Dipyridine iron complex, and preparation method and applications thereof

A bipyridine iron and complex technology, applied in the field of isoprene catalyzed polymerization, can solve the problems of poor microstructure controllable adjustment ability and high catalyst cost, and achieve the effects of excellent selectivity, high molecular weight and high activity

Inactive Publication Date: 2019-09-27
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

[0003] Aiming at the technical problems of the high cost of the catalyst used in the synthesis process of polyisoprene and the poor controllability and adjustment ability of the microstructure, the present invention provides a bipyridyl iron complex with the structural formula:

Method used

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  • Dipyridine iron complex, and preparation method and applications thereof
  • Dipyridine iron complex, and preparation method and applications thereof
  • Dipyridine iron complex, and preparation method and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1. Synthesis of bipyridyl iron complex 1.

[0029] The bipyridyl iron complex described in the present embodiment has the structural formula:

[0030] Prepared by the following method:

[0031] Add anhydrous FeCl to a 50 mL Schlenk bottle under argon atmosphere 2 (164.8mg, 1.3mmol), dissolved in 10mL of absolute ethanol at 60°C; then a solution of 2,2'-bipyridine (203.0mg, 1.3mmol) in ethanol (10mL) was added dropwise to the system. React at 60°C for 1 hour. The orange-red complex precipitated from the system, was filtered, washed twice with cold ethanol, concentrated to remove the solvent, and dried in vacuum for 12 hours to obtain orange-red solid product 1 with a yield of 74%.

[0032] Mass Spectrometry: C 10 h 8 Cl 2 FeN 2 :[M-Cl]+: theoretical value: 246.9720; measured value: 246.9718.

[0033] Elemental Analysis: C 10 h 8 Cl 2 FeN 2 : Theoretical value: C, 42.45%; H, 2.85%; N, 9.90%; Measured value: C, 42.72%; H, 2.67%; N, 9.82%.

Embodiment 2

[0034] Embodiment 2: the synthesis of bipyridyl iron complex 2.

[0035] The bipyridyl iron complex described in the present embodiment has the structural formula:

[0036] Prepared by the following method:

[0037] Add anhydrous FeCl to a 50 mL Schlenk bottle under argon atmosphere 3 (210.6mg, 1.3mmol), dissolved in 10mL of absolute ethanol at 60°C; then a solution of 2,2'-bipyridine (203.0mg, 1.3mmol) in ethanol (10mL) was added dropwise to the system. React at 60°C for 1 hour. The yellow complex precipitated from the system, filtered, washed twice with cold ethanol, concentrated to remove the solvent, and dried in vacuo for 12 hours to obtain apricot yellow solid product 2 with a yield of 77%.

[0038] Mass Spectrometry: C10 h 8 Cl 3 FeN 2 : [M-Cl]+: theoretical value: 281.9408; measured value: 281.9404.

[0039] Elemental Analysis: C 10 h 8 Cl 3 FeN 2 : Theoretical value: C, 37.73%; H, 2.53%; N, 8.80%; Measured value: C, 37.98%; H, 2.26%; N, 8.55%.

Embodiment 3

[0040] Embodiment 3: the synthesis of bipyridyl iron complex 3.

[0041] The bipyridyl iron complex described in the present embodiment has the structural formula:

[0042] Prepared by the following method:

[0043] Add anhydrous Fe(acac) to a 50 mL Schlenk bottle under argon atmosphere 2 (127.0mg, 0.5mmol), dissolved in 6mL of absolute ethanol at 60°C; then a solution of 2,2'-bipyridine (78.1mg, 0.5mmol) in ethanol (4mL) was added dropwise to the system. React at 60°C for half an hour, then return to room temperature and stir overnight. The filtrate was collected by filtration, concentrated, washed twice with cold ethanol, and dried in vacuum for 12 h to obtain product 3 as a brownish yellow solid with a yield of 68%.

[0044] Mass Spectrometry: C 20 h 22 FeN 2 o 4 :[M+H]+: theoretical value: 411.1002; measured value: 410.0998.

[0045] Elemental Analysis: C 20 h 22 FeN 2 o 4 : Theoretical value: C, 58.55%; H, 5.41%; N, 6.83%; Measured value: C, 58.34%; H, 5.53%...

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Abstract

The invention discloses a dipyridine iron complex, and a preparation method and applications thereof, and belongs to the field of isoprene catalytic polymerization. The preparation method is capable of solving technical problems in the prior art that in conventional polyisoprene synthesis process, the adopted catalyst is high in cost, and micro structure controllable adjusting capacity is poor. The dipyridine iron complex is prepared through reaction of an ethanol solution of dipyridine with an ethanol solution of a ferrous salt or a ferric salt. The dipyridine iron complex is taken as a main catalyst in polyisoprene polymerization, the activity is high, the molecular weight of obtained polymers is high, and molecular weight distribution range is narrow. The preparation method can be used in polyisoprene industrialized production.

Description

technical field [0001] The invention relates to the field of catalytic polymerization of isoprene, in particular to a bipyridyl iron complex and its preparation method and application. Background technique [0002] For a long time, the contradiction between rolling resistance and wet skid resistance of tire compounds has hindered the development and promotion of "green tires". Trans-1,4-polyisoprene rubber (TPI), high vinyl polybutylene rubber The emergence of new materials such as vinylene rubber (HVBR) and 3,4-polyisoprene rubber (3,4-PIP) has opened up a new way for the research and application of "green tires". 3,4-polyisoprene (3,4-PIP) has high wet skid resistance, low rolling resistance and good shock absorption performance, and can be used to manufacture high-performance tires; the water resistance of this isoprene rubber The air tightness is close to butyl rubber; it can also be used together with ethylene-propylene rubber to prepare vulcanized rubber with high per...

Claims

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Application Information

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IPC IPC(8): C08F136/08C08F4/70C07F15/02
CPCC07F15/025C08F136/08C08F2500/01C08F2500/03C08F4/7006
Inventor 王庆刚王亮朱广乾张献辉荆楚杨
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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