mLTHF, stirred for 12 hours. Precipitation occurred after the reaction, and the supernatant was filtered, concentrated until a sol...

Embodiment 2

[0059] [μ,μ-(SiMe 2 ) 2 (n-BuC 5 h 2 ) (MeC 5 h 2 )]Synthesis

[0060] Bis(dimethylsilyl) bridged dicyclopentadiene was synthesized according to the method in Example 1. Then take 4000 mL of tetrahydrofuran solution containing 1 mol of disilica-bridged dicyclopentadiene, add 1000 mL of hexane solution containing 1 mol of n-butyllithium at 0°C, react for half an hour, then naturally rise to room temperature, react for 10 hours, and drain Solvent, the solid was washed with 2000mL of n-hexane, then pumped dry, the solid was dissolved in 4000mL of THF, then cooled to -15°C with an acetone liquid nitrogen bath, 1mol of chlorobutane was added to react for 12 hours, the solvent was removed, and the solid was washed with n-hexane After extraction, add 500 mL of hexane solution containing 1 mol of n-butyllithium at 0°C for half an hour, slowly rise to about 25°C for 10 hours, then add 1.0 mol of methyl iodide at -10°C for 12 hours. In addition to solvent removal, n-hexane extrac...

Embodiment 3

[0062] [μ,μ-(SiMe 2 ) 2 ((CH 3 ) 3 Si-C5 h 2 )(CH 2 =CHCH 2 -C 5 h 2 )]Synthesis

[0063] Bis(dimethylsilyl) bridged dicyclopentadiene was synthesized according to the method in Example 1. Then take 4000 mL of tetrahydrofuran solution containing 1 mol of disilica-bridged dicyclopentadiene, add 1000 mL of hexane solution containing 1.0 mol of n-butyllithium at 0°C, react for half an hour, then naturally rise to room temperature, react for 12 hours, pump Dry the solvent, wash the solid with 1500mL of n-hexane, then drain it, dissolve the solid with 4000mL of THF, then cool it down to -15°C with an acetone liquid nitrogen bath, add 1.0mol of trimethylchlorosilane to react for 16 hours, remove the solvent, and the solid After extraction with n-hexane, add 500mL hexane solution containing 1mol n-butyllithium at 0°C for half an hour, slowly rise to about 25°C and react for 10 hours, then add 1mol allyl bromide at 0°C for reaction 14 Hours, after solvent removal, n-hexane e...

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Abstract

The invention relates to a bis-silicon-bridged dinuclear metallocene compound and preparation and application thereof. The bridged cyclopentadienyl rings of the bis-silicon-bridged dinuclear metallocene compound contain different substituents. Dimethyldichlorosilane reacts with cyclopentadienyl sodium, so that light yellow solution is obtained; the light yellow solution reacts with n-butyl lithium, and dimethyldichlorosilane is then added for reaction, so that bis-silicon-bridged dicyclopentadiene is obtained; the bis-silicon-bridged dicyclopentadiene reacts with n-butyl lithium, halogenide is then added for reaction, n-butyl lithium is then added for reaction, and finally, another halogenide is added for reaction, so that ligand L is obtained; and cyclopentadienyl titanium trichloride orcyclopentadienyl zirconium trichloride or substituetd cyclopentadienyl titanium trichloride or substituetd cyclopentadienyl zirconium trichloride is added in the ligand L, so that the compound is obtained. The synthesis route is reasonable, the yield is high, separation and purification are easy, the amount of needed cocatalysts is less when the compound is used for catalyzing the copolymerization of ethylene, such as ethylene / hexene-1, ethylene / octene-1 and ethylene / decylene, and long-chain Alpha-alkene, the catalytic activity is high, the insertion rate of the long-chain Alpha-alkene is high, and molecular weight distribution is wide.

Description

technical field [0001] The present invention relates to a di-silicon bridged dinuclear metallocene compound containing different substituents on the bridged alocene ring and its preparation method, and its application in ethylene polymerization, ethylene / 1-hexene and ethylene / 1-octene copolymerization . Background technique [0002] Since Professor Kaminsky of the University of Hamburg in the early 1980s discovered that the metallocene catalytic system composed of bis-cyclocene zirconium chloride and methylaluminoxane has high activity in catalyzing ethylene polymerization, various metallocene catalysts have been used for their excellent catalytic performance. The characteristics are widely used, and the market share is gradually increasing. The researchers also conducted in-depth studies on the molecular design of the catalyst and the structural properties of polyolefin materials. Studies have found that small changes in the structure of metallocene compounds, especially ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F17/00C07F7/08C08F4/76C08F210/16
CPCC07F17/00
Inventor 米普科张德顺许胜王斯晗张宝军钱锦华李建忠陈谦邢秋菊王桂芝张琰王力博刘敏杨忠华阎维修于部伟卢攀峰孙淑坤江玲韩雪梅杨俊凤黄付玲郭翔李玉龙王亚丽王秀绘韩文
Owner PETROCHINA CO LTD
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