Monoimino pyrrole iron and preparation method and application thereof

A monoimine pyrrole, -CH3 technology, applied in the direction of iron organic compounds, etc., can solve the problems of transition metal complex catalysts that are rarely explored, and achieve good industrial application prospects, high yield, and less by-products.

Inactive Publication Date: 2013-04-03
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

By synthesizing molecules with similar structures to pyridine bis-imine ligands (such as changing pyridine rings to pyrrole rings, bis-imine systems to mono-imine systems, etc.), a large number of such catalysts have been obtained. However, for Ligands are changed from the parent structure to prepare late transition metal complex catalysts, but few people have explored

Method used

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  • Monoimino pyrrole iron and preparation method and application thereof
  • Monoimino pyrrole iron and preparation method and application thereof
  • Monoimino pyrrole iron and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The general structural formula of monoimine pyrrole iron is:

[0027] Formula I

[0028] where R 1 for -CH 3 ,R 2 is H, X is Cl - .

[0029] The chemical name is: dichloro 2-{1-[(2,6-xylyl)imine]ethyl}pyrrolate iron (II)

[0030] The preparation method of above-mentioned monoimine pyrrole iron is made up of the following steps:

[0031] (1) Mix 0.1313g of 2-acetylpyrrole and 0.1342g of substituted aniline of formula II according to the molar ratio of 1:1.2, and react under microwave conditions with a power of 700W for 25 minutes. The crude product is subjected to conventional chromatography Separation and purification give monoimine pyrrole, namely 2-{1-[(2,6-xylyl)imine]ethyl}pyrrole. R in Formula II 1 for -CH 3 ,R 2 for -H.

[0032] (2) Add 5mL of FeCl with a concentration of 20mmol / L 2 Ethanol solution and 4.5 mL of 2-{1-[(2,6-xylyl)imine] ethyl}pyrrole ethanol solution prepared in step (1) with a concentration of 20 mmol / L under nitrogen protection at ...

Embodiment 2

[0034] In the present embodiment, the general structural formula of monoimine pyrrole iron is formula I, wherein R 1 for -CH 3 ,R 2 is H, X is Cl - , the chemical name is: Dichloro·2-{1-[(2,6-xylyl)imine]ethyl}pyrrolate iron (II).

[0035] The preparation method of above-mentioned monoimine pyrrole iron is made up of the following steps:

[0036] (1) Mix 0.1313g of 2-acetylpyrrole with 0.1118g of substituted aniline of formula II according to the molar ratio of 1:1, react for 25 minutes under microwave conditions with a power of 700W, and chromatographically separate the crude product according to conventional methods , purified to obtain monoimine pyrrole;

[0037] where R in formula II 1 for -CH 3 , R 2 for -H.

[0038] (2) Add 5mL of FeCl with a concentration of 20mmol / L 2 The ethanol solution was mixed with 4 mL of monoimine pyrrole ethanol solution with a concentration of 20 mmol / L under nitrogen protection at a molar ratio of 1:0.8, reacted at room temperature for...

Embodiment 3

[0040] In the present embodiment, the general structural formula of monoimine pyrrole iron is formula I, wherein R 1 for -CH 3 , R 2 is H, X is Cl - , the chemical name is: Dichloro·2-{1-[(2,6-xylyl)imine]ethyl}pyrrolate iron (II).

[0041] The preparation method of above-mentioned monoimine pyrrole iron is made up of the following steps:

[0042] (1) Mix 0.1313g of 2-acetylpyrrole with 0.1677g of substituted aniline of formula II according to the ratio of molar ratio of 1:1.5, react for 25 minutes under microwave conditions with a power of 700W, and chromatographically separate the reaction crude product according to conventional methods, Purify to obtain monoimine pyrrole; wherein R in formula II 1 for -CH 3 , R 2 for -H.

[0043] (2) Add 5mL of FeCl with a concentration of 20mmol / L 2 Ethanol solution and 5 mL of monoimine pyrrole ethanol solution with a concentration of 20 mmol / L were mixed under nitrogen protection at a molar ratio of 1:1, reacted at room temperatu...

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Abstract

The invention relates to a new compound monoimino pyrrole iron and a preparation method and application thereof. A ligand is changed from a parent structure so that the monoimino pyrrole iron has the advantages of novel structure, easy purification, strong water and oxygen resistance and good stability; and the monoimino pyrrole iron is prepared by adopting the steps of: using 2-acetyl pyrrole as a precursor, carrying out condensation reaction with one series of substituted anilines under the condition of microwaves, and complexing with a ferrous compound. The preparation method has the advantages of simpleness in operation, high yield and less byproducts; and by adopting a microwave method, the preparation method is high in reaction speed and simple in operation, can be applied to vinyl polymerization, is capable of effectively limiting the direction and the size of vinyl polymerization to achieve the shearing function on the molecular level of a polymerization product, and has a better industrial application prospect.

Description

technical field [0001] The invention belongs to the technical field of research on late transition metal olefin polymerization catalysts, and particularly relates to a monoimine pyrrole iron compound and its preparation method and application. Background technique [0002] At present, petrochemical industry is still the basis of chemical industry. Polyolefin products made of ethylene, propylene, butadiene, styrene, etc. as raw materials occupy the most important position in the national economy. Catalyst selection is one of the core technologies of the chemical industry. Olefin polymerization catalysts have three important development stages: Ziegler-Natta catalyst system; metallocene catalyst; non-organometallocene olefin catalyst. [0003] Non-organometallocene olefin catalysts refer to those organometallic complexes that do not contain cyclopentadienyl, the coordination atoms are O, N, S and C, etc., and the central metal includes all transition metal elements and some ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/03C08F10/02C08F4/70
Inventor 张喜文苏碧云李谦定
Owner PETROCHINA CO LTD
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