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Bis-silicon-bridged metallocene compound, preparation method and application thereof

A technology of metallocene compound and silicon bridge, which is applied in the field of double silicon bridge metallocene compound, can solve the problem of no substituent group in the bridged ring, and achieve the effect of high olefin polymerization activity

Active Publication Date: 2010-02-03
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0026] Obviously, there is no substituent on the bridging ring of this compound

Method used

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  • Bis-silicon-bridged metallocene compound, preparation method and application thereof
  • Bis-silicon-bridged metallocene compound, preparation method and application thereof
  • Bis-silicon-bridged metallocene compound, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Ligand L1{μ,μ-[(Me 2 Si) 2 (η 5 -AllylC 5 h 2 ) 2 ]}Synthesis

[0058] Add 50mL (0.42mol) (CH 3 ) 2 SiCl 2 , and then add 100 mL of n-hexane, and stir evenly. Add 260 mL (0.84 mol) of 1.6 M CpNa dropwise under ice-water bath conditions, react for 6 hours, add 50 mL 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 × 20 mL of 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, and obtain 18.05 g of a light yellow liquid product; add the above product to a 250 mL Schlenk bottle, and dissolve with 80 mL of n-hexane. Add about 53mL of 1.8M n-BuLi dropwise under ice-water bath, stir the reaction for 4 hours, then add 11.6mL (CH 3 ) 2 SiCl 2 and 20mLTHF, stirred overnight. Precipitate after completion of the reaction, filter the supernatant, concentrat...

Embodiment 2

[0060] Ligand L2{μ,μ-[(Me 2 Si) 2 (η 5 -BuC 5 h 2 ) 2 ]}Synthesis

[0061] Add 50mL (0.42mol) (CH 3 ) 2 SiCl 2 , and then add 100 mL of n-hexane, and stir evenly. Add 260 mL (0.84 mol) of 1.6 M CpNa dropwise under ice-water bath conditions, react for 6 hours, add 50 mL 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 × 20 mL of 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, and obtain 18.05 g of a light yellow liquid product; add the above product to a 250 mL Schlenk bottle, and dissolve with 80 mL of n-hexane. Add about 53mL of 1.8M n-BuLi dropwise under ice-water bath, stir the reaction for 4 hours, then add 11.6mL (CH 3 ) 2 SiCl 2 and 20mLTHF, stirred overnight. Precipitate after completion of the reaction, filter the supernatant, concentrate u...

Embodiment 3

[0063] Ligand L3{μ,μ-[(Me 2 Si) 2 (η 5 -Me 3 SiC 5 h 2 ) 2 ]}Synthesis

[0064] Also press embodiment 1 method, use Me 3 SiCl replaces allyl bromide, and the ligand L3{μ,μ-[(Me 2 Si) 2 (η 5 -Me 3 SiC 5 h 2 ) 2 ]} white solid 52mmol, product yield 52%.

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Abstract

The invention relates to a bis-silicon-bridged metallocene compound, a preparation method and application thereof. Substituents such as alkyl, alkenyl and silicon base are introduced to a double bridge ligand and a cyclopentadienyl ring of CpMC3, particularly to the double bridge ligand to obtain a series of bis-silicon-bridged metallocene compounds containing the substituents on the bridged cyclopentadienyl ring; the compound has a simple synthetic route, high product yield, and easy separation and purification and less needed cocatalyst when the compounds are used for catalyzing the copolymerization between ethylene such as ethylene / hexene-1, ethylene / octylene-1 and the like and long chain alpha-olefin; the compound has high catalytic activity, the long chain alpha-olefin has high insertion rate; the compound catalyzes the copolymerization of the ethylene / hexene-1, the polymerization activity is 3.22*10<6>gPE / mol.cat.h., and the content of hexene-1 in a polymer is 6.83 percent; and the compound catalyzes the copolymerization of the ethylene / octylene-1, the polymerization activity is 2.64*10<6>gPE / mol.cat.h., and the content of octylene-1 in the polymer is 5.26 percent.

Description

technical field [0001] The invention relates to a double-silicon bridged metallocene compound with substituents on the bridged metallocene ring and its preparation method, and its application in ethylene polymerization, ethylene / 1-hexene and ethylene / 1-octene copolymerization. Background technique [0002] In the 1950s, Ziegler-Natta (G.Natta; P.Ginnini, J.Am.Chem.Soc., 1954, 79:2975) catalysts were successfully applied to the polymerization of ethylene and propylene; since 1960, a large number of new metal Organic compounds have been successfully synthesized, providing industry with a series of new catalysts with high activity and high selectivity, which are widely used in α-olefin polymerization and various organic chemical reactions, and have also shown great vitality in the synthesis of new materials and life sciences. [0003] In the 1980s, Kaminsky et al. (W.Kaminsky, M.Miri, H.Sinn, R.Woldt, Makromol.Common., 1983, 4:417) found that methylaluminoxane (MAO) and Cp 2 Z...

Claims

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Application Information

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IPC IPC(8): C07F17/00C08F4/6592C08F10/02
Inventor 米普科钱锦华王斯晗许胜李建忠张德顺邢秋菊张宝军刘敏曲家波张琰陈谦阎修维王桂芝卢攀峰韩雪梅江玲孙淑坤杨俊凤李玉龙黄付玲王亚丽王秀慧王力搏张志凤张婧元张学业张文超
Owner PETROCHINA CO LTD
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