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Pyridinimine cobalt complex containing diphenylmethoxy group and its preparation method and application

A technology of diphenylmethoxyl and cobalt pyridinium, applied in the field of cobalt pyridinium complexes and their preparation

Active Publication Date: 2021-07-27
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

As a new catalyst system, there are still some difficulties in basic research and constraints to promote industrialization

Method used

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  • Pyridinimine cobalt complex containing diphenylmethoxy group and its preparation method and application
  • Pyridinimine cobalt complex containing diphenylmethoxy group and its preparation method and application
  • Pyridinimine cobalt complex containing diphenylmethoxy group and its preparation method and application

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Experimental program
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Effect test

Embodiment 1

[0019] (1) Preparation of ligand

[0020] A catalytic amount of p-toluenesulfonic acid was added in batches to 2,6-diacetylpyridine (23.0 mmol) and 2,6-bis(4,4′-dimethoxybenzhydryl)-6 - Methylaniline (20.0mmol) in toluene mixture, heated to 120°C, continued to reflux for 9 hours, concentrated the solution, using petroleum ether / ethyl acetate (v / v=20:1) as eluent, column The reaction product was purified by chromatography to obtain the intermediate product M.

[0021] Add the intermediate product M (2mmol) in batches to the toluene solution of 2,4,6-trimethylaniline (2.5mmol), add an appropriate amount of p-toluenesulfonic acid in batches under stirring, heat to 120°C, and reflux After 15 hours, after the reaction was complete, concentrate, use petroleum ether / ethyl acetate (v / v=100:3) as the eluent, purify by column chromatography, wash, suction filter, and crystallize to obtain diphenylmethoxyl-containing Pyridine imine ligand compound L1;

[0022] L2(R 1 =Et,R 2 =H), L3...

Embodiment 2

[0038] Polymerization of ethylene under pressure using complex C1 and MAO cocatalyst:

[0039] Under an ethylene environment, 25 mL of toluene, 25 mL of toluene solution of catalyst C1 (1.5 μmol), 2.6 mL of cocatalyst MAO (1.46 mol / L toluene solution), and 50 mL of toluene were sequentially added to a 250 mL stainless steel autoclave. At this time, Al / Co=2500:1. Start the mechanical stirring and keep it at 400 rpm. When the polymerization temperature reaches 60°C, fill the reactor with ethylene, and the polymerization reaction starts. Maintain an ethylene pressure of 10 atm at 60°C and stir for 30 min. The reaction was quenched with 5% hydrochloric acid and ethanol solution to obtain a polymer precipitate, which was washed several times with ethanol, dried in vacuum until constant weight, and weighed.

[0040] Polymerization activity: 8.71×10 6 g·mol -1 (Co)·h -1 , Polymer T m = 117.1°C. (T m For the melting temperature of polymer, obtained by DSC test), polymer molecu...

Embodiment 3

[0042] Polymerization of ethylene under pressure using complex C2 and MAO cocatalyst:

[0043] Under an ethylene environment, 25 mL of toluene, 25 mL of toluene solution of catalyst C1 (1.5 μmol), 2.6 mL of cocatalyst MAO (1.46 mol / L toluene solution), and 50 mL of toluene were sequentially added to a 250 mL stainless steel autoclave. At this time, Al / Co=2500:1. Start the mechanical stirring and keep it at 400 rpm. When the polymerization temperature reaches 60°C, fill the reactor with ethylene, and the polymerization reaction starts. Maintain an ethylene pressure of 10 atm at 60°C and stir for 30 min. The reaction was quenched with 5% hydrochloric acid and ethanol solution to obtain a polymer precipitate, which was washed several times with ethanol, dried in vacuum until constant weight, and weighed. Polymerization activity: 6.37×10 6 g·mol -1 (Co)·h -1 , Polymer T m =117.5°C, M w =3.38×10 5 g·mol -1 , PDI=1.6.

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Abstract

The invention provides a diphenylmethoxy-containing pyridineimine cobalt complex, a preparation method and application thereof. The crystal structure of the cobalt complex shows a tetrahedral geometric structure in which the main part and the metal center are twisted. The preparation of the cobalt complex of the present invention starts from simple and inexpensive raw materials, and each step is easy to implement and the yield is high. Activated with MAO, the cobalt complexes showed high activity for ethylene polymerization, up to 8.71 × 10 6 g PE(mol of Ni) ‑1 h ‑1 , and produce polyethylene with high molecular weight, high melting point and narrow molecular weight distribution. In addition, according to the analysis of the microstructure of the polymer product by high temperature nuclear magnetic spectrum, it is found that the change of the substituents on the ligand has a great influence on the catalytic performance of the cobalt complex and the microstructure of polyethylene. The cobalt complex can be used as a catalyst in ethylene polymerization.

Description

technical field [0001] The invention relates to late transition metal complexes, in particular to cobalt complexes, more specifically to a pyridinimine cobalt complex containing benzhydryloxy group and its preparation method and application. Background technique [0002] Transition metal complexes as catalysts for olefin polymerization have always been a hot spot in applied research. At present, industrialized polyethylene catalysts include Ziegler-Natta type catalysts, Phillips type catalysts and metallocene type catalysts. High-efficiency catalysts for ethylene oligomerization and polymerization of late-transition metal complexes are not only easy to prepare, have high catalytic activity, and can control the molecular weight and distribution of polymers, so they have quickly become a hot spot in applied research. In 1998, a class of iron and cobalt complexes of iminopyridines was independently reported by Brookhart and Gibbson. These complexes have high activity in cataly...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F15/06C08F110/02C08F4/70
CPCC07F15/065C08F110/02C08F4/7042
Inventor 袁世芳闫艺孙文华
Owner SHANXI UNIV
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