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

A metallocene compound and bridging technology, which is applied in the field of olefin polymerization catalysts and its preparation and application, can solve the problems of unfavorable catalyst stability and reduced catalytic activity, and achieve the effect of improving the application range and added value

Inactive Publication Date: 2008-06-11
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 synthetic reaction equation 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 bottle, slowly add 18ml dropwise under ice-salt condition, 2.0 M 4-Methyl-phenyl lithium salt (4-Me-PhLi, 36 mmol) in ether. Under stirring conditions, it was gradually raised to room temperature and reacted for about 30 hours. The reaction mixture was poured into cold water, and the pH value 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 washed with MgSO 4 dry. The desiccant was removed by filtration, the solvent was evaporated under reduced pressure, and column chromatography (developing solvent: dichloromethane / petroleum ether...

Embodiment 2

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

[0042] Under a nitrogen atmosphere, add 15.90ml of ether solution containing 2,3,4,5-tetramethylcyclopent-2-en-1-one (36mmol) to the reaction flask, and slowly Add 20ml of a 1.8M ether solution of 4-isopropyl-phenyllithium salt (4-ipr-PhLi, 36mmol). . Under the condition of stirring, it was gradually raised to room temperature and reacted 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 (120ml), washed with MgSO 4 dry. The desiccant was removed by filtration, the solvent was evaporated under reduced pressure, and the product was separated by column chromatography (developing solvent: dichloromethane / petroleum ether=1:3 mixed solvent) to obtain 6.66 g of the pr...

Embodiment 3

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

[0046] Under a nitrogen atmosphere, add 15.90ml of ether solution containing 2,3,4,5-tetramethylcyclopent-2-en-1-one (36mmol) to the reaction flask, and slowly Add 22.5 mL of a 1.6M ether solution of 4-tert-butyl-phenyllithium salt (4-tbu-PhLi, 36 mmol). . Under the condition of stirring, it was gradually raised to room temperature and reacted 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 (120ml), washed with MgSO 4 dry. The desiccant was removed by filtration, the solvent was evaporated under reduced pressure, and the product was separated by column chromatography (developing solvent: dichloromethane / petroleum ether=1:3 mixed solvent) to obtain 7.23 g of ...

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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 invention relates to a novel non-bridging mixed-type mono / dinonuclear metallocene compound, which is suitable for catalyzing the 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 research and development of olefin polymerization, metallocene catalysts have shown incomparable advantages over traditional catalysts, mainly manifested in changing the structure of the main catalyst, and adjusting the main ligand and The substitution effect of the auxiliary ligand can achieve the excellent reaction performance of catalytic olefin polymerization, such as the improvement of catalytic reactivity, the improvement of polymer performance: controllable molecular wei...

Claims

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Application Information

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IPC IPC(8): C07F17/00C08F4/642C08F10/00
Inventor 母瀛伍乔林苏清
Owner JILIN UNIV
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