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Phosphorescent iridium complex containing isosulfocyanate radical and preparation method and application thereof

A technology of phosphorescent iridium complexes and isothiocyanic acid, applied in the fields of compounds containing elements of group 8/9/10/18 of the periodic table, fluorescence/phosphorescence, chemical instruments and methods, etc., can solve the value of metal iridium complexes It has not yet been fully developed, and there are no problems such as anionic iridium complexes, etc., to achieve the effects of eliminating interference, long luminescent life, and high detection sensitivity

Inactive Publication Date: 2009-12-02
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, as phosphorescent materials with superior performance, the value of metal iridium complexes for stoichiometric agents has not been fully exploited
So far, only a few cationic iridium complexes have been used to detect heavy metal ions, and no anionic iridium complexes have been reported for the detection of mercury ions.

Method used

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  • Phosphorescent iridium complex containing isosulfocyanate radical and preparation method and application thereof
  • Phosphorescent iridium complex containing isosulfocyanate radical and preparation method and application thereof
  • Phosphorescent iridium complex containing isosulfocyanate radical and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Preparation of iridium complex: weigh IrCl 3 ·3H 2 O (5.52mmol) and 2,4-difluorophenylpyridine (11.04mmol) were added into the three-necked flask, and then a mixed solution of 2-ethylene glycol ether and water was added to dissolve it (2-ethylene glycol ether and The volume ratio of water is 3:1); then the reaction mixture was heated to 110°C and stirred for 24 hours; after the reaction was completed, it was cooled to 10-25°C; a precipitate formed. The resulting precipitate was washed with water and ethanol, respectively, and dried in vacuo to obtain a bright yellow solid 2,4-difluorophenylpyridine iridium dichloro bridge complex, Ir 2 (dfppy) 4 Cl 2 .

[0028] Then weigh 2,4-difluorophenylpyridine iridium dichloro bridge complex (0.2g, 0.16mmol) and tetrabutyl ammonium isothiocyanate solid (0.6g, 2mmol) into the three-necked flask, add 30ml of dichloromethane , reflux for 15 hours. After the reaction, recrystallize and purify with dichloromethane and ether to obt...

Embodiment 2

[0031] The ultraviolet spectrum test of the response of the phosphorescent iridium complex containing isothiocyanate to mercury ions: the product obtained in Example 1 was dissolved in acetonitrile, the concentration of the complex was 20 μmol / L, and then an equal volume of 0-2eq pure water was added to configure of mercury nitrate solution. After being balanced, measure the ultraviolet spectrum, and the test results are shown in figure 1 , with the addition of mercury ions, the intensity of the original three strong absorption peaks at 260nm, 320nm and 370nm gradually weakened, while two new strong absorption peaks at 355nm and 310nm appeared and their intensity gradually increased.

Embodiment 3

[0033] The fluorescence spectrum test of the phosphorescent iridium complex containing isothiocyanate obtained in Example 1 responds to mercury ions: the iridium complex is dissolved in acetonitrile, and the concentration of the complex is 20 μmol / L, and then an equal volume of 0-2eq of pure Mercury nitrate solution in water. After being balanced, measure the fluorescence ultraviolet spectrum, the test result is shown in figure 2 , with the addition of mercury ions, the fluorescence intensity (475nm) gradually decreased until it was quenched.

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Abstract

The invention discloses a phosphorescent iridium complex containing isosulfocyanate radical. The phosphorescent iridium complex has a structural formula shown as a formula (I), and is an anionic iridium complex, wherein the isosulfocyanate radical can be combined with mercury ion to generate mercuric isosulfocyanate; solvent molecule acetonitrile replaces the isosulfocyanate radical to be coordinated with iridium so as to influence the spectral quality of a generated product; and the mercury ion is detected by the change of the spectral quality, and is not interfered by other metallic ions. The complex can be used for preparing a phosphorescent stoichiometric agent for qualitatively detecting the mercury ion. The invention also provides a preparation method for the phosphorescent iridium complex containing the isosulfocyanate radical.

Description

technical field [0001] The invention relates to the technical field of phosphorescent stoichiometric agents, in particular to an anionic phosphorescent iridium complex, specifically a phosphorescent iridium complex containing isothiocyanate, a preparation method and a qualitative detection of mercury ions. Background technique [0002] Phosphorescent heavy metal complexes have attracted more and more attention in the field of photochemistry due to their superior photophysical properties. They have the following characteristics: the emission wavelength changes with the environment; they have a larger (Stokes) Stokes shift and a longer emission lifetime than organic phosphorescent materials, and the long emission lifetime is conducive to the use The time-resolved technology distinguishes the phosphorescence signal from the background phosphorescence signal, which can effectively avoid the interference of background fluorescence. [0003] Mercury is a chemical substance with s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/00C09K11/06G01N21/33G01N21/64
Inventor 杨红杨仕平
Owner SHANGHAI NORMAL UNIVERSITY
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