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Bridged dinuclear metallocene compound for sPP as well as preparation method and application thereof

A technology of metallocene compounds and compounds, applied in metallocenes, chemical instruments and methods, organic chemistry, etc., can solve problems such as molecular weight reduction, achieve stable steric configuration, increase complex yield, and high activity

Active Publication Date: 2015-04-15
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Moreover, contrary to mononuclear catalytic systems, the molecular weight decreases with increasing Al / Zr ratio

Method used

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  • Bridged dinuclear metallocene compound for sPP as well as preparation method and application thereof
  • Bridged dinuclear metallocene compound for sPP as well as preparation method and application thereof
  • Bridged dinuclear metallocene compound for sPP as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Ligand L1[(CH 3 ) 2 C(C 5 h 4 )(C 13 h 9 )] 2 (CH 2 C 6 h 4 CH 2 )Synthesis

[0056] Ligand L1[(CH 3 ) 2 C(C 5 h 4 )(C 13 h 9 )] 2 (CH 2 C 6 h 4 CH 2 ) The synthetic route is as follows:

[0057]

[0058] Under the protection of argon, with carbon tetrachloride as a solvent, p-xylene (5.04g, 47.53mmol), NBS (30g) and BPO (2g) were added to the bottle for reaction, heated, and when heated to 70°C, The solid and liquid in the bottle begin to melt, after stabilization, continue heating to 80°C, reflux for 20 hours, cool down, there is white solid in the upper layer, light yellow clear liquid in the lower layer, cool to 40°C, filter, take the filtrate, put it in the refrigerator After 24 hours, white crystals, about 5 g, were p-dibromobenzyl, and the yield was 40%.

[0059] Add fluorene (10g, 60.24mmol), 100mL of n-hexane, and 20mL of diethyl ether into a 200mL Schlenk bottle, and slowly add n BuLi (36.7mL, 1.64mol / L), a precipitate formed immedia...

Embodiment 2

[0067] Ligand L2[(C 6 h 5 ) 2 C(C 5 h 4 )(C 13 h 9 )] 2 (CH 2 C 6 h 4 CH 2 )Synthesis

[0068] At 0°C, a solution of 6,6-diphenylfulvene (11.08g, 48.18mmol) in ether (40mL) was added dropwise to a solution of FluLi (8g, 48.18mmol) in ether (80mL). After 8 hours, Precipitation appeared, and a large amount of precipitates formed after 20 hours of reaction. The solvent was removed by pressure filtration, and the solid was washed twice with ether and once with hexane, and dried to obtain 12.41 g of solid, with a yield of 65%.

[0069] The above-mentioned lithium salt (15.19mmol) of 6.18g is dissolved in 50mLTHF, and yellowish redness, under ice bath, slowly add the THF (40mL) solution (light yellow) of p-dibromide (2.01g, 7.59mmol) dropwise, rise naturally to After room temperature, the color of the solution deepened slightly, dark red to yellow, and reacted for two days. For hydrolysis, use acetic acid to adjust the pH to neutral, separate the liquids, take the organ...

Embodiment 3

[0075] Ligand L3[(CH 2 ) 5 C(C 5 h 4 )(C 13 h 9 )] 2 (CH 2 C 6 h 4 CH 2 )Synthesis

[0076] Under ice-cooling, a solution of 6,6-pentamethylenefulvene (8.89g, 48.18mmol) in ether (40mL) was added dropwise to a solution of FluLi (8g, 48.18mmol) in ether (80mL). Precipitation was formed. After about 8 hours, a precipitate appeared. After 20 hours of reaction, a large amount of precipitate was formed. The solid was washed twice with ether and once with hexane, and dried to obtain 11.49 g of solid, with a yield of 68%.

[0077] The above-mentioned lithium salt (15.19mmol) of 4.91g is dissolved in 50mLTHF, and yellowish redness, under ice bath, slowly add the THF (40mL) solution (light yellow) of p-dibromide (2.01g, 7.59mmol) dropwise, rise naturally to After room temperature, the color deepened slightly, dark red to yellowish, and reacted for 40 hours. Hydrolyze, adjust the pH to neutral with acetic acid, separate the liquids, take the organic phase, extract the aqueou...

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Abstract

The invention provides a bridged dinuclear metallocene compound for sPP as well as a preparation method and application thereof. The structure of the metallocene compound is as shown in the formula I, wherein R1 is selected from hydrogen, methyl, methylene, ethyl and phenyl; R2 is selected from hydrogen, tert-butyl, bromine and chlorine. The preparation method of the compound comprises the following steps: carrying out a reaction on p-xylene, N-bromosuccinimide and benzoyl peroxide to obtain p-cyclite; carrying out a reaction on an alkene-enriched compound and a fluorene lithium compound to obtain bridged lithium fluorene metallocene salt; carrying out a reaction on p-cyclite and the bridged lithium fluorene metallocene salt to obtain a ligand; carrying out a reaction on the ligand and n-butyl lithium, and carrying out a reaction with zirconium tetrachloride to obtain the bridged dinuclear metallocene compound for sPP. The invention further provides the application for using the metallocene compound as a catalyst to catalyze a propylene polymerization reaction.

Description

technical field [0001] The invention relates to a bridging dinuclear metallocene compound for SPP and a preparation method and application thereof, belonging to the technical field of metallocene catalysts. Background technique [0002] Since Fina produced sPP in a liquid-phase loop reactor in 1993, foreign companies such as Basell, Huntsman, Dow, ExxonMobil, Mitsui Topress, and Idemitsu Petrochemical have devoted themselves to the development of sPP. At present, Fina, Basell, ExxonMobil, and Japan's Idemitsu Petrochemical Company have realized the industrial production of sPP. [0003] This kind of mononuclear metallocene catalyst has become the focus of research by scientists from all over the world. The mononuclear catalyst that has been patented covers almost all aspects of this research field, and it is difficult to have great original innovation. It is a new field of research to connect bridging mononuclear metallocene compounds with certain bridging groups to obtain ...

Claims

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Application Information

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IPC IPC(8): C07F17/00C08F4/6592C08F10/06
CPCC07F17/00C08F10/06C08F4/65927
Inventor 米普科许胜刘敏
Owner PETROCHINA CO LTD
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