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Iridium complex-containing phosphor material as well as preparation and application in beryllium ion detection

A phosphorescent material, iridium complex technology, applied in luminescent materials, material analysis by optical means, material analysis and other directions, can solve problems such as inability to detect beryllium ions, achieve high anti-interference performance, simple synthesis route, high sensitivity Effect

Active Publication Date: 2018-05-29
ANHUI UNIVERSITY OF TECHNOLOGY
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  • Abstract
  • 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

Method used

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  • Iridium complex-containing phosphor material as well as preparation and application in beryllium ion detection
  • Iridium complex-containing phosphor material as well as preparation and application in beryllium ion detection
  • Iridium complex-containing phosphor material as well as 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: 3,4-dihydroxybenzaldehyde and lithium hydroxide are dissolved in water, then 1,4-dichloroethyl ether solution is added dropwise thereto, under nitrogen condition, The reaction temperature is 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), Reaction 48-86h (48h, 50h, 52h, 54h, 56h, 58h, 60h, 62h, 64h, 66h, 68h, 70h, 72h, 74h, 76h, 78h, 80h, 82h, 84h, 86h, etc. can be selected for specific applications Numerical value) obtains the derivative of 9-crown-3;

[0062]

[0063]The amount of the reactant is in molar parts, 1 part of 3,4-dihydroxybenzaldehyde, 1-2 parts of 1,4-dichloroethyl ether (1 part, 1.1 part, 1.2 part, 1.3 part can be selected in specific application , 1.4 parts, 1.5 parts, 1.6 part...

Embodiment 1

[0079] Synthesis of 9-Crown-3 Derivatives (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 1,4-dichloroethyl ether, dropwise Reflux for 86 hours after the addition, add a dilute solution of hydrochloric acid to adjust the pH to about 2, then repeatedly extract with dichloromethane and water several times, and wash the organic phase with 4% NaOH aqueous solution after washing; dry after washing, spin Dry, and finally use petroleum ether ethyl acetate system silica gel column chromatography to obtain a yellow oily product 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 2-Benzothiazole-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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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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