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Semi-sandwich alum-chromium olefin polymerizing catalyst, preparation and uses thereof

A polymerization catalyst, core chromocene olefin technology, applied in the field of semi-sandwich chromocene olefin polymerization catalyst and its preparation, can solve the problems of high production cost and easy poisoning, and achieve the effect of high catalytic activity

Inactive Publication Date: 2009-04-08
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although metallocene catalysts are highly active, they require a large amount of expensive co-catalyst MAO, which is expensive to produce and easily poisoned, which limits their application.

Method used

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  • Semi-sandwich alum-chromium olefin polymerizing catalyst, preparation and uses thereof
  • Semi-sandwich alum-chromium olefin polymerizing catalyst, preparation and uses thereof
  • Semi-sandwich alum-chromium olefin polymerizing catalyst, preparation and uses thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1: the preparation of semi-sandwich chromocene olefin polymerization catalyst 1a:

[0019] Under the protection of anhydrous, oxygen-free and nitrogen, add 0.10 mmol of n-butyllithium to the tetrahydrofuran or toluene solution containing 0.10 mmol of β-monoketimine ligand L1 at -78 ° C, and gradually raise to room temperature , and stirred for 6 hours. At -78°C, the obtained lithium salt was transferred to 0.10 mmol of dichlorocyclopentadiene chromium tetrahydrofuran tetrahydrofuran solution (the ratio of the amount of the two substances was 1:1), and after stirring at room temperature for 12 hours, the Dry solvent, add 10ml of dichloromethane, centrifugal filter to remove inorganic salts, concentrate the filtrate to 3ml, add 10ml of n-hexane, freeze at low temperature, precipitate crystals, filter, wash with n-hexane, and vacuum dry to obtain the corresponding blue-green semi-sandwich chromocene olefin Polymerization Catalyst 1a. Yield 48%.

[0020] Eleme...

Embodiment 2

[0021] Embodiment 2: the preparation of semi-sandwich chromocene olefin polymerization catalyst 1b:

[0022] Under the protection of anhydrous, oxygen-free and nitrogen, add 0.34mmol of n-butyllithium to the tetrahydrofuran or toluene solution containing 0.34mmol of β-monoketimine ligand L2 at -78°C, and gradually raise to room temperature , and stirred for 6 hours. At -78°C, the obtained lithium salt was transferred to a tetrahydrofuran solution of 0.34 mmol dichlorocyclopentadiene chromium tetrahydrofuran (the ratio of the amount of the two substances was 1:1), and after stirring at room temperature for 12 hours, Drain the solvent, add 15ml of dichloromethane, remove inorganic salts by centrifugal filtration, concentrate the filtrate to 5ml, add 20ml of n-hexane, freeze at low temperature, precipitate crystals, filter, wash with n-hexane, and dry in vacuum to obtain the corresponding blue-green semi-sandwich chromocene Olefin Polymerization Catalyst 1b. Yield 46%.

[0023...

Embodiment 3

[0024] Embodiment 3: the preparation of semi-sandwich chromocene olefin polymerization catalyst 1c:

[0025] Under the protection of anhydrous, oxygen-free and nitrogen, add 10mmol of n-butyllithium to the tetrahydrofuran or toluene solution containing 10mmol of β-monoketimine ligand L3 at -78°C, gradually rise to room temperature, and stir 6 hours. At -78°C, the obtained lithium salt was transferred to a tetrahydrofuran solution of 10 mmol of dichlorocyclopentadiene chromium tetrahydrofuran (the ratio of the amount of the two substances was 1:1), and after stirring at room temperature for 12 hours, the Dry solvent, add 20ml of dichloromethane, centrifugal filter to remove inorganic salts, concentrate the filtrate to 5ml, add 25ml of n-hexane, freeze at low temperature, precipitate crystals, filter, wash with n-hexane, and dry in vacuum to obtain the corresponding blue-green semi-sandwiched chromocene olefin Polymerization Catalyst 1c. Yield 51%.

[0026] Elemental Analysis...

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Abstract

The invention pertains to the technical field of an olefin polymerization catalyst, in particular to a half-sandwich cyclopentadienyl chromium olefin polymerization catalyst and a preparation method and an application thereof. The expression formula of the catalyst is CpCrLCl, L represents Beta-mono ketimine or Beta-bi-imine ligand; and a cocatalyst is aluminium ethide and assists in being used for vinyl polymerization reaction. The type of the catalyst has excellent capacity of catalyzing vinyl polymerization and polyethylene obtained has rather high molecular weight (10<5> to 10<6>).

Description

technical field [0001] The invention belongs to the technical field of olefin polymerization catalysts, in particular to a semi-sandwich chromocene olefin polymerization catalyst formed by reacting β-monoketimine and β-bis-imine ligands with cyclopentadiene chromium dichloride and a preparation method thereof and apply. Background technique [0002] As the pillar industry of modern polymer materials, the development of polyolefin industry is an important symbol to measure the development of a country's petrochemical industry. Polyolefin products have greatly promoted the development of human civilization, and olefin polymerization catalysts are the key to the development of polyolefin industry. core. Since the advent of olefin polymerization catalysts in 1953, there have been three important milestones in the Ziegler-Natta catalytic system, metallocene catalytic system and late transition metal catalytic system in just over fifty years. Although metallocene catalysts are h...

Claims

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Application Information

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IPC IPC(8): C08F4/69C08F10/00C08F110/02
Inventor 金国新黄远标
Owner FUDAN UNIV
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