Mellitic acid rare-earth coordination polymer as well as preparation method and application

A technology of mellitic acid and complexes, which is applied in the field of preparation of rare earth metal coordination polymers, can solve the problems of weak absorption, low luminous efficiency, and weak luminescence of a single rare earth ion, and achieve high yield, good reproducibility, Effect of high thermal stability and phase purity

Inactive Publication Date: 2015-11-18
TIANJIN NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the rare earth ions f - f The transition belongs to the forbidden band transition, so it shows very weak absorption in the visible and ultraviolet regions, and the luminescence of a single rare earth ion is relatively weak, and the luminous efficiency is low.

Method used

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  • Mellitic acid rare-earth coordination polymer as well as preparation method and application
  • Mellitic acid rare-earth coordination polymer as well as preparation method and application
  • Mellitic acid rare-earth coordination polymer as well as preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Mellitic acid rare earth metal coordination polymer A Synthesis:

[0028] Dissolve mellitic acid (0.1 mmol, 34.2 mg) and dysprosium nitrate hexahydrate (0.3 mmol, 136.8 mg) in 10.0 mL of double distilled water, adjust the pH of the reaction mixture to 5 with solid sodium hydroxide, and stir the mixture for several Minutes later, it was sealed in a hydrothermal reaction kettle. After the reaction kettle was kept at 200°C for three days, it was heated at 5.0°C·h –1 The rate program cooled down to room temperature to obtain colorless blocky crystals, which were washed with water twice and dried in air.

Embodiment 2

[0030] Mellitic acid rare earth metal coordination polymer B Synthesis:

[0031] Dissolve mellitic acid (0.2 mmol, 68.4 mg) and erbium nitrate hexahydrate (0.5 mmol, 230.5 mg) in 12.0 mL of double-distilled water, adjust the pH of the reaction mixture to 4 with solid sodium hydroxide, and stir the mixture for several Minutes later, it was sealed in a hydrothermal reaction kettle. After the reaction kettle was kept at 180°C for three days, the –1 The rate program cooled down to room temperature to obtain colorless blocky crystals, which were washed with water twice and dried in air.

[0032] The mellitic acid rare earth metal coordination polymer prepared by the present invention (embodiment 1-2, A - B ) is characterized by the following structure:

[0033] (1) Determination of crystal structure ( figure 1 )

[0034] Select a single crystal of a rare earth metal coordination polymer with a suitable size under a microscope, and use graphite monochromatized Mo-Kα rays (λ=...

Embodiment 3

[0042] Prepared by the present invention (embodiment 1-2, A - B ) Rare earth metal coordination polymer optical performance test is as follows:

[0043] After enriching the solid-state coordination polymer crystals prepared in Example 1-2, after further grinding, a solid fluorescence test was carried out on a JobinYvon (Horiba) Fluorolog-3 fluorescence spectrometer. The solid fluorescence test results are shown in Figure 4 . The test results show that under the excitation of 366nm ultraviolet light, the complex sample A has strong fluorescence emission peaks at 482, 573 and 600nm, and the luminescence intensity at 573nm is the largest; under the excitation of 371nm ultraviolet light, the complex sample B has There are two ligand-based fluorescence emission peaks at 417 and 434nm, in addition to a weaker fluorescence emission peak at 504nm.

[0044] The rare earth metal coordination polymer proposed by the present invention is a high-grade fluorescent material that can exis...

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Abstract

The invention relates to a rare-earth metal coordination polymer containing mellitic acid ligands as well as a preparation method and application of the rare-earth metal coordination polymer. The chemical formula of the rare-earth metal coordination polymer is {[Ln (H2O)4(Cl2O12)0.5].H2O}, wherein Ln refers to the rare earth ion Dy (III) or Er (III) of the lanthanide series; Cl2O12<6> refers to a hexavalent negative ion of mellitic acid. The coordination compound is prepared through the hydrothermal method, high in productivity and thermostability, and excellent in reproducibility. The coordination polymer fluorescent material is a three-dimensional rare-earth metal solid coordination polymer based on a rigid mellitic acid ligand. Under UV-irradiation, the coordination compound can emit an emission peak with the rare-earth ion characteristics or an emission peak of an organic ligand and has enormous application value in the material science field as a molecular-based fluorescent material.

Description

[0001] Statement Regarding Funding Research or Development [0002] The present invention has been applied for by the National Natural Science Foundation of China (fund No.: 21171129, 21173157 and 21371134), Tianjin Higher Education Science and Technology Development Fund Project (fund No.: 2012ZD02) and Tianjin Higher Education Innovation Team Training Program (fund No.: TD12-5038) ) for joint funding. technical field [0003] The invention relates to the technical field of metal-organic coordination polymers and molecular-based fluorescent materials thereof, in particular to a preparation method and application of a rare earth metal coordination polymer with rigid mellitic acid as a ligand. The compound is a rare-earth metal three-dimensional coordination polymer with completely deprotonated mellitic acid as the main ligand, and its unique optical properties enable it to be used as a molecular-based fluorescent material in the field of material science. Background techniqu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/00C07C63/313C07C51/41C07C51/00C09K11/06
CPCC07F5/003C07B2200/13C07C51/418C09K11/06C09K2211/182C07C63/313
Inventor 赵小军余佳纹杨恩翠张超
Owner TIANJIN NORMAL UNIVERSITY
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