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Alkyl-substituted pyridinamine iron-based catalyst and preparation method and application thereof

A pyridine amine iron series and pyridine amine iron technology are applied in the pyridine amine iron series catalyst, the application in the polymerization of isoprene, and the field of catalyst preparation, which can solve the problem of unclear catalyst structure active center, low molecular weight of synthetic polymer, Problems such as poor selectivity, to achieve the effect of small temperature dependence, good industrialization value, and low cost

Active Publication Date: 2018-12-21
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

At present, the nitrogen-containing ligands for the polymerization of isoprene catalyzed by iron catalysts are mainly sp 2 –N,sp 2 -N pyridine imines, but the system has catalyst structures or unclear active centers, low activity, poor selectivity, and low molecular weight of synthetic polymers

Method used

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  • Alkyl-substituted pyridinamine iron-based catalyst and preparation method and application thereof
  • Alkyl-substituted pyridinamine iron-based catalyst and preparation method and application thereof
  • Alkyl-substituted pyridinamine iron-based catalyst and preparation method and application thereof

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Embodiment 1

[0033] This embodiment prepares pyridine amine iron complex A:

[0034] The 25mL Schlenk reaction tube was pumped and baked three times, and 15mL redistilled dichloromethane, equimolar ratio of anhydrous FeCl 2 And benzyl-substituted pyridinium amine ligand (1.5mmol) (structural formula LA), stirred at room temperature for 48h. After the reaction, filter under an argon atmosphere, collect the filter residue, vacuum-dry dichloromethane, add 10 mL of distilled n-hexane to wash twice (the filtrate is colorless and clear), and vacuum-dry to constant weight to obtain a white solid, structural formula:

[0035]

[0036] Mass Spectrometry: C 13 h 14 Cl 2 FeN 2 :[M-Cl] + : Theoretical value: 289.0189; measured value: 289.0191.

[0037] Elemental Analysis: C 13 h 14 Cl 2 FeN 2 : Theoretical value: C, 48.04; H, 4.34; N, 8.62; Measured value: C, 48.10%; H, 4.30%; N, 8.58%.

Embodiment 2

[0039] This embodiment prepares pyridine amine iron complex B:

[0040] The 25mL Schlenk reaction tube was pumped and baked three times, and 15mL redistilled dichloromethane, equimolar ratio of anhydrous FeCl 2and methoxy-substituted benzylpyridinium ligand (1.5mmol) (structural formula LB), stirred at room temperature for 48h. After the reaction was completed, filter under an argon atmosphere, collect the filter residue, vacuum-dry dichloromethane, add 10 mL of distilled n-hexane to wash twice (the filtrate is colorless and clear), and vacuum-dry to constant weight to obtain a light yellow solid, structural formula :

[0041]

[0042] Mass Spectrometry: C 14 h 16 Cl 2 FeN 2 o : [M-Cl] + : Theoretical value: 319.0295; measured value: 319.0290.

[0043] Elemental Analysis: C 13 h 14 Cl 2 FeN 2 : Theoretical value: C, 47.36; H, 4.54; N, 7.89; Measured value: C, 47.41%; H, 4.55%; N, 7.93%.

Embodiment 3

[0045] This embodiment prepares pyridine amine iron complex C:

[0046] The 25mL Schlenk reaction tube was pumped and baked three times, and 15mL redistilled dichloromethane, equimolar ratio of anhydrous FeCl 2 And trifluoromethyl-substituted benzylpyridinium ligand (1.5mmol) (structural formula LC), stirred at room temperature for 48h. After the reaction was completed, filter under an argon atmosphere, collect the filter residue, vacuum-dry dichloromethane, add 10 mL of distilled n-hexane to wash twice (the filtrate is colorless and clear), and vacuum-dry to constant weight to obtain a light yellow solid, structural formula :

[0047]

[0048] Mass Spectrometry: C 14 h 13 Cl 2 f 3 FeN 2 :[M-Cl] + : Theoretical value: 357.0063; measured value: 357.0065.

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Abstract

The invention discloses an alkyl-substituted pyridinamine iron-based catalyst and a preparation method and application thereof, and relates to the technical field of catalytic polymerization of conjugated diene. The alkyl-substituted pyridinamine iron-based catalyst consists of a main catalyst and an auxiliary catalyst, wherein the main catalyst is an alkyl-substituted pyridinamine iron-based complex, the auxiliary catalyst is methylaluminoxane or aluminum alkyl, and the molar ratio of the main catalyst to the auxiliary catalyst is 50:1 to 2000:1. The alkyl-substituted pyridinamine iron-basedcatalyst has superhigh activity in the polymerization of isoprene, so that the obtained polymer has high molecular weight and narrower molecular weight distribution; the micro-structure of the polymercan be regulated and controlled by adjusting the structure of the main catalyst; the reaction activity is determined by the main catalysts of different substitution groups and the auxiliary catalystsof different types.

Description

technical field [0001] The invention relates to the field of catalytic polymerization of conjugated dienes, in particular to a pyridine amine iron-based catalyst, and also relates to a preparation method of the catalyst and its application in isoprene polymerization. Background technique [0002] The rubber industry is one of the important basic industries of the national economy. It not only provides people with daily and medical light industrial rubber products that are indispensable in daily life, but also is an important raw material in the fields of transportation, aviation, machinery and national defense, which is related to the national economy and people's livelihood. At present, my country has become the world's largest consumer of natural rubber (>5 million tons / year), but domestic natural rubber resources are relatively scarce, the self-sufficiency rate is seriously insufficient (<20%), and there is a large dependence on foreign countries. There are serious ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F36/08C08F4/70
CPCC08F36/08C08F4/7006
Inventor 王庆刚王亮荆楚杨王晓武赵梦梦咸漠
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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