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In situ ligand generated and ligand crystallized lanthanide complex and its preparation method

A technology of in-situ ligands and complexes, which is used in compounds containing Group 3/13 elements of the periodic table, chemical instruments and methods, luminescent materials, etc., to achieve good fluorescence performance and magnetic function, and the effect of simple and easy synthesis

Inactive Publication Date: 2012-06-27
TIANJIN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is very challenging to design and construct such molecular-based magnetic materials with special structures and properties and fluorescent materials with good luminescent properties.

Method used

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  • In situ ligand generated and ligand crystallized lanthanide complex and its preparation method
  • In situ ligand generated and ligand crystallized lanthanide complex and its preparation method
  • In situ ligand generated and ligand crystallized lanthanide complex and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A method for preparing the lanthanide complex formed by the in-situ ligand and coordinated crystallization, the steps are as follows:

[0019] 1) Dissolve 1mmol of 8-hydroxyquinoline, 2mmol of terbium nitrate and 1mmol of sodium azide in 10ml of ethanol solvent, stir for 10 minutes and seal in a hydrothermal axe;

[0020] 2) Insulate at 120°C for two days, then cool down to room temperature at a rate of 5°C per hour, and the obtained blocky crystal is the target object.

[0021] Characterization of the lanthanide complex:

[0022] 1) Determination of crystal structure

[0023] Select a single crystal with a suitable size under a microscope, and use Mo-Kα rays (λ=0.71073 ),by to collect diffraction data. All diffraction data were corrected for absorption using the SADABS program]. The unit cell parameters were determined using the least squares method. Data restoration and structure elucidation were done using the SAINT and SHELXTL programs, respectively. Partia...

Embodiment 2

[0032] A method for preparing the lanthanide complex formed by the in-situ ligand and coordinated crystallization, the steps are as follows:

[0033] 1) Dissolve 1mmol of 8-hydroxyquinoline, 1.5mmol of gadolinium nitrate and 2mmol of sodium azide in 10ml of ethanol solvent, stir for 15 minutes and seal in a water heat axe;

[0034] 2) Insulate at 130°C for two days, then cool down to room temperature at a rate of 5°C per hour, and the obtained blocky crystal is the target object.

[0035] Characterization of the lanthanide complex:

[0036] 1) Determination of crystal structure:

[0037] The lanthanide complex and the lanthanide complex prepared in Example 1 are isomorphic compounds.

[0038] 2) Magnetic performance test:

[0039] The magnetic test of the lanthanide complex was completed with the Quantum Design MPMS XL-7SQUID device. The test showed that there is a weak magnetic interaction between the rare earth ions in the lanthanide complex, which has a magnetic refriger...

Embodiment 3

[0041] A method for preparing the lanthanide complex formed by the in-situ ligand and coordinated crystallization, the steps are as follows:

[0042] 1) Dissolve 1mmol of 8-hydroxyquinoline, 2mmol of ytterbium nitrate and 2mmol of sodium azide in 10ml of ethanol solvent, stir for 20 minutes and seal in a hydrothermal axe;

[0043] 2) Insulate at 140°C for two days, then cool down to room temperature at a rate of 5°C per hour, and the obtained blocky crystal is the target object.

[0044] The lanthanide complex and the lanthanide complex prepared in Example 1 are isomorphic compounds.

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Abstract

An in situ ligand generated and ligand crystallized lanthanide complex has the following chemical formula: Ln3L4(NO3)2(H2O)2H3O, wherein Ln is lanthanide rare earth ion, L is an organic ligand 1,1-[7,7'-bis-(8-hydroxy negative ion quinoline)]. The organic ligand is in situ generated during the preparation process of a lanthanide coordination polymer and has the following molecular formula: [C20H14N2O2]2-. A preparation method of the lanthanide complex comprises the following steps of: 1) dissolving 8-hydroxyquinoline, lanthanide nitrate and sodium azide in ethanol, stirring and sealing in a hydrothermal kettle; and 2) insulating at 120-140 DEG C for two days and cooling to room temperature according to a program to obtain a bulky crystal, namely the target. The invention has the following advantages: the organic ligand which is directly obtained by a one-pot method participates in coordination to obtain the lanthanide complex; the synthesis of the ligand and the complex is simple and easy to operate; and the compound obtained has good fluorescence performance and magnetic function.

Description

【Technical field】 [0001] The invention relates to the synthesis technology of molecular-based materials, in particular to a lanthanide complex formed by in-situ ligand formation and coordinated crystallization and a preparation method thereof. 【Background technique】 [0002] In recent years, the design and synthesis of molecular-based materials with specific structures and physical functions has aroused great interest, see: You Xiaozeng, Molecular Materials-Photoelectric Functional Compounds, Shanghai Science and Technology Press, 2001; Zhu Daoben, Progress in Chemistry of Functional Materials , Chemical Industry Press, 2005; Hong Maochun, Chen Rong, Liang Wenping, Inorganic Chemistry in the 21st Century, Science Press, 2005; Larsson, K. Molecule-Based Materials: The Structural Network Approach, Elsevier B.V.: Amsterdam, 2005; Li Hui Hui, Coordination Chemistry, Chemical Industry Press, 2006. It is different from traditional inorganic materials. When molecules are aggregate...

Claims

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Application Information

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IPC IPC(8): C07F5/00C09K11/06
Inventor 刘福臣赵炯鹏赵翠焦永坤刘叶
Owner TIANJIN UNIVERSITY OF TECHNOLOGY
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