Pyridine tertiary amine iron complex and preparation method thereof, and method for catalyzing polymerization of conjugated diene by using pyridine tertiary amine iron complex

A technology of pyridine tertiary amine iron and conjugated diene, which is applied in the direction of iron-organic compounds, can solve the problems of lower catalyst activity and selectivity, poor heat resistance of iron-based catalysts, and change, and achieve low cost and high molecular weight , Preparation is simple and easy to obtain

Active Publication Date: 2020-06-19
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention aims to solve the problem that the structure of the existing pyridyl imine or pyridyl amine iron catalyst is easily changed by the influence of the co-catalyst, thereby reducing the catalyst activity and selectivity and the existing To solve the technical problem of poor heat resistance of iron-based catalysts, a pyridine tertiary amine iron complex and its preparation method and a method for using it to catalyze the polymerization of conjugated dienes are provided

Method used

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  • Pyridine tertiary amine iron complex and preparation method thereof, and method for catalyzing polymerization of conjugated diene by using pyridine tertiary amine iron complex
  • Pyridine tertiary amine iron complex and preparation method thereof, and method for catalyzing polymerization of conjugated diene by using pyridine tertiary amine iron complex
  • Pyridine tertiary amine iron complex and preparation method thereof, and method for catalyzing polymerization of conjugated diene by using pyridine tertiary amine iron complex

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specific Embodiment approach 1

[0051] Specific embodiment one: the structural formula of a kind of pyridine tertiary amine iron complex of the present embodiment is:

[0052]

[0053] Its preparation method is as follows: under argon atmosphere, 25mL Schlenk tube was pumped and baked three times, and then 10mL redistilled dichloromethane, 1.0mmol anhydrous FeCl 2and 1.0 mmol of pyridine tertiary amine ligand L1, stirred at room temperature for 24 hours, after the reaction was completed, filtered under an argon atmosphere, vacuum-dried dichloromethane, and then washed twice with 10 mL redistilled n-hexane until the filtrate was clear, and then vacuum-pumped Dry to constant weight to obtain a yellow solid, that is, pyridine tertiary amine iron complex (referred to as catalyst 1) (217.2 mg, yield: 83%).

[0054] Mass Spectrometry: C 16 h 24 Cl 4 Fe 2 N 4: [M-FeCl 2 +H] + : Theoretical value: 399.0806; measured value: 399.0807.

[0055] Elemental Analysis: C 16 h 24 Cl 4 Fe 2 N 4 : Theoretical v...

specific Embodiment approach 2

[0056] Specific embodiment two: the structural formula of a kind of pyridine tertiary amine iron complex of the present embodiment is:

[0057]

[0058] Its preparation method is as follows: under an argon atmosphere, a 25mL Schlenk tube was pumped and baked three times, and then 10mL redistilled dichloromethane, 1.0mmol anhydrous FeCl 2 and 1.0 mmol pyridine tertiary amine ligand L2, stirred at room temperature for 24 hours, after the reaction was completed, filtered under argon atmosphere, vacuum-dried dichloromethane, and then washed twice with 10 mL redistilled n-hexane until the filtrate was clear, and then vacuum-pumped Dry to constant weight to obtain a yellow solid, that is, pyridine tertiary amine iron complex (referred to as catalyst 2) (237.8 mg, yield: 82%).

[0059] Mass Spectrometry: C 20 h 32 Cl 4 Fe 2 N 4: [M-FeCl 3 ] + : Theoretical value: 419.1665; measured value: 419.1663.

[0060] Elemental Analysis: C 20 h 32 Cl 4 Fe 2 N 4 : Theoretical val...

specific Embodiment approach 3

[0061] Specific embodiment three: the structural formula of a kind of pyridine tertiary amine iron complex of the present embodiment is:

[0062]

[0063] Its preparation method is as follows: under an argon atmosphere, a 25mL Schlenk tube was pumped and baked three times, and then 10mL redistilled dichloromethane, 1.0mmol anhydrous FeCl 2 and 1.0 mmol of pyridine tertiary amine ligand L3, stirred at room temperature for 24 hours, after the reaction was completed, filtered under an argon atmosphere, vacuum-dried dichloromethane, and then washed twice with 10 mL redistilled n-hexane until the filtrate was clear, and then vacuum-pumped Dry to constant weight to obtain a yellow solid, ie pyridine tertiary amine iron complex (referred to as Catalyst 3) (272.2 mg, yield: 81%).

[0064] Mass Spectrometry: C 28 h 32 Cl 4 Fe 2 N 4: [M-FeCl 3 ] + : Theoretical value: 515.1665; measured value: 515.1666.

[0065] Elemental Analysis: C 28 h 32 Cl 4 Fe 2 N 4 : Theoretical v...

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Abstract

The invention relates to a pyridine tertiary amine iron complex and a preparation method thereof, and a method for catalyzing polymerization of conjugated diene by using the pyridine tertiary amine iron complex, belonging to the field of catalytic polymerization of conjugated diene. The invention aims to solve the technical problem that the activity and selectivity of the catalyst are reduced since the structures of existing pyridine imine or pyridine amine iron catalysts are easily changed under the influence of cocatalysts and the technical problem that the heat resistance of conventional iron-based catalysts. The pyridine tertiary amine iron complex disclosed by the invention is obtained by mixing and reacting a pyridine tertiary amine ligand and anhydrous FeCl2. An iron catalytic system of the invention is a pyridine tertiary amine iron complex with a clear molecular structure; and the complex is simple in preparation, easy to obtain, low in cost, mainly used for catalyzing polymerization of conjugated olefin, and free of the possibility that a ligand skeleton reacts with a cocatalyst compared with conventional pyridine tertiary amine iron catalysts.

Description

technical field [0001] The invention belongs to the field of catalytic polymerization of conjugated diene, and in particular relates to a pyridine tertiary amine iron complex, a preparation method thereof and a method for catalyzing the polymerization of conjugated diene. Background technique [0002] In recent years, environmentally friendly late-transition metal-catalyzed olefin polymerization has attracted increasing attention from scientists. Iron-based catalysts have also received extensive attention in the polymerization of conjugated olefins due to their environmental friendliness, economy, biocompatibility, and good tolerance to polar monomers. [0003] At present, the nitrogen-containing ligands catalyzed by iron catalysts for the polymerization of conjugated olefins are mainly pyridine imines or pyridine amines, but the skeletons of these two systems are prone to addition reactions or hydrogen extraction reactions under the influence of co-catalysts, thereby changi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/03C08F136/06C08F136/08C08F236/06C08F236/08C08F4/70
CPCC07F15/03C08F136/06C08F136/08C08F236/06C08F236/08C08F4/7006
Inventor 王庆刚王亮荆楚杨朱广乾张献辉
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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