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Metallocene catalyst and preparation method thereof

A metallocene catalyst and catalyst technology, applied in the field of polyolefins, can solve the problems of high cost, low total yield, and many steps, and achieve the effect of short synthesis route, high yield, and avoiding the use of expensive reagents

Inactive Publication Date: 2011-09-14
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.

Method used

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  • Metallocene catalyst and preparation method thereof
  • Metallocene catalyst and preparation method thereof
  • Metallocene catalyst and preparation method thereof

Examples

Experimental program
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preparation example Construction

[0040] The preparation method of catalyst (II) is as follows:

[0041] 1) Synthesis of fluorenyl ligands

[0042] Dissolve 5,6-dichloro-1-hexene in an organic solvent, lower the temperature to -90~-60°C, slowly add the fluorene lithium solution dropwise, the dropping time is 0.5~1 hour, and continue to react for 8~12 hours after the addition is completed ; The molar ratio of 5,6-dichloro-1-hexene and fluorene lithium is: 5,6-dichloro-1-hexene: fluorene lithium=3~10:1

[0043] The organic solvent is selected from dichloromethane, toluene, tetrahydrofuran.

[0044] The synthesis method is shown in the following formula:

[0045]

[0046] Theoretically, the reaction of 5,6-dichloro-1-hexene with lithium fluorene will give the ligands of the two structures shown in the structural formulas A and B in the above formula, but in fact, due to the large volume of lithium fluorene, There is a large steric hindrance effect, so, under the low temperature and long reaction time of the...

Embodiment 1

[0077] 1) Synthesis of fluorenyl ligands

[0078] Dissolve 0.5mol of 5,6-dichloro-1-hexene in 200ml of tetrahydrofuran, cool down to -78°C, slowly add 0.05mol of lithium fluorene in petroleum ether, dropwise for 1 hour, and continue the reaction for 12 hours; the product was hydrolyzed, separated and purified, and the yield was 80.1%.

[0079] 2) Synthesis of C2 bridged indenyl fluorenyl ligand

[0080] -78°C, 62mmol indene lithium in 100ml petroleum ether solution, slowly added dropwise to 61mmol of the fluorenyl ligand obtained in step 1), stirred and reacted for 24 hours; the product was hydrolyzed, separated and purified, and the yield was 52.3%.

[0081] 3) Synthesis of Ligand Lithium Salt

[0082] 0.0266 mol of ligand was dissolved in 80 ml of n-hexane, and 0.0532 mol of n-butyl lithium was added dropwise in an ice-water bath. After the dropwise addition was completed, the solution was naturally raised to room temperature and reacted for 10 hours. The n-hexane was remov...

Embodiment 2

[0089] 1) Synthesis of fluorenyl ligands

[0090] Dissolve 0.5mol of 5,6-dichloro-1-hexene in 200ml of toluene, cool down to -90°C, slowly add 0.10mol of fluorenelithium petroleum ether solution for 1.5 hours, and continue the reaction for 10 hours; the product was hydrolyzed, separated and purified, and the yield was 83.2%.

[0091] 2) Synthesis of C2 bridged indenyl fluorenyl ligand

[0092] -90°C, 60mmol indene lithium in 100ml petroleum ether solution was slowly added dropwise to 59mmol of the fluorenyl ligand obtained in step 1), and the reaction was stirred for 48 hours; the product was hydrolyzed, separated and purified, and the yield was 54.1%.

[0093] 3) Synthesis of Ligand Lithium Salt

[0094] Dissolve 0.025 mol of ligand in 80 ml of ether, add 0.061 mol of n-butyllithium dropwise in an ice-water bath, after the addition is complete, let it rise to room temperature naturally, and react for 8 hours. The n-hexane was removed by filtration, and the n-hexane was suc...

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Abstract

The invention provides a heterobinuclear metallocene catalyst of which the structural formula is shown in the specifications, wherein M is rare earth. The invention further provides a preparation method of the catalyst. The catalyst is applied to olefinic polymerization together with alkyl aluminoxane serving as a catalyst promoter, and has high polymerization reactivity. By adopting the catalyst, an olefinic polymerization product with high molecular weight and wide molecular weight distribution can be obtained.

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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IPC IPC(8): C08F10/00C08F10/02C08F10/06C08F4/6592
Inventor 班青
Owner QILU UNIV OF TECH
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