Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

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
View PDF1 Cites 5 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • 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%...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com