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Synthetic method of bridged metallocene dinuclear catalyst

A synthesis method and metallocene technology, applied in the field of polyolefins, can solve the problems of cumbersome post-processing, low total yield, and many steps, and achieve the effects of avoiding the use of expensive reagents, short synthesis routes, and high yields

Inactive Publication Date: 2013-03-27
QILU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent applications 200710015194.2 and 200710015193.8 disclose bridged metallocene binuclear catalysts and their preparation methods, but there are many steps, high cost and low overall yield.
201110030833.9 discloses a C2 bridged metallocene Zr-rare earth binuclear catalyst and its preparation method, but there are many steps and cumbersome post-processing

Method used

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  • Synthetic method of bridged metallocene dinuclear catalyst
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  • Synthetic method of bridged metallocene dinuclear catalyst

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preparation example Construction

[0029] The preparation method of bridged metallocene dinuclear catalyst is as follows:

[0030] 1) Synthesis of fluorenyl ligands

[0031] Dissolve 5-chloro-6-bromo-1-hexene in an organic solvent, lower the temperature to -30-0°C, slowly add the fluorene lithium solution dropwise, the dropping time is 1.5-2.5 hours, and continue the reaction for 10-12 hours after the dropping ;

[0032] The molar ratio of 5-chloro-6-bromo-1-hexene to lithium fluorene is: 5-chloro-6-bromo-1-hexene:lithium fluorene=1~1.1:1;

[0033] The organic solvent is selected from anhydrous diethyl ether or petroleum ether.

[0034] The synthesis method is shown in the following formula:

[0035] .

[0036] The choice of solvent is very important. Using anhydrous ether or petroleum ether as a solvent can effectively control the degree of reaction, and can control the reaction of Br in 5-chloro-6-bromo-1-hexene, while Cl does not react. . When using dichloromethane, toluene or tetrahydrofuran and oth...

Embodiment 1

[0058] 1) Synthesis of fluorenyl ligands

[0059] Dissolve 5-chloro-6-bromo-1-hexene in petroleum ether, lower the temperature to -30°C, slowly add fluorene lithium solution dropwise for 2 hours, and continue the reaction for 10 hours after the addition; 5-chloro-6 The molar ratio of bromo-1-hexene to lithium fluorene is: 5-chloro-6-bromo-1-hexene:lithium fluorene=1:1.

[0060] 2) Synthesis of bridged indenylfluorenyl ligands

[0061] Step 1) adding solvent tetrahydrofuran to the obtained fluorenyl ligand, and then reacting with indene lithium to obtain a bridged indenyl fluorenyl ligand. The molar ratio of fluorenyl ligand to indene lithium is 1:1; the reaction temperature is -20°C; the reaction time is 18 hours.

[0062] 3) Synthesis of Ligand Lithium Salt

[0063] Dissolve the ligand obtained in step 2) in n-hexane, add n-butyllithium dropwise, the dropping temperature is -20°C, the molar ratio of ligand to n-butyllithium is 1:2.2, after the addition is completed, the na...

Embodiment 2

[0070] 1) Synthesis of fluorenyl ligands

[0071] Dissolve 5-chloro-6-bromo-1-hexene in petroleum ether, lower the temperature to -20°C, slowly add the fluorene lithium solution dropwise, the dropwise addition time is 2.5 hours, and continue the reaction for 8 hours after the addition; 5-chloro-6 The molar ratio of bromo-1-hexene to lithium fluorene is: 5-chloro-6-bromo-1-hexene:lithium fluorene=1.1:1.

[0072] 2) Synthesis of bridged indenylfluorenyl ligands

[0073] Step 1) adding solvent tetrahydrofuran to the obtained fluorenyl ligand, and then reacting with indene lithium to obtain a bridged indenyl fluorenyl ligand. The molar ratio of fluorenyl ligand to indene lithium is 1:1; the reaction temperature is -10°C; the reaction time is 14 hours.

[0074] 3) Synthesis of Ligand Lithium Salt

[0075] Dissolve the ligand obtained in step 2) in n-hexane, add n-butyllithium dropwise, the dropping temperature is 0°C, the molar ratio of ligand to n-butyllithium is 1:2.5, after t...

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Abstract

The invention provides a bridged metallocene dinuclear catalyst expressed in the following structural formula, wherein M=Ti or Zr. The invention also provides a preparation method of the catalyst. The catalyst is combined with a cocatalyst of aluminum alkyl aluminoxane for olefin polymerization, has high polymerization reactivity, and can obtain olefin polymerization products with a high molecular weight and wide molecular weight distribution.

Description

technical field [0001] The invention belongs to the field of polyolefin and relates to a catalyst for olefin polymerization, in particular to a bimetallic catalyst for ethylene and propylene polymerization and a preparation method thereof. Background technique [0002] Metallocene catalysts have a single active center, high catalyst activity, and polymers with very high tacticity can be obtained, and the obtained polymers have high molecular weight, and the molecular weight and molecular weight distribution can be controlled by changing the ligand structure. extensive attention. However, due to the narrow molecular weight distribution of polyolefin obtained, it is difficult to process, which limits its industrialization process. Attempts have been made to improve the molecular weight distribution of polymers with composite catalysis or dual-core multi-core catalysts. [0003] Green and his colleagues synthesized Si-bridged dinuclear compounds (T.Ushioda, M.L.H.Green, J.Hag...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F4/6592C07F17/00C08F10/00C08F10/02C08F10/06
Inventor 班青
Owner QILU UNIV OF TECH
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