[N,N,N,N] tetradentate ligand fourth subgroup transition metal complex and preparation method and application thereof

A technology of metal complexes and tetradentate ligands, which is applied in the fields of compounds of group 4/14 elements of the periodic table, titanium organic compounds, chemical instruments and methods, etc., which can solve the problems of high cost, complex catalyst structure, and many synthesis steps, etc. problem, to achieve the effect of long life, stable structure and high catalytic activity

Inactive Publication Date: 2015-10-28
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, so far, there are few catalyst systems that can be used to produce ultra-high molecular weight polyethylene, a...

Method used

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  • [N,N,N,N] tetradentate ligand fourth subgroup transition metal complex and preparation method and application thereof
  • [N,N,N,N] tetradentate ligand fourth subgroup transition metal complex and preparation method and application thereof
  • [N,N,N,N] tetradentate ligand fourth subgroup transition metal complex and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1 Type I tetradentate ligand L 11 Preparation of H2

[0035]

[0036] Under the condition of stirring at -78°C, add 10ml of a hexane solution of n-butyllithium with a concentration of 2mol / L to 20ml of a tetrahydrofuran solution of o-phenylenediamine with a concentration of 0.5mol / L, and naturally rise to room temperature to react 2 Hours, a tetrahydrofuran solution of lithium o-phenylenediamide was obtained. The tetrahydrofuran solution of lithium o-phenylenediamide was added to 20 ml of the 1 mol / L compound A tetrahydrofuran solution, and the reaction was stirred at 50° C. for 2 hours. The temperature of the reaction solution was lowered to -78°C, and 5 ml of n-butyllithium hexane solution with a concentration of 2 mol / L was added, and the reaction solution was allowed to rise to room temperature naturally, and then stirred overnight. The solvent tetrahydrofuran was distilled off, the product was extracted with dichloromethane and water, the organic phase...

Embodiment 2

[0037] Example 2 Type I tetradentate ligand L 12 Preparation of H2

[0038]

[0039] Under the condition of stirring at -78°C, add 10ml of a hexane solution of n-butyllithium with a concentration of 2mol / L to 20ml of a tetrahydrofuran solution of o-phenylenediamine with a concentration of 0.5mol / L, and naturally rise to room temperature to react 2 Hours, a tetrahydrofuran solution of lithium o-phenylenediamide was obtained. The tetrahydrofuran solution of lithium o-phenylenediamide was added to 20 ml of the 1 mol / L compound B tetrahydrofuran solution, and the reaction was stirred at 50° C. for 2 hours. The temperature of the reaction solution was lowered to -78°C, and 5 ml of n-butyllithium hexane solution with a concentration of 2 mol / L was added, and the reaction solution was allowed to rise to room temperature naturally, and then stirred overnight. The solvent tetrahydrofuran was distilled off, the product was extracted with dichloromethane and water, the organic phase...

Embodiment 3

[0040] Example 3 Type II tetradentate ligand L 21 Preparation of H2.

[0041]

[0042] Under the condition of stirring at room temperature, o-phenylenediamine (0.54g, 5.0mmol), compound C (2.25g, 10.0mmol) and p-toluenesulfonic acid (0.10g) were mixed in 20ml of toluene, and the water separator was used to reflux for 10 After 1 hour, the reaction solution was cooled to room temperature, the solvent toluene was distilled off, and column chromatography was carried out using petroleum ether / ethyl acetate for separation or recrystallization in petroleum ether / ethyl acetate solvent to obtain 2.11 g of a light yellow solid pure product with a yield of 81%. , denoted as tetradentate ligand L 21 H2.

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Abstract

The invention belongs to the technical field of olefin polymerization catalysts, and discloses an [N,N,N,N] tetradentate ligand fourth subgroup transition metal complex and a preparation method and application thereof. The [N,N,N,N] tetradentate ligand fourth subgroup transition metal complex has the general structural formula I or II shown in the specifications. According to the preparation method, a toluene solution of a Ti or Zr or Hf halide and a toluene solution of a tetradentate ligand I are mixed and react for 1-12 hours, and solvent toluene is distilled off; the mixture continues reacting for 1-3 hours, and then a crude complex can be obtained; furthermore, recrystallization is conducted in organic solvent so as to obtain the complex with the general structural formula I. Serving as a main catalyst, the complex can be applied to catalytic ethylene polymerization. The complex is stable in structure, good in heat resistance, long in service life and high in catalytic activity; polyethylene obtained in catalytic ethylene polymerization has an ultra-high molecular weight.

Description

technical field [0001] The invention belongs to the technical field of olefin polymerization catalysts, and particularly relates to a [N, N, N, N] tetradentate ligand fourth subgroup transition metal complex, a preparation method and its application in catalyzing ethylene polymerization. Background technique [0002] Polyethylene is an important synthetic resin with a wide range of uses. In the past few decades, polyolefin products have been widely used in textiles, building materials, packaging, medical equipment, It has a wide range of applications in coatings, electrical appliances, automobiles, aviation and agricultural production. The impact resistance and impact absorption of ultra-high molecular weight polyethylene rank first among plastics, and it is difficult to crack it no matter it is a strong external impact or internal pressure fluctuations. Excellent physical and mechanical properties make it widely used in military industry, machinery, transportation, chemic...

Claims

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Application Information

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IPC IPC(8): C07F7/28C07F7/00C08F110/02C08F4/642
Inventor 母瀛籍向东
Owner JILIN UNIV
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