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Differently substituted 2-hydroxy-1,3-phthalaldehyde and long-chain dual-amine mixed nickel complex and preparation method thereof

A technology of phthalaldehyde and nickel complexes, applied in the direction of nickel organic compounds, etc., can solve the problems of difficult purification and separation of samples, high risk and high temperature, and achieve the effects of high yield, overcoming high temperature and high pressure, and mild conditions.

Inactive Publication Date: 2011-09-07
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, most of the synthesis methods of nickel metal phenolic imine complexes are hydrothermal or solvothermal synthesis methods. This method has technical defects such as high temperature, high risk, low yield, and difficult purification and separation of samples.

Method used

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  • Differently substituted 2-hydroxy-1,3-phthalaldehyde and long-chain dual-amine mixed nickel complex and preparation method thereof
  • Differently substituted 2-hydroxy-1,3-phthalaldehyde and long-chain dual-amine mixed nickel complex and preparation method thereof
  • Differently substituted 2-hydroxy-1,3-phthalaldehyde and long-chain dual-amine mixed nickel complex and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0022] The preparation of embodiment 1 complex

[0023] Put 0.1mmol 5-isopropyl-2-hydroxyl-1,3-benzenedicarbaldehyde on the bottom layer of the first side of the H-type tube, add a small amount of distilled water to dissolve to form reaction solution A, add methanol and water volume to the upper layer of reaction solution A 2mL of mixed solution E with a ratio of 1:1, add 0.3mmol of 5-tert-butyl-2-hydroxyl-1,3-benzenedicarbaldehyde and 5-isopropyl-2-hydroxyl-1 to the upper layer of mixed solution E, Methanol solution C of 3-phthalaldehyde; add 0.4mmol Ni(ClO 4 ) 2 ·6H 2 O, 0.2 mmol NaN 3 , Dissolved with 5mL of distilled water to form reactant B, add 2mL of mixed solution F of methanol and water with a volume ratio of 1:1 in the upper layer of reaction solution B; then add 0.2mmol 1,3-diaminoethylamino-2 in the upper layer of solution F -Hydroxypropane, dissolved in 5mL of methanol to form reaction solution D, then slowly drop methanol into the solution until the two sides...

Embodiment 2

[0025] The preparation of embodiment 2 complexes

[0026] Put 0.1mmol 5-isopropyl-2-hydroxyl-1,3-benzenedicarbaldehyde on the bottom layer of the first side of the H-type tube, add a small amount of distilled water to dissolve to form reaction solution A, add methanol and water volume to the upper layer of reaction solution A 2mL of mixed solution E with a ratio of 1:1, add 0.3mmol of 5-tert-butyl-2-hydroxyl-1,3-benzenedicarbaldehyde and 5-isopropyl-2-hydroxyl-1 to the upper layer of mixed solution E, Methanol solution C of 3-phthalaldehyde; add 0.4mmol Ni(AcO) to the bottom layer of the II side of the H-tube 2 4H 2 O, 0.2 mmol NaN 3 , Dissolved with 5mL of distilled water to form reactant B, add 2mL of mixed solution F of methanol and water with a volume ratio of 1:1 in the upper layer of reaction solution B; then add 0.2mmol 1,3-diaminoethylamino-2 in the upper layer of solution F -Hydroxypropane, dissolved in 5mL of methanol to form reaction solution D, then slowly drop ...

Embodiment 3

[0028] The preparation of embodiment 3 complexes

[0029] Put 0.1mmol 5-isopropyl-2-hydroxyl-1,3-benzenedicarbaldehyde on the bottom layer of the first side of the H-type tube, add a small amount of distilled water to dissolve to form reaction solution A, add methanol and water volume to the upper layer of reaction solution A 2mL of mixed solution E with a ratio of 1:1, add 0.3mmol of 5-tert-butyl-2-hydroxyl-1,3-benzenedicarbaldehyde and 5-isopropyl-2-hydroxyl-1 to the upper layer of mixed solution E, Methanol solution C of 3-phthalaldehyde; add 0.4mmol NiCl to the bottom layer of the II side of the H-tube 2 ·6H2 O, 0.2 mmol NaN 3 , Dissolved with 5mL of distilled water to form reactant B, add 2mL of mixed solution F of methanol and water with a volume ratio of 1:1 in the upper layer of reaction solution B; then add 0.2mmol 1,3-diaminoethylamino-2 in the upper layer of solution F -Hydroxypropane, dissolved in 5mL of methanol to form reaction solution D, then slowly drop meth...

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Abstract

The invention relates to 5-isopropyl-2-hydroxy-1,3-phthalaldehyde, 5-tert-butyl-2-hydroxy-1,3-phthalaldehyde and 1,3-2-aminoethyl amino-2-hydroxy propane mixed nickel complex and a preparation method thereof. The complex is prepared by adopting an H-tube through a diffusion method. Multiple different ligands for coordination and metal salts are skillfully put on two ends of an H-tube to ensure that the diffusion is slower and more uniform to be good for culturing and generating ligand crystals. In addition, the reaction is carried out under normal pressure and temperature. The method ensures mild reaction condition and high yield and has good reproducibility. The obtained ligand crystals are expected to be further studied and applied in the field of magnetic materials.

Description

Technical field: [0001] The invention belongs to the field of transition metal complex materials, in particular to 5-isopropyl-2-hydroxyl-1,3-benzenedicarbaldehyde, 5-tert-butyl-2-hydroxyl-1,3-benzenedicarbaldehyde and 1,3-diaminoethylamino-2-hydroxypropane mixed nickel complex and its preparation method. Background technique: [0002] In recent years, transition metal polymers have attracted the research interests of many scholars at home and abroad because of their diverse topological structures and excellent properties. Conductive materials, nonlinear optical devices and many other fields have shown excellent application prospects. So far, a large number of complexes have been designed and synthesized, and their properties have been studied. Most of the ligands they use are carboxylic acids and nitrogen heterocycles. For a long time, nickel metal complexes have attracted extensive attention due to their rich structures and potential excellent properties, and have become...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/04
Inventor 解永树何昌华汪成杨玉华
Owner EAST CHINA UNIV OF SCI & TECH
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