Schiff base transition metal complex containing alkoxy groups, and preparation method and application thereof

A transition metal and alkoxy technology, applied in the direction of 4/14 group organic compounds without C-metal bonds, compounds of group 4/14 elements of the periodic table, titanium organic compounds, etc., can solve the problem of less use and molar ratio High, unfavorable industrial production and other problems, to achieve the effect of simple preparation method and high activity

Inactive Publication Date: 2012-06-27
SHENYANG POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Although o-vanillin has been used more and more in the synthesis of Schiff base ligands, relatively speaking, substances containing alkoxy groups are still less used in the synthesis of Schiff bases, especially in amine compounds containing alkane Oxygen
In the past, complexes synthesized by Schiff bases and late transition metals have high activity when catalyzing olefin polymerization, but toluene is mostly used as solvent, and modified methylalumoxane is used as cocatalyst, and the metal aluminum in the cocatalyst and the central metal of the cocatalyst The molar ratio is high, which is not conducive to industrial production

Method used

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  • Schiff base transition metal complex containing alkoxy groups, and preparation method and application thereof
  • Schiff base transition metal complex containing alkoxy groups, and preparation method and application thereof
  • Schiff base transition metal complex containing alkoxy groups, and preparation method and application thereof

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preparation example Construction

[0033] The above-mentioned preparation method of the Schiff base transition metal complex containing alkoxy group, it may further comprise the steps:

[0034] (1) Under anhydrous and oxygen-free conditions, in anhydrous methanol solvent, conduct condensation reaction of substituted salicylaldehyde and amine compounds at 20-60°C, filter to remove anhydrous methanol solvent, and dry the obtained solid To obtain the Schiff base ligand;

[0035] (2) Under anhydrous and oxygen-free conditions, in a dichloromethane solvent, first react the Schiff base ligand prepared above with an alkali metal compound at a molar ratio of about 1:1 at -40 to 60°C to obtain Ligand salt solution; then ligand salt solution and MCl 4 React at -40~100°C at a molar ratio of 1:1 or 2:1, drain the dichloromethane solvent under reduced pressure, dissolve the residue in dichloromethane, filter, and drain the filtrate under reduced pressure, then use petroleum ether The residual solid was washed to give the ...

Embodiment 1

[0040] Take the preparation of bis-o-vanillin (diphenyl ether) phenylimide titanium complex as an example.

[0041] (1) Preparation of bis-o-vanillin (diphenyl ether) phenylimine ligand: Add 40ml of anhydrous methanol and 0.001mol of 4,4'-diaminodiphenyl ether into a 250ml three-necked flask, stir until completely dissolved and become colorless Transparent solution; add 0.002mol o-vanillin dissolved in 10ml of anhydrous methanol into the constant pressure funnel, and slowly add the o-vanillin solution dropwise into the three-necked flask. Washed with water and methanol three times; after washing, the reaction solution was transferred to a characteristic bottle, filtered, dried and weighed to obtain ligand a with a yield of 87%.

[0042] FT-IR: 3430(-OH), 1614(C=N), 1257(C-O)

[0043] Elemental analysis theoretical value (%): C, 71.79; N, 5.98; H, 5.13. Experimental values ​​(%): C, 71.81; N, 6.12; H, 5.20.

[0044] (2) Preparation of titanium complex: Add 40ml of dichlorometh...

Embodiment 2

[0047] Take the preparation of bis-2-hydroxy-3-ethoxybenzaldehyde (diphenyl ether) phenylimide titanium complex as an example.

[0048] (1) Method for preparing bis-2-hydroxy-3-ethoxybenzaldehyde (diphenyl ether) phenylimine ligand: add 40ml of anhydrous methanol and 0.001mol of 4,4'-diaminodiphenyl to a 250ml three-necked flask Ether, stir until it is completely dissolved; add 10ml of anhydrous methanol and 0.002mol 2-hydroxy-3-ethoxybenzaldehyde in a constant pressure funnel, and stir 4,4'-diaminodiphenyl ether in a three-necked flask until it is completely dissolved. 2-Hydroxy-3-ethoxybenzaldehyde solution was slowly added dropwise to the three-necked flask. After the dropwise addition was completed, the reaction solution was reacted at 30°C for 4 hours, and then washed three times with 20ml of anhydrous methanol; after washing, the reaction solution was transferred to a characteristic bottle and filtered , dried and weighed to obtain ligand b with a yield of 80%.

[0049...

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Abstract

The invention relates to a Schiff base transition metal complex containing alkoxy groups, a preparation method thereof and application of a catalyst composition composed of the transition metal complex and aluminum alkyl in catalyzing ethene polymerization, belonging to the technical field of catalysts. The preparation method for the Schiff base transition metal complex containing alkoxy groups comprises the following steps: synthesizing Schiff base ligand through a condensation reaction between substituted salicylaldehyde and an amine compound; reacting the ligand with an alkali metal compound to obtain a ligand salt solution; and reacting the ligand salt solution with MCl4 to prepare the Schiff base transition metal complex. The preparation method is simple; and when used for ethene polymerization, the synthesized Schiff base transition metal complex containing alkoxy groups has the following advantages compared to the prior art: common aluminum alkyl is used as a cocatalyst to substitute expensive MAO during polymerization, and the catalyst composition has high activity under the condition of a small usage amount of the cocatalyst. Hexane is used as a solvent to substitute toluene during polymerization, which is favorable for industrial introduction.

Description

technical field [0001] The invention relates to a Schiff base transition metal complex containing an alkoxy group and a preparation method thereof, as well as the application of a catalyst composition composed of the transition metal complex and alkylaluminum in catalyzing ethylene polymerization; it belongs to catalyst technology field. Background technique [0002] Schiff bases have been the focus of researchers in recent years. It is a kind of ligand that is relatively easy to synthesize, and can be synthesized by reacting amines with carbonyl aldehydes and copper. Schiff base ligands contain oxygen atoms and nitrogen atoms that can coordinate, and provide enough space for metal ions to coordinate with them through the carbon chain in the middle, so Schiff bases are very easy to coordinate with late transition metals to form complexes. Chinese patent 101967112A discloses a method for synthesizing bis(5-bromosalicylaldehyde) ethylenediamine iron. The raw materials used...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/28C07F7/00C08F10/02C08F4/64
CPCC07F7/003C08F110/02C08F10/02C08F4/64189C08F2500/04C08F4/64048
Inventor 李三喜王玉现王松张爱玲
Owner SHENYANG POLYTECHNIC UNIV
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