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[OONN] tetradentate fourth subgroup metal complexes as well as preparation method and application thereof

A metal complex, the fourth technology, which is applied to the compounds of group 4/14 elements of the periodic table, organic compounds of group 4/14 without C-metal bonds, chemical instruments and methods, etc., can solve the problem of low catalytic activity, The preparation process is cumbersome and the cost is high

Pending Publication Date: 2021-05-11
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problems of relatively cumbersome preparation process, high cost and low catalytic activity in the existing olefin polymerization catalyst proposed in the above-mentioned background technology

Method used

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  • [OONN] tetradentate fourth subgroup metal complexes as well as preparation method and application thereof
  • [OONN] tetradentate fourth subgroup metal complexes as well as preparation method and application thereof
  • [OONN] tetradentate fourth subgroup metal complexes as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment 1: the synthesis of ligand s1

[0033] Concrete synthetic route is as follows:

[0034]

[0035] Specifically, take 1 equivalent of a1 in a 100ml round bottom flask, add 30ml of DMF (dimethylformamide), then weigh 3 equivalents of methyl iodide and 3 equivalents of K 2 CO 3 Add this to the round bottom flask, react at room temperature for 24h, extract with ether, dry over anhydrous magnesium sulfate, and spin dry to obtain light yellow solid a2.

[0036] Under an inert atmosphere, weigh 1 equivalent of a2 into a 50 mL Schlenk bottle, add 30 mL of dry diethyl ether, add 1.5 equivalents of nBuLi (n-Butyllithium, n-butyllithium) n-hexane solution with a syringe at 0°C, then slowly rise to room temperature and stir 3h, a large amount of lithium salt of the ligand is precipitated, then add 2.5 equivalents of trimethyl borate with a syringe, react at room temperature for 24h, add water to quench, extract with ether, dry over anhydrous magnesium sulfate, concen...

Embodiment 2

[0039] Embodiment 2: the synthesis of ligand s2

[0040] Concrete synthetic route is as follows:

[0041]

[0042] Under an inert atmosphere, weigh 1 equivalent of b1, add 30 mL of dry ether to a 50 mL Schlenk bottle, add 1.0 equivalent of nBuLi n-hexane solution with a syringe at -78°C, then slowly rise to room temperature and stir for 0.5 h, lithium salt with a large amount of ligands Precipitation is formed, under an inert atmosphere, 1 / 2 equivalent of TiCl 4 Add the toluene solution of the above-mentioned ligand to 50mL Schlenk, slowly add the lithium salt solution of the above ligand to the toluene solution of the metal chloride at -78°C, react at room temperature for 24h, extract with dichloromethane and water, and remove TiO 2 , spinning to dryness, adding an appropriate amount of methanol to precipitate, and performing suction filtration to obtain off-white solid s2.

Embodiment 3

[0043] Example 3: Ligand LnH 2 Synthesis

[0044] Concrete synthetic route is as follows:

[0045]

[0046] Weigh 2.2 equivalents of s1, 1 equivalent of s2 and 3 equivalents of K 3 PO 4 ·3H 2 O in a 100ml round bottom flask, add isopropanol and water (ratio is 2:1), after stirring at room temperature for 10min, add 0.5% equivalent Pd(OAC) 2 , Reflux at 100°C for 24h, extract with ethyl acetate and water, dry over anhydrous magnesium sulfate, concentrate, add an appropriate amount of methanol for recrystallization, and filter with suction to obtain a white solid s3.

[0047]

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PUM

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Abstract

The invention relates to the technical field of olefin polymerization catalysts, and particularly discloses [OONN] tetradentate fourth subgroup metal complexes, a preparation method and application. The [OONN] tetradentate fourth subgroup metal complexes have a structure which is shown in the specification. The [OONN] tetradentate fourth subgroup metal complexes provided by the invention can catalyze ethylene polymerization and ethylene and alpha-olefin copolymerization, and in the polymerization process, the heat resistance is good, and the polymerization time is long. The complexes are simple in synthesis method, easy to prepare and high in yield, the structure is convenient to modify, the complexes can be used for catalyzing ethylene polymerization and ethylene and alpha-olefin copolymerization after being activated by a proper cocatalyst, the problems that an existing olefin polymerization catalyst is relatively tedious in preparation process, high in cost and low in catalytic activity are solved, and the complexes have good industrial application value and wide application field.

Description

technical field [0001] The invention belongs to the technical field of olefin polymerization catalysts, in particular to a class of [OONN] tetradentate fourth subgroup metal complexes, a preparation method and application. Background technique [0002] Polyolefin products have excellent performance and low prices, and are widely used in various fields of the national economy and people's lives. Their production capacity and demand indicate the level of a country's petrochemical industry and people's living standards. After decades of continuous efforts, the domestic polyolefin industry has made great progress. In the preparation method of polyolefin products, the internal structure and morphology of polyolefin products are determined by olefin polymerization catalysts. Olefin polymerization catalysts include three major systems: Ziegler-Natta catalysts that have been widely used in industry, metallocene catalyst systems and non-metallocene polymerization systems. [0003] ...

Claims

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Application Information

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IPC IPC(8): C07F7/00C08F110/02C08F210/16C08F4/642
CPCC07F7/003C08F110/02C08F210/16C08F4/64189C08F210/14
Inventor 母瀛郑美玲
Owner JILIN UNIV
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