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Alkyl pyridine imine iron-based catalyst and preparation method and application thereof

A kind of alkyl pyridine imide iron series, pyridine imide iron technology, applied in the application of isoprene polymerization, catalyst preparation, alkyl pyridine imide iron series catalyst field, can solve the problem of low activity, molecular weight distribution Wide, unclear active center and other problems, to achieve the effect of small temperature dependence, good industrial value, and low cost

Active Publication Date: 2018-09-14
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

[0009] In order to solve the problems that the catalyst used in the above problems has catalyst structure or unclear active center, low activity, wide molecular weight distribution and structure-activity relationship between catalyst ligand structure and polymer selectivity, the present invention provides a novel alkanes Pyridinimine iron-based catalyst, the system is mainly composed of the main catalyst and co-catalyst: pyridinimine iron complex as the main catalyst, methyl aluminoxane or alkylaluminum as the co-catalyst

Method used

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  • Alkyl pyridine imine iron-based catalyst and preparation method and application thereof
  • Alkyl pyridine imine iron-based catalyst and preparation method and application thereof
  • Alkyl pyridine imine iron-based catalyst and preparation method and application thereof

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Experimental program
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Effect test

Embodiment 1

[0044]The present embodiment prepares the pyridine imine iron complex shown in formula (1):

[0045] The 25mL Schlenk reaction tube was pumped and baked three times, and 15mL redistilled dichloromethane, equimolar ratio of anhydrous FeCl 2 And isopropyl substituted pyridinimine ligand, stirred at room temperature for 24h. After the reaction, dichloromethane was vacuum-dried, washed twice with 10 mL redistilled n-hexane (the filtrate was colorless and clear), and vacuum-dried to constant weight to obtain a red solid.

[0046]

[0047] Mass Spectrometry: C 9 h 12 ClFeN 2 [M-Cl] + : Theoretical value: 239.0033; measured value: 239.0033.

[0048] Elemental Analysis: C 9 h 12 Cl 2 FeN 2 : Theoretical value: C, 39.32%; H, 4.40%; N, 10.19%; Measured value: C, 39.39%; H, 4.45%; N, 10.17%.

[0049] Magnetic susceptibility: (500MHz, CD 2 Cl 2 ):μ eff =4.92μ B (5.0 mg / mL).

[0050] H NMR spectrum: 1 H NMR (500MHz, CD 2 Cl 2 ,25℃,δ):88.2(Δ ν1 / 2 =356Hz), 66.8(Δ ν1 / 2 ...

Embodiment 2

[0052] The preparation process of the pyridinium iron complex shown in formula (2) prepared in this embodiment is as follows:

[0053] The 25mL Schlenk reaction tube was pumped and baked three times, and 15mL redistilled dichloromethane, equimolar ratio of anhydrous FeCl 2 And tert-butyl substituted pyridine imine ligand, stirred at room temperature for 24h. After the reaction, dichloromethane was vacuum-dried, washed twice with 10 mL redistilled n-hexane (the filtrate was colorless and clear), and vacuum-dried to constant weight to obtain a dark red solid.

[0054]

[0055] Mass Spectrometry: C 10 h 14 ClFeN 2 [M-Cl] + : Theoretical value: 253.0189; measured value: 253.0188.

[0056] Elemental Analysis: C 10 h 14 Cl 2 FeN 2 : Theoretical value: C, 41.56%; H, 4.88%; N, 9.69%; Measured value: C, 41.48%; H, 4.84%; N, 9.72%.

[0057] Magnetic susceptibility: (500MHz, CD 2 Cl 2 ):μ eff =5.21μ B (2.5 mg / mL).

[0058] H NMR spectrum: 1 H NMR (500MHz, CD 2 Cl 2 ,...

Embodiment 3

[0060] The pyridine imine iron complex shown in the formula (3) prepared in this embodiment, the preparation process is as follows:

[0061] The 10mL Schlenk reaction tube was pumped and baked three times, and 5mL redistilled dichloromethane, equimolar ratio of anhydrous FeCl2 and cyclohexyl-substituted pyridinimine ligand were sequentially added into the glove box, and stirred at room temperature for 48h. After the reaction, dichloromethane was vacuum-dried, washed twice with 10 mL redistilled n-hexane (the filtrate was colorless and clear), and vacuum-dried to constant weight to obtain a reddish-purple solid.

[0062]

[0063] Mass Spectrometry: C 12 h 16 ClFeN 2 [M-Cl] + : Theoretical value: 279.0346; Measured value: 279.0347.

[0064] Elemental Analysis: C 12 h 16 Cl 2 FeN 2 : Theoretical value: C, 45.75%; H, 5.12%; N, 8.89%; Measured value: C, 45.84%; H, 5.16%; N, 8.83%.

[0065] Magnetic susceptibility: (500MHz, CD 2 Cl 2 ):μ eff =5.08μ B (2.5 mg / mL).

...

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Abstract

The invention discloses an alkyl pyridine imine iron-based catalyst and a preparation method and application thereof and relates to the technical field of conjugated diene catalytic polymerization. The iron-based catalyst is composed of a main catalyst and an auxiliary catalyst, the main catalyst is a pyridine imine iron complex, the auxiliary catalyst is methylaluminoxane or alkyl aluminum, and amolar ratio of the auxiliary catalyst to the main catalyst is 20:1-1000:1. An iron catalysis system presents ultrahigh activity in isoprene polymerization, obtained polymer is high in molecular weight and narrow in molecular weight distribution, microstructure of the polymer can be controlled by adjusting structure of the main catalyst, and reaction activity depends on the main catalyst with different substituent groups and the auxiliary catalyst of different types; selectivity of the microstructure of the polymer slightly depends on temperature.

Description

technical field [0001] The invention relates to the field of catalytic polymerization of conjugated dienes, in particular to an alkylpyridineimine iron-based catalyst, and also to a preparation method of the catalyst and its application in isoprene polymerization. Background technique [0002] At present, the catalytic systems for the industrial synthesis of isoprene rubber mainly include rare earth systems, titanium systems and lithium systems. Rare earth-based polyisoprene catalysts have high activity and good selectivity, but high cost; titanium-based polyisoprene rubber has high molecular weight and high cis-structure content, but has defects such as wide molecular weight distribution and easy residue; lithium The polyisoprene rubber prepared by the catalytic system has high relative molecular weight and narrow molecular weight distribution, but poor stereoselectivity. Therefore, in view of the problems existing in the catalytic system of the controllable polymerization...

Claims

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Application Information

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IPC IPC(8): C08F136/08C08F4/80
CPCC08F4/80C08F136/08
Inventor 王庆刚王亮王晓武赵梦梦咸漠张献辉
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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