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Synthesis method of C2 bridged metallocene Ti-rare earth dinuclear catalyst

A synthesis method, metallocene technology, applied in the field of polyolefins, can solve the problems of difficult post-processing, low total yield, high cost, etc., and achieve the effect of avoiding the use of expensive reagents, short synthesis route and high yield

Inactive Publication Date: 2013-03-13
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 difficult post-processing

Method used

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  • Synthesis method of C2 bridged metallocene Ti-rare earth dinuclear catalyst
  • Synthesis method of C2 bridged metallocene Ti-rare earth dinuclear catalyst
  • Synthesis method of C2 bridged metallocene Ti-rare earth dinuclear catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0072] 1) Synthesis of fluorenyl ligands

[0073] Dissolve 9-chloro-10-bromo-1-decene in petroleum ether, lower the temperature to -20°C, slowly add fluorene lithium solution dropwise for 2 hours, and continue the reaction for 12 hours after the addition; 9-chloro-10 The molar ratio of bromo-1-decene to fluorene lithium is: 9-chloro-10-bromo-1-decene: fluorene lithium = 1:1.

[0074] 2) Synthesis of C2 bridged indenyl fluorenyl ligands

[0075] Step 1) adding solvent tetrahydrofuran to the obtained fluorenyl ligand, and then reacting with indenyl lithium to obtain a C2 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 16 hours.

[0076] 3) Synthesis of Ligand Lithium Salt

[0077] 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 com...

Embodiment 2

[0085] Others are the same as embodiment 1, the difference is:

[0086] 1) Synthesis of fluorenyl ligands

[0087] Dissolve 9-chloro-10-bromo-1-decene in petroleum ether, lower the temperature to -10°C, slowly add the fluorene lithium solution dropwise for 1.5 hours, and continue the reaction for 16 hours after the addition; 9-chloro-10 The molar ratio of bromo-1-decene to lithium fluorene is: 9-chloro-10-bromo-1-decene:lithium fluorene=1.1:1.

[0088] 2) Synthesis of C2 bridged indenyl fluorenyl ligands

[0089] Step 1) adding solvent tetrahydrofuran to the obtained fluorenyl ligand, and then reacting with indenyl lithium to obtain a C2 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.

[0090] 3) Synthesis of Ligand Lithium Salt

[0091] Dissolve the ligand obtained in step 2) in n-hexane, add n-butyllithium dropwise, the dropping temperature is 0°C, and the mo...

Embodiment 3

[0098] Others are the same as embodiment 1, the difference is:

[0099] 1) Synthesis of fluorenyl ligands

[0100] Dissolve 9-chloro-10-bromo-1-decene in anhydrous ether, cool down to 0°C, slowly add fluorene lithium solution dropwise for 1 hour, and continue to react for 14 hours after the addition; 9-chloro-10 The molar ratio of bromo-1-decene to fluorene lithium is: 9-chloro-10-bromo-1-decene: fluorene lithium = 1:1.

[0101] 2) Synthesis of C2 bridged indenyl fluorenyl ligands

[0102] Step 1) adding solvent tetrahydrofuran to the obtained fluorenyl ligand, and then reacting with indenyl lithium to obtain a C2 bridged indenyl fluorenyl ligand. The molar ratio of fluorenyl ligand to indene lithium is 1:1; the reaction temperature is -5°C; the reaction time is 13 hours.

[0103] 3) Synthesis of Ligand Lithium Salt

[0104] Dissolve the ligand obtained in step 2) in n-hexane, add n-butyllithium dropwise, the dropping temperature is 10°C, and the molar ratio of ligand to n...

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Abstract

The invention provides an iso-C2 bridged metallocene Ti-rare earth dinuclear catalyst represented by the following structural formula, wherein M refers to rare earth. The invention further provides a preparation method of the catalyst. The catalyst can be matched with a cocatalyst, namely alkylaluminoxane for olefinic polymerization, has high polymerization activity and can obtain olefinic polymerization products with high molecular weight and broad 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. People try to use composite catalysis (see KAMINSKY W, STEIGER R. Polymerization of olefins with homogeneous zirconocene / alumoxane catalysts, Polyhedron, 1988, 7(22-23): 2375-2381) or dual-core multi-nuclear catalysts (see Feng Zuofeng, Xie Jun, Che...

Claims

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Application Information

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