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Nitrogen-containing bidentate heterocycle-substituted 1,2,3-triazole rare earth complex and synthetic method thereof

A technology of rare earth complexes and synthesis methods, which is applied in the fields of compounds containing Group 3/13 elements of the periodic table, chemical instruments and methods, luminescent materials, etc. High, product purity, cost reduction effect

Active Publication Date: 2013-08-28
GUANGDONG SYNYOO NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Up to now, no new rare earth luminescent complexes suitable for practical application, even for OLED display and lighting technology have been reported.

Method used

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  • Nitrogen-containing bidentate heterocycle-substituted 1,2,3-triazole rare earth complex and synthetic method thereof
  • Nitrogen-containing bidentate heterocycle-substituted 1,2,3-triazole rare earth complex and synthetic method thereof
  • Nitrogen-containing bidentate heterocycle-substituted 1,2,3-triazole rare earth complex and synthetic method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Example 1: Synthesis and fluorescence emission spectrum test of tris[5-(2,2'-bipyridin-6-yl)-1,2,3-1H-triazole]europium(III) (compound 5)

[0045] Step 1: Preparation of N-oxy-2,2’-bipyridine (compound 2)

[0046]

[0047] First, add 2,2’-bipyridine (compound 1, 100g) and acetic acid (500mL) into a 2L three-necked flask, stir well, and add 30% H 2 o 2 (70mL), heated to 70-75°C, stirred for 3 hours, cooled to room temperature, added 30% H 2 o 2 (70mL), continue heating to 60-110°C, and react for 3 hours. After cooling to room temperature, acetic acid was concentrated under reduced pressure to obtain a reddish-brown viscous oil, which was diluted with water (1000 mL), and the pH was adjusted to 8-9 with solid sodium carbonate. The resulting solution was extracted with dichloromethane (1000 mL+500 mL×3), and the organic phases were combined and dried with anhydrous sulfuric acid. After filtration, the filtrate was concentrated under pressure to obtain a reddish-bro...

Embodiment 2

[0061] Example 2: Synthesis and fluorescence emission spectrum test of tris[5-(2,2'-bipyridin-6-yl)-1,2,3-1H-triazole]terbium(III) (compound 6)

[0062]

[0063] Compound 4 (6.7g) obtained in Example 1 and terbium trichloride hexahydrate (3.7g) were respectively dissolved in 50mL of absolute ethanol: water (V:V) = 1:3 mixed solvent to form a solution C and D. Add 1.2g of sodium hydroxide to solution C, and stir for half an hour. Then, the D solution was added dropwise into the reaction bottle of the C solution, and the reaction was stirred at room temperature for 16 hours. After the reaction, the solvent was evaporated to dryness under reduced pressure, and the solid was vacuum-dried at 50° C. for 3 hours to obtain 9.4 g of yellow powder.

[0064] MS: [M+1] 826.1, TbC 36 h 24 N 15 M.W.=825, the ratio of M+H peak 826 and 827 peak heights is close to the isotopic abundance ratio of Tb 2:1.

[0065] It can be known from the fluorescence emission spectrum test that the fl...

Embodiment 3

[0066] Example 3: Tris[5-(4,4'-dimethyl-2,2'-bipyridin-6-yl)-1,2,3-1H-triazole]europium(III) (compound 11 ) synthesis and fluorescence emission spectrum test

[0067] The first step: Preparation of N-oxy-4,4'-dimethyl-2,2'-bipyridine (compound 8)

[0068]

[0069] First, add 4,4'-dimethyl-2,2'-bipyridine (compound 7, 100g) and chloroform (600mL) into a 2L three-necked flask, stir evenly and cool to 0°C, slowly add A solution of m-chloroperoxybenzoic acid (180 g) in chloroform (500 mL). Gradually rise to room temperature, stir and react for 3 hours; continue heating to 60°C, and react for another 3 hours. Cool to room temperature, concentrate the chloroform under reduced pressure, dilute with water (1000 mL), and adjust the pH to 8-9 with solid sodium carbonate. The mixture was heated to 90-95°C for half an hour, cooled, and filtered with suction to remove the unreacted raw material 4,4'-dimethyl-2,2'-bipyridine. The obtained filtrate was extracted with dichloromethane (...

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Abstract

The invention discloses a nitrogen-containing bidentate heterocycle-substituted 1,2,3-triazole rare earth complex LnL3 having a structure represented by formula 1, and a preparation method thereof. In the formula 1, Ar is a nitrogen-containing bidentate heterocyclic ring; R1 is selected from H, alkyl groups, halogenated alkyl groups and aryl groups; and a central rare earth Ln is anyone selected from yttrium, lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium and lutetium. The preparation method is characterized in that the adoption of one of nitrogen-containing bidentate heterocycle-substituted triazole compounds comprising dipyridine, phenanthroline triazole and the like as a single ligand can also satisfy the coordination saturation, and the triazolyl group in the complex adopted as a negative ion and the central rare earth metal cation realize the charge balance to obtain the electric neutrality. The preparation method has the advantages of high yield, short reaction time, simple operation and great cost reduction, and the obtained rare earth complex has the advantages of good purity and high thermal stability, and can be processed through an evaporation film forming technology or a solution film forming technology to make devices.

Description

Technical field: [0001] The invention relates to a nitrogen-containing bidentate heterocyclic substituted 1,2,3-triazole rare earth complex and a synthesis method thereof. Background technique: [0002] At present, my country has a unique resource advantage for the development of rare earth applications. Among the world's rare earth resources that have been identified, 80% (36-37%, WIKI) of rare earth resources are in my country, and the variety is complete. In order to protect resources and avoid environmental problems caused by over-exploitation, my country began to control the export of rare earth ores in 2009, but was protested by countries such as the United States, Japan and Europe. This reflects the preciousness of rare earth resources and the necessity and urgency of vigorously developing rare earth deep processing from another perspective. In view of my country's rich and distinctive rare earth resources, when my country's rare earth industry urgently needs to tran...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/00C09K11/06
Inventor 史华红宋继国方航兵梁东宁尚恩
Owner GUANGDONG SYNYOO NEW MATERIAL
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