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Non-bridged single/double-nucleus metallocene compound and uses thereof

A metallocene compound and bridging technology, which is applied to olefin polymerization catalysts and their preparation and application fields, can solve problems such as unfavorable catalyst stability, reduced catalytic activity and the like, and achieve the effect of improving application scope and added value.

Inactive Publication Date: 2011-09-14
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the stability of the catalyst also has its disadvantages. It is easy to form dimer oxygen-bridged metallocene compounds in the solution, thereby reducing its catalytic activity.

Method used

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  • Non-bridged single/double-nucleus metallocene compound and uses thereof
  • Non-bridged single/double-nucleus metallocene compound and uses thereof
  • Non-bridged single/double-nucleus metallocene compound and uses thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Example 1 Synthesis of 1-(4-methyl)-phenyl-2,3,4,5-tetramethylcyclopentadienyl ligand The reaction equation of the synthesis is:

[0037]

[0038] The specific process is: in N 2 Under the atmosphere, add 15.9ml 2,3,4,5-tetramethylcyclopent-2-en-1-one (36mmol) ether solution to the reaction flask, slowly drop 18ml, 2.0 under ice salt conditions M 4-methyl-phenyl lithium salt (4-Me-PhLi, 36 mmol) in ether. Under stirring conditions, gradually rise to room temperature and react for about 30 hours. The reaction mixture was poured into cold water, and the pH was adjusted to about 1 with hydrochloric acid. The aqueous layer was extracted with ether, and the combined organic phase was washed with 120 ml of saturated ammonium chloride aqueous solution, and then MgSO 4 dry. The desiccant was removed by filtration, the solvent was evaporated under reduced pressure, and column chromatography was separated (developing solvent: dichloromethane / petroleum ether = 1:1 mixed solvent) to...

Embodiment 2

[0041] Example 2 Synthesis of 1-(4-isopropyl)-phenyl-2,3,4,5-tetramethylcyclopentadienyl ligand

[0042] Under nitrogen atmosphere, add 15.90ml of ether solution containing 2,3,4,5-tetramethylcyclopent-2-en-1-one (36mmol) into the reaction flask, and slowly Add 20ml, 1.8M 4-isopropyl-phenyllithium salt (4-ipr-PhLi, 36mmol) in ether. . Under stirring conditions, gradually rise to room temperature and react for 30 hours. The reaction mixture was poured into ice water, and the pH was adjusted to about 1 with hydrochloric acid. The aqueous layer was extracted with ether, and the combined organic phase was washed with a saturated aqueous solution of ammonium chloride (120 ml) and then MgSO 4 dry. The desiccant was removed by filtration, the solvent was evaporated under reduced pressure, and the product was separated by chromatography (developing solvent: dichloromethane / petroleum ether = 1:3 mixed solvent) to obtain 6.66 g of the product, with a yield of 77%.

[0043] 1 Analysis of ...

Embodiment 3

[0045] Example 3 Synthesis of 1-(4-tert-butyl)-phenyl-2,3,4,5-tetramethylcyclopentadienyl ligand

[0046] Under nitrogen atmosphere, add 15.90ml of ether solution containing 2,3,4,5-tetramethylcyclopent-2-en-1-one (36mmol) into the reaction flask, and slowly Add 22.5ml, 1.6M 4-tert-butyl-phenyllithium salt (4-tbu-PhLi, 36mmol) in ether. . Under stirring conditions, gradually rise to room temperature and react for 30 hours. The reaction mixture was poured into ice water, and the pH value was adjusted to about 1 with hydrochloric acid. The aqueous layer was extracted with ether, and the combined organic phases were washed with a saturated aqueous solution of ammonium chloride (120 ml), and then MgSO 4 dry. The desiccant was removed by filtration, the solvent was evaporated under reduced pressure, and the product was separated by chromatography (developing solvent: dichloromethane / petroleum ether = 1:3 mixed solvent) to obtain 7.23 g of the product, with a yield of 79%.

[0047] 1...

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Abstract

The invention relates to a non-bridge mono / bi-nuclear metallocene compound and a relative application olefin polymerization catalyst technical field. The compound contains 1-(4-methyl)-phenyl-2, 3, 4, 5-tetramethyl cyclopentadienyl-(2, 4, 6-tertiary butyl phenoxy)-titanium chloride, and (3, 3', 5, 5'-quattuor isopropyl-4, 4'-biphenyl oxygen)-bi-[1-(4-methyl)-phenyl-2, 3, 4, 5-tetramethyl cyclopentadienyl-titanium dichloride] or the like. The metallocene compound can be used as main catalyst, while alkyl aluminum is used as promoter, or organic boron compound and alkyl aluminum are assembled into a promoter system, to catalyze and synthesize high-molecular-weight atactic polypropylene with improved catalysis activity and polymer molecular weight, which can catalyze the polymerization of vinyl and alpha-olefin, to obtain the polymer with suitable molecular weight in narrow distribution and high co-monomer content.

Description

Technical field [0001] The invention belongs to the technical field of olefin polymerization catalyst and its preparation and application. Specifically, the present invention relates to a novel non-bridged mixed-type mono / dinuclear metallocene compound, which is suitable for the catalytic synthesis of high molecular weight random polypropylene, and the copolymerization of most comonomers and ethylene. Background technique [0002] In recent years, a large number of studies have proved that in the field of olefin polymerization research and development, metallocene catalysts show advantages that traditional catalysts can’t match, mainly by changing the structure of the main catalyst, and regulating the main ligand and The substitution effect of the auxiliary ligand can achieve the excellent reaction performance of catalyzing olefin polymerization, such as the improvement of catalytic reaction activity and the improvement of polymer performance: controllable polymer molecular weigh...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F17/00C08F10/00C08F4/642
Inventor 母瀛伍乔林苏清
Owner JILIN UNIV
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