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Iron complex on basis of flexible frameworks, method for preparing iron complex and application of iron complex to isoprene polymerization

A technology of iron complexes and flexible skeletons, applied in the direction of iron organic compounds, etc., can solve the problems of wide molecular weight distribution of polymers, high polymerization cost, and regulated polymerization by catalytic microstructure, and achieve the effect of simple synthesis method and low price.

Active Publication Date: 2018-10-16
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to solve the problems of wide polymer molecular weight distribution, high polymerization cost and inability to control the catalytic microstructure in the existing isoprene polymerization technology, the application provides a new type of iron catalyst

Method used

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  • Iron complex on basis of flexible frameworks, method for preparing iron complex and application of iron complex to isoprene polymerization
  • Iron complex on basis of flexible frameworks, method for preparing iron complex and application of iron complex to isoprene polymerization
  • Iron complex on basis of flexible frameworks, method for preparing iron complex and application of iron complex to isoprene polymerization

Examples

Experimental program
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Effect test

preparation example 1

[0035] This embodiment prepares the pyridinium imine iron complex shown in formula II:

[0036] 100mL dry reaction bottle, add 4A molecular sieve and bake for 30 minutes. Under argon atmosphere, dry dichloromethane (40 mL), 4-fluorobenzylamine (1.2 g, 9.3 mmol) and pyridine-2-carbaldehyde (1.0 g, 9.3 mmol) were added sequentially. The reaction was carried out overnight at room temperature, and the reaction of the aldehyde substrate was detected by TLC plate to complete the reaction. Filtration, spinning to dryness, and drying under vacuum gave a yellow liquid (1.9g, yield: 93%), the structural formula was

[0037] 25mL dry reaction tube, add 15mL redistilled dichloromethane, equimolar ratio of anhydrous FeCl in the glove box 2 (100.0 mg, 0.8 mmol) and the above-prepared pyridine imine ligand (169.0 mg, 0.8 mmol) were stirred at room temperature for 15 h. After the reaction, dichloromethane was vacuum-dried, washed 3 times by adding 10 mL of dry n-hexane, and vacuum-dried ...

preparation example 2

[0041] This embodiment prepares the pyridinium imine iron complex shown in formula III:

[0042]100mL dry reaction bottle, add 4A molecular sieve and bake for 30 minutes. Under argon atmosphere, dry dichloromethane (40 mL), 2,6-difluorobenzylamine (1.34 g, 9.34 mmol) and 2-pyridinecarbaldehyde (1.0 g, 9.34 mmol) were added sequentially. The reaction was carried out overnight at room temperature, and the reaction of the aldehyde substrate was detected by TLC plate to complete the reaction. Filtration, spinning to dryness, and drying under vacuum gave a yellow solid (1.7g, yield: 79%), the structural formula was

[0043] 25mL dry reaction tube, add 15mL redistilled dichloromethane, equimolar ratio of anhydrous FeCl in the glove box 2 (100.0 mg, 0.8 mmol) and the above-prepared pyridine imine ligand (183.0 mg, 0.8 mmol) were stirred at room temperature for 15 h. After the reaction was completed, the dichloromethane was vacuum-dried, and 10 mL of dry n-hexane was added to was...

preparation example 3

[0047] The present embodiment prepares the pyridine imine iron complex shown in formula IV:

[0048] 100mL dry reaction bottle, add 4A molecular sieve and bake for 30 minutes. Under argon atmosphere, dry dichloromethane (60 mL), 4-trifluoromethylbenzylamine (2.5 g, 14.0 mmol) and pyridine-2-carbaldehyde (1.5 g, 14.0 mmol) were added sequentially. The reaction was carried out overnight at room temperature, and the reaction of the aldehyde substrate was detected by TLC plate to complete the reaction. Filtration, spinning to dryness, and drying under vacuum gave a yellow liquid (3.3g, yield: 90%), the structural formula was

[0049] 25mL dry reaction tube, add 15mL redistilled dichloromethane, equimolar ratio of anhydrous FeCl in the glove box 2 (100.0 mg, 0.8 mmol) and the above-prepared pyridine imine ligand (208.5 mg, 0.8 mmol) were stirred at room temperature for 15 h. After the reaction, dichloromethane was vacuum-dried, washed with 10 mL of dry n-hexane for 3 times, an...

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Abstract

The invention discloses an iron complex on the basis of flexible frameworks, a method for preparing the iron complex and application of the iron complex to isoprene polymerization. The iron complex onthe basis of the flexible frameworks is used as a primary catalyst. Co-catalysts include trimethylaluminium, triethylaluminum, triisobutylaluminum, methylaluminoxane or modified methylaluminoxane. The application includes steps of adding the primary catalyst, solvents and the co-catalysts; adding isoprene monomers and carrying out polymerization reaction to obtain polyisoprene. The ranges of theproportions of cis-1, 4 structures in obtained isoprene rubber are 29-48%, and the ranges of the proportions of 3, 4 structures are 52-71%. The iron complex, the method and the application have the advantages that polymers are high in molecular weight and narrow in molecular weight distribution; the use efficiency of iron-based catalysts can be effectively improved by the aid of a method for preparing the isoprene rubber, and the industrial application values of the iron-based catalysts can be effectively increased by the aid of the method for preparing the isoprene rubber.

Description

technical field [0001] The present invention relates to the field of chemical synthesis. Background technique [0002] As one of the synthetic rubber varieties with superior comprehensive performance, isoprene rubber not only has some similar characteristics to natural rubber, but also has the advantages of wide sources of synthetic raw materials and good processing performance, and is playing an increasingly important role in the synthetic rubber industry. effect. Since Williams separated isoprene from natural rubber decomposition products in 1860, more and more scientists have devoted themselves to the research of synthesizing natural rubber from isoprene. Polyisoprene has four different microstructures: cis-1,4-polyisoprene; trans-1,4-polyisoprene; 3,4-polyisoprene and 1,2- Polyisoprene. Because there are different structural units and structural unit connection methods in polyisoprene, there are large performance differences between different polyisoprenes. For examp...

Claims

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Application Information

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IPC IPC(8): C07F15/02C08F136/08C08F4/70
CPCC07F15/02C08F136/08C08F4/7006
Inventor 王庆刚赵梦梦王晓武王亮咸漠张献辉
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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