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A kind of iron-based catalyst and its preparation method and application in isoprene polymerization

A technology for isoprene and polyisoprene, which is applied in the field of preparation of iron-based catalysts, can solve the problems of high cost, catalyst microstructure control, wide molecular weight distribution, etc., and achieves low cost, narrow molecular weight distribution, and high molecular weight. Effect

Active Publication Date: 2018-10-26
QUFU NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the problems of wide molecular weight distribution, high cost, and inability to adjust the microstructure of the catalyst in the catalyst used in the polymerization of isoprene in the prior art to make the polymer performance diverse Problem, this application provides a new iron-based catalyst, the pyridinium iron complex is used as the main catalyst, and under the activation of the industrialized co-catalyst methylaluminoxane (MAO), it catalyzes the polymerization of isoprene, showing Higher catalytic activity was obtained, and polymers with high molecular weight and adjustable microstructure were obtained. The microstructure of the polymer can be regulated by tailoring the structure of the main catalyst, and it is not sensitive to the reaction temperature.

Method used

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  • A kind of iron-based catalyst and its preparation method and application in isoprene polymerization
  • A kind of iron-based catalyst and its preparation method and application in isoprene polymerization
  • A kind of iron-based catalyst and its preparation method and application in isoprene polymerization

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Experimental program
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Effect test

Embodiment 1

[0036] The present embodiment prepares the pyridine imine iron complex shown in formula (I):

[0037] Under nitrogen atmosphere, add equimolar ratio of adamantyl-substituted pyridinimine ligand and anhydrous FeCl2 into a dry Schlenk tube, then add 10ml CH2Cl2 and stir at room temperature (about 20°C, the same below) for 24 After 1 hour, the product was filtered and washed with 10 ml of n-hexane, washed three times, and vacuum-dried to constant weight to obtain 0.35 g of an orange solid, which is the target product of this example, with a yield of 95%.

[0038] Mass spectrometry: theoretical value: C16H20ClFeN2: 331.0664, measured value: 330.9991[M-Cl]+( figure 1 ).

[0039] Elemental analysis results: theoretical value: C16H20Cl2FeN2: C, 52.35%; H, 5.49%; N, 7.63%; measured value: C, 52.58%; H, 5.34%; N, 7.38%.

[0040] Infrared analysis: IR(KBr) / cm-1:1588, ν(C=N).

Embodiment 2

[0042] The pyridine imine iron complex shown in the formula (II) prepared in this example, wherein R1'=H, R2'=H, the preparation process is as follows: under nitrogen atmosphere, add in a dry Schlenk tube Equimolar ratio of trityl substituted pyridine imine ligand and anhydrous FeCl2, then add 10ml CH2Cl2 and stir at room temperature for 24 hours, the product is filtered and washed with 10ml n-hexane, washed three times, vacuum dried to constant weight, and light pink color is obtained The solid is 0.46g, which is the target product of this example, and the yield is 96%.

[0043] Mass spectrometry: theoretical value: C25H20ClFeN2: 439.0664, measured value: 439.0714[M-Cl]+( figure 2 ).

[0044] Elemental analysis results: theoretical value: C25H20Cl2FeN2: C, 63.19%; H, 4.24%; N, 5.90%; measured value: C, 62.92%; H, 4.19%; N, 5.72%.

[0045] Infrared analysis: IR(KBr) / cm-1:1587, ν(C=N).

Embodiment 3

[0047] The pyridine imine iron complex shown in the formula (III) prepared in this embodiment, wherein R1"=H, R2"=H, R3"=CH3, the preparation process is as follows:

[0048] Under a nitrogen atmosphere, add an equimolar ratio of 2,6-bis(benzhydryl)-4-methylphenyl substituted pyridinimine ligand and anhydrous FeCl in a dry Schlenk tube, and then Add 10ml CH2Cl2 and stir at room temperature for 24 hours, filter the product and wash with 10ml n-hexane, wash three times, and vacuum-dry to constant weight to obtain 0.61g wine red solid, which is the target product of this example, with a yield of 93%.

[0049] Mass spectrometry: theoretical value: C39H32ClFeN2: 619.1603, measured value: 619.0020[M-Cl]+( image 3 ).

[0050] Elemental analysis results: theoretical value: C39H32Cl2FeN2: C, 71.47%; H, 4.92%; N, 4.27%; measured value: C, 71.98%; H, 4.88%; N, 4.18%.

[0051] Infrared analysis: IR(KBr) / cm-1:1593, ν(C=N).

[0052] 2. Polymerization of isoprene

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Abstract

The invention relates to the technical field of conjugated diene catalytic polymerization, in particular to an iron-based catalyst; the iron-based catalyst comprises a main catalyst and an auxiliary catalyst; the main catalyst is pyridylimine iron complex, the auxiliary catalyst is methylaluminoxane, and a molar ratio of aluminum in the auxiliary catalyst to iron in the main catalyst is 500:1. Application of the iron-based catalyst in isoprene polymerization is also disclosed. The iron-based catalyst of the application has high activity in catalyzing isoprene, the obtained polymer has high molecular weight and narrow molecular weight distribution, the microscopic structure of the polymer may be controlled through cutting the main catalyst structure, the proportion of cis-1,4 structure in isoprene is adjustably in the range of 62.7% to 86.7%, the proportion of trans-1,4 structure is adjustably in the range of 2.8% to 8.2%, and the proportion of 3,4 structure is adjustably in the range of 6.7% to 34.5%. The iron-based catalyst is insensitive to reaction temperature.

Description

technical field [0001] The present invention relates to the technical field of catalytic polymerization of conjugated diolefins, in particular to an iron-based catalyst, a preparation method of the iron-based catalyst, and the use of an iron-based catalyst in catalyzing the polymerization of isoprene to prepare high molecular weight and microstructure. Applications of controlled polyisoprene. Background technique [0002] Isoprene can synthesize cis-1,4 structure, trans-1,4 structure, 1,2 structure and 3,4 structure through 1,4 addition, 1,2 addition and 3,4 addition polymer. The difference in microstructure determines the different properties of polyisoprene. For example, the performance of cis-1,4 polyisoprene is similar to that of natural rubber. It can be widely used in many rubber processing fields such as tires, tapes, hoses, and rubber shoes. It is a rubber with the best comprehensive performance among synthetic rubbers. The performance of trans-1,4 polyisoprene is...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F36/08C08F136/08C08F4/70
CPCC08F4/7006C08F36/08C08F136/08C08F2500/01
Inventor 郭丽华刘哲刘燕兰刘文静
Owner QUFU NORMAL UNIV
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