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Tree polynuclear pyridine diimine iron catalyst precursor for olefine polymerization and preparation method thereof

A technology of nuclear pyridine bis-imine and pyridine bis-imine, which is applied in the field of olefin polymerization catalyst precursors, can solve the problems of slow reaction speed and catalyst embedding, and achieve the effects of stable properties and convenient preparation

Inactive Publication Date: 2006-04-12
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] One of the solutions is to bond the catalyst to the macromolecule to prepare a macromolecule catalyst, such as Gibson's Cp(RN)VCl 3 Connected to polystyrene (Chem.Commun.1998, 1673), but the reaction speed is slow when polymerized, and the phenomenon that the catalyst is often embedded by the polymer molecular chain

Method used

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  • Tree polynuclear pyridine diimine iron catalyst precursor for olefine polymerization and preparation method thereof
  • Tree polynuclear pyridine diimine iron catalyst precursor for olefine polymerization and preparation method thereof
  • Tree polynuclear pyridine diimine iron catalyst precursor for olefine polymerization and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] In a 100ml reaction flask, add 0.754ml of 2,6-diisopropylaniline, 0.652g of 2,6-diacetylpyridine, dropwise add 1ml of formic acid as a catalyst, stir at room temperature for 24 hours under nitrogen, a yellow precipitate appears, after filtration , the obtained yellow powder was washed 3 times with cold methanol to obtain the monoimine compound, then the monoimine compound was dissolved in 30ml of isopropanol, a small amount of dichloromethane was added to make it completely dissolved, and then an excess of 4-allyl- 2,6-Diisopropylaniline, 1 mL of formic acid was used as a catalyst, and a yellow precipitate appeared when heated under reflux for 24 hours. After filtration, the obtained yellow powder was washed three times with cold isopropanol and dried in vacuo to obtain 1.3 g of pyridinebisimine compound, Yield 77%. 1 HNMR (CDCl 3 ): δ8.46-8.5 (br, 2H, Py-Hm), 7.94 (br, 1H, Py-Hp), 7.17 (d, 2H, Ph-Hm), 7.11 (t, 3H, Ph-Hp), 6.98 (s, 2H, Ph-Hm), 6.05 (br, 1H, -CH=C), 5....

Embodiment 2

[0031] Use 2,6-dimethylaniline 0.54g (4mmol) to replace the 2,6-diisopropylaniline in Example 1, and a slightly excess 4-allyl-2,6-dimethylaniline to replace the example 4-allyl-2,6-diisopropylaniline in 1, and other operations were the same as those in Example 1, to obtain 1.2 g of a pyridinebisimine compound with a yield of 75%.

Embodiment 3

[0033] In a 100mL reaction flask, 1.36g (10mmol) of tetravinylsilicon and 7.5g (80mmol) of dimethylchlorosilane were added, 1mg of chloroplatinic acid was added in an ice-water bath, stirred for 2 hours, and then reacted at room temperature for 8 hours, and then the solvent was removed in vacuo With excess chlorosilane, 4.9 g of tetrakis (chlorosilane) compound was obtained with a yield of 95%.

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Abstract

The invention discloses a tree form pyridine diimine Fe (II) olefin polymerization catalyst precursor having the structure disclosed in the specification, wherein X is Cl or Br, R is methyl or isopropyl, by activation of alkyl aluminoxane, the catalyst precursor according to the invention can be used in the catalyzing of ethane polymerization for preparing polyethylene with high molecular weight.

Description

technical field [0001] The present invention relates to an olefin polymerization catalyst precursor, its preparation method and its application in catalyzing ethylene polymerization. Background technique [0002] Polyolefins are a class of synthetic polymer materials with the largest yield and the most extensive applications. Industrial production requires highly active catalysts with controllable structures. The emergence of metallocene and late transition metal catalysts makes this requirement possible. They have high activity, The advantages of a single active center, etc., have attracted great interest, and related patents have also emerged. , WO98 / 30612), in 1999 BP Chemical Company disclosed a class of structurally similar olefin polymerization catalysts (WO 99 / 12981). Such pyridinebisimine Fe(II) olefin polymerization catalyst precursors have the following structure: [0003] [0004] Wherein X is Cl or Br; R is hydrogen, methyl, isopropyl or tert-butyl, etc. Un...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F4/80C08F10/02
Inventor 李悦生郑战江
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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