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O-phenanthroline triazole rare earth complex and preparation method thereof

A technology of phenanthroline triazoles and phenanthroline triazoles, which is applied in the field of new-type o-phenanthroline triazole rare earth complexes and their preparation, achieving the effects of cost reduction, high yield, and high product purity

Active Publication Date: 2013-06-26
GUANGDONG SYNYOO NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Up to now, no new rare earth luminescent complexes suitable for practical applications, even for OLED display and lighting technology have been reported.

Method used

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  • O-phenanthroline triazole rare earth complex and preparation method thereof
  • O-phenanthroline triazole rare earth complex and preparation method thereof
  • O-phenanthroline triazole rare earth complex and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Example 1: Synthesis and fluorescence emission spectrum test of tris[5-(1,10-phenanthroline-2-yl)-1,2,4-1H-triazole]europium(III) (compound 6)

[0041] The first step: preparation of N-oxy-1,10-phenanthroline (compound 2)

[0042]

[0043] First, compound (1) o-phenanthroline (100g) and acetic acid (100mL) were added into a 2L three-neck flask, stirred evenly, and 30% H 2 o 2 Aqueous solution (75mL), heated to 70-75°C, stirred for 3 hours. Cool to room temperature, add 30% H 2 o 2 (70mL), continue heating to 60-110°C, and react for 3 hours. After cooling to room temperature, the acetic acid was concentrated under reduced pressure to obtain a reddish-brown viscous oil, which was diluted with water (500 mL), and the pH was adjusted to 9-10 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 concentr...

Embodiment 2

[0058] Example 2: Synthesis and fluorescence emission spectrum test of tris[5-(1,10-phenanthroline-2-yl)-1,2,4-1H-triazole]terbium(III) (compound 7)

[0059]

[0060] Compound 4 (7.4g) 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 8 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 9.3 g of yellow powder.

[0061] Mass spectrum such as figure 2 As shown, [M+1]898.1, TbC 42 h 24 N 15 M.W.=897, the ratio of M+H peak 898 to 899 peak height is detected close to the isotopic abundance ratio of Tb 2:1.

[0062] It can be known from th...

Embodiment 3

[0063] Example 3: Tris[5-(4,7-dimethyl-1,10-phenanthroline-2-yl)-1,2,4-1H-triazole]europium(III) (compound 13 ) synthesis and fluorescence emission spectrum test

[0064] Step 1: Preparation of N-oxy-4,7-dimethyl-1,10-phenanthroline (compound 9)

[0065]

[0066] First, add 4,7-dimethyl-1,10-phenanthroline (compound 8, 100g) and chloroform (800mL) into a 2L three-necked flask, stir evenly and cool to 0°C, slowly add A solution of m-chloroperoxybenzoic acid (90 g) in chloroform (600 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 can be heated to 90-95°C for half an hour, cooled and filtered with suction to remove unreacted raw material 4,7-dimethyl-1,10-phenanthroline. The obtained filtrate was extracted with dichloromethane...

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Abstract

The invention provides a novel o-phenanthroline triazole rare earth complex LnL3 and a preparation method thereof. The structural formula of the o-phenanthroline triazole rare earth complex LnL3 is shown in formula 1, wherein R1 is selected from amino, alkyl or aromatic hydrocarbon groups, R2 is selected from amino, alkyl or aromatic hydrocarbon groups, R3 is selected from amino, halogen, alkyl, halogenated alkyl or aromatic hydrocarbon groups, and a central rare earth ion Ln is selected from any one of yttrium, lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium and lutetium. The o-phenanthroline triazole rare earth complex LnL3 disclosed by the invention takes an o-phenanthroline triazole trident compound as a single ligand, and satisfies the ligand saturation, and a situation that a charge balance is electrically neutral is realized between triazole groups in the complex as anions and central rare earth metal cations. The rare earth complex disclosed by the invention is high in thermal stability, and is suitable for device preparation implemented by using an evaporation film-forming process or a solution film-forming process. The preparation method is high in yield, good in product purity, short in reaction time and simple in operation, and the cost is greatly reduced.

Description

Technical field: [0001] The invention relates to a novel o-phenanthroline triazole rare earth complex and a preparation method thereof. Background technique: [0002] 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 transform into a high-tech functional material indus...

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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