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Efficient iron series catalyst for catalyzing isoprene polymerization as well as preparation method and application thereof

A technology of isoprene and catalyst, which is applied in the direction of iron organic compounds and iron group organic compounds without C-metal bonds, etc., can solve the problems of high cost, insensitivity, and wide molecular weight distribution, and achieve low cost and high molecular weight distribution. Narrow, high molecular weight effect

Active Publication Date: 2018-09-28
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

[0011] In order to solve the problems that the catalyst used in the above problems has a wide molecular weight distribution, high cost, and a wider range of regulation of the catalyst structure, especially the ligand structure, to synthesize polymers, the present invention provides a New high-efficiency iron-based catalysts, pyridinium iron complexes as the main catalyst (imine nitrogen substituents are linked to CHR 2 or CH 2 R group, CH or CH 2 The H on has Lewis acidity), catalyzed the polymerization of isoprene under the activation of commercial cocatalyst methylaluminoxane (MAO), this type of system has extremely high activity, and obtained high molecular weight and microstructure controllable The polymer, the microstructure of the polymer can be regulated by the modification of the ligand on the main catalyst, and the selectivity of this type of system is not sensitive to the reaction temperature

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  • Efficient iron series catalyst for catalyzing isoprene polymerization as well as preparation method and application thereof
  • Efficient iron series catalyst for catalyzing isoprene polymerization as well as preparation method and application thereof
  • Efficient iron series catalyst for catalyzing isoprene polymerization as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] The present embodiment prepares the pyridine imine iron complex shown in formula (1):

[0050] The 25mL Schlenk reaction tube was pumped and baked three times, and 15mL redistilled dichloromethane, equimolar ratio of anhydrous FeCl 2 And benzyl-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 340 mg of purple solid (85% yield).

[0051] Mass Spectrometry: C 13 h 12 ClFeN 2 [M-Cl] + : Theoretical value: 287.0038; measured value: 287.0031.

[0052] Elemental Analysis: C 13 h 12 Cl 2 FeN 2 : Theoretical value: C, 48.34%; H, 3.74%; N, 8.67%; Found value: C, 48.11%; H, 3.82%; N, 8.55%.

[0053] Magnetic susceptibility: (500MHz, CD 2 Cl 2 ):μ eff =5.32μ B (8.50 mg / mL).

[0054] H NMR spectrum: 1 H NMR (500MHz, CD 2 Cl 2 ,40℃,δ):95.8(Δ ν1 / 2 =460Hz), 68.8(Δ...

Embodiment 2

[0056] The preparation process of the pyridinium iron complex shown in formula (2) prepared in this embodiment is as follows:

[0057] The 25mL Schlenk reaction tube was pumped and baked three times, and 10mL redistilled dichloromethane, anhydrous FeCl 2 And methyl phenyl substituted pyridine imine ligand, stirred at room temperature for 48h. After the reaction, dichloromethane was vacuum-dried, washed twice with 10 mL distilled n-hexane (the filtrate was colorless and clear), and vacuum-dried to constant weight to obtain 208 mg of blue-purple solid (>99% yield).

[0058] Mass Spectrometry: C 14 h 14 ClFeN 2 [M-Cl] +: Theoretical value: 301.0189; Measured value: 301.0189

[0059] Elemental Analysis: C 14 h 14 N 2 Cl 2 Theoretical Fe: C, 49.89%; H, 4.19%; N, 8.31%; Found: C, 49.70%; H, 3.96%; N, 8.21%.

[0060] Magnetic susceptibility (500MHz, CD 2 Cl 2 ):μ eff =4.98μ B (7.9mg / mL).

[0061] H NMR spectrum: 1 H NMR (500MHz, CD 2 Cl 2 ,40℃,δ):91.1(Δ ν1 / 2 =477Hz...

Embodiment 3

[0063] The pyridine imine iron complex shown in the formula (3) prepared in this embodiment, the preparation process is as follows:

[0064] The 10mL Schlenk reaction tube was pumped and baked three times, and 5mL redistilled dichloromethane, anhydrous FeCl 2 And diphenyl substituted pyridine imine ligand, 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 170 mg of red-purple solid (85% yield).

[0065] Mass Spectrometry: C 38 h 32 ClFeN 4 [M-FeCl 3 ] + : Theoretical value: 635.1659; measured value: 635.1658.

[0066] Elemental Analysis: C 38 h 32 Cl 4 Fe 2 N 4 Theoretical: C, 57.18%; H, 4.04%; N, 7.02%; Found: C, 57.26%; H, 4.10%; N, 7.01%.

[0067] Magnetic susceptibility (500MHz, CD 2 Cl 2 ):μ eff =5.32μ B (8.50mg / mL).

[0068] H NMR spectrum: 1 H NMR (500MHz, CD 2 Cl 2 ,40℃,δ):82.2(Δ ...

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Abstract

The invention discloses an efficient iron series catalyst for catalyzing isoprene polymerization as well as a preparation method and application thereof, and relates to the technical field of conjugated diene catalytic synthesis. The catalyst is prepared from iron pyridine compounds and methylaluminoxane. The preparation raw materials of the catalyst are simple and can be easily obtained; the costis low. When the catalyst is used for catalyzing isoprene polymerization, the ultrahigh activity is shown; the obtained polymers have high molecular weight; the molecular weight distribution is narrow; meanwhile, the structure of a main catalyst can be regulated and controlled by regulating ligands; the polymer structure can be further regulated in controllable way; in the same reaction, the influence of cocatalysts, the temperature and the main catalyst quantity on the reaction selectivity is not great.

Description

technical field [0001] The invention relates to the field of catalytic polymerization of conjugated diolefins, in particular to an iron-based catalyst, and also relates to its preparation method, polymerization process, isoprene polymerization to prepare polyisoprene and the application of polymer microstructure controllable polymerization. Background technique [0002] Polyisoprene is a natural unsaturated hydrocarbon polymer that can be isolated from the latex of the Hevea tree, which is the main source of natural rubber. Existing analysis studies have shown that natural rubber is a mixture of 94% rubber hydrocarbons, 2.5% acetone extract, 2.% protein, 0.5% moisture, 0.3% ash, and 0.2% magazines. The microstructure of polyisoprene includes cis-1,4 structure, trans-1,4 structure, 1,2 structure and 3,4 structure. It is well known that the diversity of microstructure determines the macroscopic physical properties of polyisoprene. For example, the performance of cis-1,4 poly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F4/70C08F2/06C08F136/08C07F15/02
CPCC07F15/025C08F136/08C08F4/7006C08F2/06
Inventor 王庆刚王晓武王亮赵梦梦咸漠张献辉
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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