M-methyl pyridine tetrazole copper [I] complex blue-light emitting material and preparation method thereof

A technology of m-picoline tetrazolium copper and picoline tetrazolium copper is applied in the directions of luminescent materials, copper organic compounds, chemical instruments and methods, etc., and can solve problems such as shortage of raw materials, scarcity of content, and difficulty in mining.

Active Publication Date: 2018-02-02
JIANGXI UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

The transition metals of the fifth and sixth periods (except for a few metals of the first and second subgroups) are scarce in the earth’s crust and are difficult to mine. Therefore, the cost of using luminescent complexes based on such noble metals is relatively high, and large-scale applications It will also bring raw material tension
However, there are few literature reports on the construction of polynuclear copper[I] complex luminescent materials using nitrogen heterocyclic multidentate chelating ligands and organic bisphosphine auxiliary ligands, especially the blue light emitting materials of multinuclear copper[I] complexes
[0005] Design and Synthesis of Tetranuclear Copper[I] Using Pyridine Tetrazolium Multidentate Chelating Ligand 5-[5-Methyl-2-pyridyl]tetrazolium and Diphosphine Auxiliary Ligand Bis[diphenylphosphine]methane The complex blue light-emitting material and its preparation method have not yet been publicly reported in the literature

Method used

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  • M-methyl pyridine tetrazole copper [I] complex blue-light emitting material and preparation method thereof
  • M-methyl pyridine tetrazole copper [I] complex blue-light emitting material and preparation method thereof
  • M-methyl pyridine tetrazole copper [I] complex blue-light emitting material and preparation method thereof

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preparation example Construction

[0031] The present invention provides a kind of preparation method of m-picoline tetrazolium copper [I] complex blue light material (this is the first preparation method), comprising the following steps:

[0032] Step 1: Under an argon atmosphere, [Cu[MeCN] with a molar ratio of 2:2:1 4 ][ClO 4 ], bis[diphenylphosphine]methane, 5-[5-methyl-2-pyridyl]tetrazolium [pytzH for short] in methylene chloride at room temperature and stirred for 2-4 hours to obtain the first reaction mixture .

[0033]Step 2: adding sodium hydroxide in an equimolar amount to the 5-[5-methyl-2-pyridyl]tetrazolium ligand to the first reaction mixture, and continuing to stir and react at room temperature for 1-2 hours to obtain Second reaction mixture.

[0034] Step 3: Evaporate the solvent of the second reaction mixture to dryness, use dichloromethane-n-hexane mixed solvent for recrystallization, filter and recrystallize to obtain a colorless crystalline product, use ether to wash 3-4 times, and obtain...

Embodiment 1

[0045] Under an argon atmosphere, [Cu[MeCN] 4 ][ClO 4 ] (20.9mg, 0.064mmol), bis[diphenylphosphine]methane (24.6mg, 0.064mmol) and 5-[5-methyl-2-pyridyl]tetrazolium (5.2mg, 0.032mmol) in 10mL Stir and react at room temperature in dichloromethane for 3 hours, then add sodium hydroxide (1.28mg, 0.032mmol) to the reaction solution, continue to stir and react at room temperature for 1 hour, then evaporate the solvent to dryness with a rotary evaporator, and dichloromethane (1mL)-n-hexane (10mL) mixed solvent [volume ratio 1:10] for recrystallization. The colorless crystalline product obtained by recrystallization was filtered, washed 3-4 times with 10 mL of ether, and dried in vacuo to obtain a colorless solid product (30.1 mg, 0.013 mmol), with a yield of 81%.

[0046] Elemental analysis calculated value (C 114 h 100 Cl 2 Cu 4 N 10 o 8 P 8 ) as (%): C 59.25, H 4.36, N 6.06; Found: C 59.27, H 4.38, N 6.03.

[0047] X-ray single crystal diffraction: crystal belongs to tri...

Embodiment 2

[0050] Under argon atmosphere, copper perchlorate hexahydrate [Cu[ClO 4 ] 2 ·6H 2 O] (10.4mg, 0.028mmol) and excess copper powder (12.0mg, 0.189mmol) were stirred at room temperature in 5mL acetonitrile for 30 minutes, then added bis[diphenylphosphine]methane (21.5mg, 0.056mmol) in 10mL di Chloromethane solution, continue to stir and react for 1 hour, then add 5-[5-methyl-2-pyridyl]tetrazolium (4.5mg, 0.028mmol), continue to stir and react for 2 hours at room temperature, and then add Sodium hydroxide (1.12mg, 0.028mmol), and continue stirring reaction at room temperature for 1 hour, after filtering, evaporate the solvent to dryness with a rotary evaporator, and use dichloromethane (1mL)-n-hexane (10mL) mixed solvent [volume ratio is 1 :10] for recrystallization. The colorless crystalline product obtained by recrystallization was filtered, washed 3-4 times with 10 mL of diethyl ether, and dried in vacuo to obtain a colorless solid product (25.4 mg, 0.011 mmol) with a yield ...

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Abstract

The invention relates to a M-methyl pyridine tetrazole copper [I] complex blue-light emitting material. The M-methyl pyridine tetrazole copper [I] complex blue-light emitting material is characterizedby being a perchlorate [Cu4[5-(5-methyl-2-pyridyl)tetrazolate]2[bis(diphenylphosphino)methane]4][ClO4]2 complex with the molecular formula of Cl14H100Cl2Cu4N10O8P8. The invention further provides twopreparation methods of the M-methyl pyridine tetrazole copper [I] complex blue-light emitting material. The M-methyl pyridine tetrazole copper [I] complex blue-light emitting material belongs to a new blue-light emitting material and has a favorable development prospect.

Description

technical field [0001] The invention relates to a blue-light material of m-picoline tetrazolium copper [I] complex and a preparation method thereof, belonging to the technical field of synthesis of new luminescent materials. Background technique [0002] Due to the influence of heavy atom effect and strong spin-orbit coupling, metal luminescent complexes can theoretically utilize all singlet and triplet energies, greatly improving the luminous efficiency. At present, the research on metallluminescent complexes mainly focuses on the fifth and sixth periods, especially transition metals of group VIII, such as ruthenium, osmium, iridium and platinum. The transition metals of the fifth and sixth periods (except for a few metals of the first and second subgroups) are scarce in the earth’s crust and are difficult to mine. Therefore, the cost of using luminescent complexes based on such noble metals is relatively high, and large-scale applications Finally, there will be tension in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6596C07F1/08C09K11/06
Inventor 何丽华陈景林刘遂军王万曼廖金生温和瑞
Owner JIANGXI UNIV OF SCI & TECH
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