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Hydrogen-bonded rare-earth metal europium complex fluorescent material and preparation method thereof

A rare earth metal, europium complex technology, applied in luminescent materials, chemical instruments and methods, compounds containing periodic table Group 3/13 elements, etc. Assembly and application in the field of fluorescent materials without giving structural information of rare earth metal complexes, etc., to achieve the effect of narrow emission peak, high fluorescence intensity and excellent fluorescence performance

Inactive Publication Date: 2014-04-02
EAST CHINA UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Chinese patents CN1618788A, CN101723962A, CN103254337A, CN102584871A, CN102633823A, etc. respectively disclose the use of picolinic acid, 1,10-phenanthroline, bipyridine, and β-diketone , Schiff bases are rare earth functional materials prepared by single or mixed ligands, but the molecular design of rare earth complexes does not involve hydrogen bond supramolecular self-assembly
[0005] Chinese patent CN101456875A discloses a class of hydrogen-bonded rare earth metal complex antibacterial materials, but does not give the structural information of the rare earth metal complexes and its role in the field of fluorescent materials application
Proton transfer compounds such as pyridine-2,6-dicarboxylic acid and guanidine and their complexes with metal cadmium Cd(II) (A. Moghimi, S.Sheshmani, A. Shokrollahi, et al. Z. Anorg. Allg. Chem ., 2004, 630, 617-624), proton transfer compounds of 1,10-phenanthroline-2,9-dicarboxylic acid and 2,6-diaminopyridine and their complexes with metal cobalt Co(Ⅱ) ( A. Moghimi, R.Alizadeh, A. Shokrollahi, et al. Inorg. Chem., 2003, 42, 1616-1624), proton transfer compounds of pyridine-2,6-dicarboxylic acid and 2,6-diaminopyridine and Its complexes with metal cerium Ce(Ⅲ) and bismuth Bi(Ⅲ) (S.Sheshmani, P.D.Kheirollahi, H.Aghabozorg, et al. Z. Anorg. Allg. Chem., 2005, 631, 3058-3065), However, the literature only involves the structure of related hydrogen-bonded metal complexes, and does not involve the research on its application performance as a new type of functional material.

Method used

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  • Hydrogen-bonded rare-earth metal europium complex fluorescent material and preparation method thereof
  • Hydrogen-bonded rare-earth metal europium complex fluorescent material and preparation method thereof
  • Hydrogen-bonded rare-earth metal europium complex fluorescent material and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Weigh 0.2676 g (0.6 mmol) of Eu(NO 3 ) 3 ·6H 2 O was dissolved in 50 mL of water to obtain solution A1; 0.2183 g (2 mmol) of 2,6-diaminopyridine and 0.3342 g (2 mmol) of pyridine-2,6-dicarboxylic acid were weighed and dissolved in 100 mL of ethanol solution, Stir and reflux at 60°C for 24 h, filter with suction, wash with ethanol three times, and dry in vacuum at 60°C for 4 h to obtain 0.4326 g (pydaH 2 )(pydc) proton transfer compound B1, yield 78.3%;

[0033] Weigh 0.3315 g (1.2 mmol) B1 and dissolve it in 30 mL water to obtain B1 solution; raise the temperature to 80°C, add A1 solution dropwise to B1 solution, stir and react for 5 h, filter, wash with ethanol three times, and dry at 60°C After 4 h, 0.2212 g of off-white solid powder was obtained, with a yield of 41.4%; the filtrate was slowly crystallized at room temperature to obtain pale yellow blocky crystal C1. C1 was washed three times with a small amount of water and ethanol, and filtered to obtain a comple...

Embodiment 2

[0035] Weigh 0.3664 g (1 mmol) of EuCl 3 ·6H 2 O was dissolved in 5 mL of ethanol to obtain solution A2; 0.2728 g (2.5 mmol) of 2,6-diaminopyridine and 0.4345 g (2.6 mmol) of pyridine-2,6-dicarboxylic acid were weighed and dissolved in 15 mL of water, 70 ℃, stirred and refluxed for 12 h, filtered with suction, washed with water three times, and dried in vacuum at 50 °C for 6 h to obtain 0.6451 g (pydaH 2 )(pydc) proton transfer compound B2, yield 91.2%;

[0036] Weigh 0.3315 g (1.2 mmol) of B2 and dissolve it in a mixed solvent of 10 mL of water and 50 mL of ethanol to obtain the B2 solution; raise the temperature to 50°C, add the A2 solution dropwise into the B2 solution, stir for 6 h, filter, and wash with ethanol After washing three times and drying at 50°C for 5 h, 0.2885 g of off-white solid powder was obtained, with a yield of 48.9%. The filtrate was slowly crystallized at room temperature to obtain light yellow blocky crystal C2. C2 was washed three times with a smal...

Embodiment 3

[0038] Weigh 0.3380 g (0.5 mmol) of Eu 2 (C 2 o 4 ) 3 ·6H 2 O was dissolved in 10 mL of water and 10 mL of ethanol mixed solvent to obtain solution A3; weigh 0.5238 g (4.8 mmol) of 2,6-diaminopyridine and 0.7688 g (4.6 mmol) of pyridine-2,6-dicarboxylic acid and dissolve in In 40 mL ethanol solution, stirred and refluxed at 50 °C for 20 h, filtered with suction, washed with ethanol three times, and dried in vacuum at 70 °C for 4 h to obtain 1.1737 g (pydaH 2 )(pydc) proton transfer compound B3, yield 90.8%;

[0039] Weigh 0.8288 g (3 mmol) B3 and dissolve it in the mixed solution of 10 mL water and 5 mL ethanol to obtain the B3 solution; warm up to 50 °C, add the A3 solution dropwise into the B3 solution, stir for 4 h, filter, and use After washing with absolute ethanol three times, drying at 60°C for 4 h, 0.5787 g of off-white solid powder was obtained, with a yield of 52.0%. The filtrate was slowly crystallized at room temperature to obtain C3 as pale yellow blocky crys...

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Abstract

The invention discloses a hydrogen-bonded rare-earth metal europium complex fluorescent material and a preparation method thereof. The hydrogen-bonded rare-earth metal europium complex is prepared from a proton transfer compound formed by a rare earth metal element europium and 2,6-diamido-pyridine and pyridine-2,6-dioctyl phthalate in a hydrogen bond coordination manner. The hydrogen-bonded rare-earth metal europium complex fluorescent material has the characteristics of narrow fluorescence emission peak, good monochromaticity, strong fluorescence intensity, good thermal stability and the like, and is an ideal red fluorescent material.

Description

technical field [0001] The invention relates to a hydrogen-bonding rare earth metal complex and a preparation method thereof, in particular to a rare earth europium complex fluorescent material and a preparation method thereof, belonging to the technical field of rare earth functional materials. Background technique [0002] Rare earth luminescent materials are particularly eye-catching among rare earth functional materials, and they are also new materials that will be developed during the "Twelfth Five-Year Plan" period in my country. Rare-earth metal complexes composed of rare-earth metals and ligands with high absorption coefficients have the characteristics of good fluorescence monochromaticity and high luminous intensity, and have been paid more and more attention by people. [0003] On the other hand, using molecules or ions as templates to assemble molecules or ions into molecular aggregates with one-dimensional or multi-dimensional structures through hydrogen bonds i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/00C09K11/06
Inventor 陈建定高勰蔡梦军
Owner EAST CHINA UNIV OF SCI & TECH
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