A phosphorescent material containing iridium complex and its preparation and application in beryllium ion detection

A technology of phosphorescent materials and iridium complexes, which is applied in the direction of luminescent materials, material analysis and material analysis through optical means, can solve the problems of inability to detect beryllium ions, etc., and achieve high anti-interference performance, fast response speed and high detection sensitivity Effect

Active Publication Date: 2020-05-12
ANHUI UNIVERSITY OF TECHNOLOGY
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  • Description
  • Claims
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Problems solved by technology

But there is following deficiency in this invention: although mercury ion and beryllium ion all belong to divalent metal ion, because beryllium ion radius is much smaller than mercury ion radius, but Be 2+ The Hg ion probe cannot detect beryllium ions because it cannot exchange with its side ligands

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  • A phosphorescent material containing iridium complex and its preparation and application in beryllium ion detection
  • A phosphorescent material containing iridium complex and its preparation and application in beryllium ion detection
  • A phosphorescent material containing iridium complex and its preparation and application in beryllium ion detection

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preparation example Construction

[0060] A preparation method of phosphorescent material containing iridium complex, the preparation method is as follows:

[0061] (1) The synthetic route of 9-crown-3 derivatives: Dissolve 3,4-dihydroxybenzaldehyde and lithium hydroxide in water, then add dichloroethyl ether solution dropwise therein, under nitrogen condition, the reaction temperature is at 100 -120°C (100°C, 102°C, 104°C, 106°C, 108°C, 110°C, 112°C, 114°C, 116°C, 118°C, 120°C and other values ​​can be selected for specific applications), the reaction time is 48-86h (In specific applications, you can choose 48h, 50h, 52h, 54h, 56h, 58h, 60h, 62h, 64h, 66h, 68h, 70h, 72h, 74h, 76h, 78h, 80h, 82h, 84h, 86h and other values) to get 9 - 4-(formyl)benzo-9-crown-3, a derivative of crown-3;

[0062]

[0063] Wherein the amount of the reactant is in molar parts, 1 part of 3,4-dihydroxybenzaldehyde, 1-2 parts of dichloroethyl ether (1 part, 1.1 part, 1.2 part, 1.3 part, 1.4 part, 1.5 part can be selected during speci...

Embodiment 1

[0079] Synthesis of 9-crown-3 derivative 4-(formyl)benzo-9-crown-3 (abbreviated as 9C3)

[0080] Dissolve 2.4g of 3,4-dihydroxybenzaldehyde (17.4mmol) in 250mL of water, then add dropwise 1.43g (59.7mmol) of lithium hydroxide, 2ml (17.4mmol) of dichloroethyl ether, and reflux after the dropwise addition 86h, add a dilute solution of hydrochloric acid to adjust the pH to about 2, then repeatedly extract with dichloromethane and water for several times, and wash the organic phase with 4% NaOH aqueous solution after washing; dry it after washing, spin dry, and finally use Petroleum ether ethyl acetate system silica gel column chromatography; a yellow oily product was obtained with a yield of 17.9%.

[0081] 1 H NMR (400MHz, CDCl 3 )δ9.87(s,1H),7.57(d,J=2.0Hz,1H),7.54(dd,J=8.3,2.1Hz,1H),7.09(d,J=8.2Hz,1H),4.70– 4.64(m,2H),4.35–4.28(m,2H),4.00–3.94(m,2H),3.94–3.89(m,2H).

Embodiment 2

[0083] Synthesis of 4-(Benzo[d]thiazol-2yl)benzo-9-crown-3

[0084] 0.5g (2.4mmol) the product that embodiment 1 makes is dissolved in 10mL N, N dimethylformamide, drips into 0.6mL (5.6mmol) 2-aminothiophenol solution again, anhydrous magnesium sulfate 0.552g ( 4.6mmol) was reacted for 24h under the protection of nitrogen. After the reaction was completed, it was cooled to room temperature, back-extracted with water and ethyl acetate; Yield 40.8%.

[0085] 1 H NMR (400MHz, CDCl 3 )δ8.03(d, J=8.7Hz, 1H), 7.87(d, J=9.2Hz, 1H), 7.77(s, 1H), 7.68(d, J=11.0Hz, 1H), 7.41(d, J=46.9Hz, 2H), 7.06(d, J=8.4Hz, 1H), 4.52(d, J=6.7Hz, 2H), 4.38(s, 2H), 4.11(d, J=7.1Hz, 1H) ,3.99–3.86(m,4H).

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Abstract

The invention discloses an iridium complex-containing phosphor material as well as preparation and application in beryllium ion detection, belongs to the technical field of photoelectric phosphor materials, and solves the problem in the prior art that the anti-jamming capability of a fluorescent probe for detecting beryllium ions is weaker. The preparation method of the iridium complex-containingphosphor material is characterized by enabling 9-metallacrown-3 to react with 3,4-dihydroxy benzaldehyde, thus obtaining a 9-metallacrown-3 derivative; then synthesizing a dichloro-bridged compound ofiridium on the basis of the 9-metallacrown-3 derivative; then enabling the dichloro-bridged compound of the iridium to interact with a corresponding auxiliary ligand, thus preparing an iridium complex-based phosphor chemical sensor. The iridium complex-containing phosphor material comprises two structural formulas which can be respectively applied to beryllium ion detection in an ionic type solution and a neutral solution; compared with a traditional fluorescent sensor, the iridium complex-based phosphor chemical sensor has larger stokes displacement and longer emission lifetime; meanwhile, the iridium complex-based phosphor chemical sensor has strong anti-jamming capability on multiple metal cations.

Description

technical field [0001] The invention belongs to the technical field of photoelectric phosphorescent materials, and in particular relates to an iridium-containing complex phosphorescent material and its preparation and application in beryllium ion detection. Background technique [0002] Beryllium is a kind of off-white alkaline earth metal, which is increasingly valued as a new material. Beryllium is an indispensable and precious material in atomic energy, rockets, missiles, aviation, space navigation and metallurgical industries. But beryllium and its compounds are highly toxic. Therefore, the detection of beryllium ions in the environment, food and biological samples has attracted widespread attention. At present, the commonly used methods for detecting the content of beryllium ions include spectrophotometry, fluorescence photometry, atomic absorption method, atomic emission method and electrochemical method. But most of the methods require tedious pre-treatment process, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F15/00C09K11/06G01N21/64
CPCC07F15/0033C09K11/06C09K2211/185G01N21/643
Inventor 童碧海潘淼胡媛媛赵卓张千峰
Owner ANHUI UNIVERSITY OF TECHNOLOGY
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