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A kind of substituted bipyridine ferrous complex and its preparation method and application

A technology of ferrous bipyridyl and complexes, 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 catalyst cost and poor controllability of polymer microstructure, and achieve High molecular weight, excellent selectivity, and easy preparation

Active Publication Date: 2021-12-21
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] In order to solve the problem that the cost of the catalyst used in the synthesis of polyisoprene is high and the microstructure of the obtained polymer is poor in controllability and regulation, the present invention provides a substituted bipyridyl ferrous complex, whose structural formula is:

Method used

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  • A kind of substituted bipyridine ferrous complex and its preparation method and application
  • A kind of substituted bipyridine ferrous complex and its preparation method and application
  • A kind of substituted bipyridine ferrous complex and its preparation method and application

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Embodiment 1

[0025] Embodiment 1: the synthesis of substituted bipyridyl ferrous complex 1.

[0026] The structural formula of the substituted bipyridine ferrous complex 1 described in this embodiment is: Prepared by the following method:

[0027] Add anhydrous FeCl to a 50 mL Schlenk bottle under argon atmosphere 2 (139.4mg, 1.1mmol), dissolved in 10mL of absolute ethanol at 60°C; then a solution of 5,5'-dimethyl-2,2'-bipyridine (202.7mg, 1.1mmol) in ethanol (10mL) Add dropwise to the system. React at 60°C for 1 hour. The orange-red complex was precipitated from the system, filtered, washed twice with cold ethanol, concentrated to remove the solvent, and vacuum-dried for 12 hours to obtain apricot-yellow solid product 1 with a yield of 78%.

[0028] Mass Spectrometry: C 12 h 12 Cl 2 FeN 2 : [M-Cl]+: theoretical value: 275.0033; measured value: 275.0038.

[0029] Elemental Analysis: C 12 h 12 Cl 2 FeN 2 : Theoretical value: C, 46.35%; H, 3.89%; N, 9.01%; Measured value: C, 46...

Embodiment 2

[0030] Embodiment 2: the synthesis of substituted bipyridyl ferrous complex 2.

[0031] The structural formula of the substituted bipyridyl ferrous complex 2 described in this embodiment is: Prepared by the following method:

[0032] Add anhydrous FeCl to a 50 mL Schlenk bottle under argon atmosphere 2 (139.4mg, 1.1mmol), dissolved in 10mL of absolute ethanol at 60°C; then 4,4'-Dimethyl-2,2'-dipyridine (202.7mg, 1.1mmol) in ethanol (10mL) Add dropwise to the system. React at 60°C for 1 hour. The brown-yellow complex was precipitated from the system, filtered, washed twice with cold ethanol, concentrated to remove the solvent, and vacuum-dried for 12 hours to obtain the orange-yellow solid product 2 with a yield of 74%.

[0033] Mass Spectrometry: C 12 h 12 Cl 2 FeN 2 :[M-Cl]+: theoretical value: 275.0033; measured value: 275.0040.

[0034] Elemental Analysis: C 12 h 12 Cl 2 FeN 2 : Theoretical value: C, 46.35%; H, 3.89%; N, 9.01%; Measured value: C, 46.85%; H, 3....

Embodiment 3

[0035] Embodiment 3: the synthesis of substituted bipyridyl iron complex 3.

[0036] The structural formula of the substituted bipyridine ferrous complex 3 described in this embodiment is: Prepared by the following method:

[0037] Add anhydrous FeCl to a 50 mL Schlenk bottle under argon atmosphere 2 (76.0mg, 0.6mmol), dissolved in 6mL of absolute ethanol at 60°C; The solution was added dropwise to the system. React at 60°C for 1 hour. The brown-red complex was precipitated from the system, filtered, washed twice with cold ethanol, concentrated to remove the solvent, and dried in vacuum for 12 hours to obtain dark red solid product 3 with a yield of 47%.

[0038] Mass Spectrometry: C 12 h 12 Cl 2 FeN 2 o 2 :[M-Cl]+: theoretical value: 306.9931; measured value: 306.9935.

[0039] Elemental Analysis: C 12 h 12 Cl 2 FeN 2 o 2 : Theoretical value: C, 42.02%; H, 3.53%; N, 8.17%; Measured value: C, 42.51%; H, 3.26%; N, 8.43%.

[0040] Embodiment 4: the synthesis of s...

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Abstract

A substituted bipyridyl ferrous complex and its preparation method and application belong to the field of isoprene catalytic polymerization. In order to solve the problem that the cost of the catalyst used in the synthesis of polyisoprene is high and the microstructure of the obtained polymer is poorly controllable and adjustable, the present invention provides a substituted bipyridyl ferrous complex, which is the ethanol compound of bipyridine The solution and the ethanol solution of the ferrous salt are mixed according to the equivalence ratio of 1:1 and then reacted. The isoprene polymer is prepared by using the substituted bipyridyl ferrous complex, which has high molecular weight and narrow molecular weight distribution. The invention is suitable for industrialized production of isoprene.

Description

technical field [0001] The invention relates to the field of catalytic polymerization of isoprene, in particular to a ferrous substituted bipyridyl complex and its preparation method and application. Background technique [0002] In recent years, with people's emphasis on environmental protection, the shortage of oil resources in the world and the rapid development of the automobile industry, high speed, safety, comfort and energy saving have become the basic requirements of automobiles. The tires used must have high wet skid resistance and low rolling resistance and good abrasion resistance. However, these three properties restrict each other, how to improve these three properties at the same time has become an important direction of tire research. 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 ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F15/02C08F36/08C08F136/08C08F4/70
CPCC07F15/025C08F36/08C08F136/08C08F4/7006
Inventor 王庆刚朱广乾王亮张献辉荆楚杨
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI