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Iridium complex-containing phosphorescent materials, preparation thereof and application method for detecting mercuric ions and acetonitrile

A technology of iridium complexes and phosphorescent materials, applied in luminescent materials, chemical instruments and methods, compounds containing elements of Group 8/9/10/18 of the periodic table, etc., can solve problems such as hindering the sensitivity of sensors, and achieve large Effects of stoke transfer, long emission life, high photostability

Inactive Publication Date: 2011-09-21
NANJING UNIV OF POSTS & TELECOMM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This hinders the improvement of the sensitivity of the sensor, and it is urgent to develop new varieties

Method used

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  • Iridium complex-containing phosphorescent materials, preparation thereof and application method for detecting mercuric ions and acetonitrile
  • Iridium complex-containing phosphorescent materials, preparation thereof and application method for detecting mercuric ions and acetonitrile
  • Iridium complex-containing phosphorescent materials, preparation thereof and application method for detecting mercuric ions and acetonitrile

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Experimental program
Comparison scheme
Effect test

Embodiment 1、4

[0036] Embodiment 1,4, the preparation of 6-diphenylpyrimidine

[0037] Take 1,3-diphenyl-1,3-beta diketone (0.448g, 2mmol) and 10ml of formamide (0.196mol) into a single-necked flask, then stir overnight at 180°C, after cooling to room temperature Pour into a large amount of water, extract with ethyl acetate, wash the organic phase with water several times, spin dry and pass through a column with silica gel (petroleum ether: ethyl acetate = 6: 1) to obtain a white solid. The product was recrystallized from petroleum ether to obtain 0.371 g, and the yield was 80%.

[0038] GC-MS (EI-m / z): 232 (M + ).

Embodiment 2

[0039]The preparation of embodiment 2,4-(4-bromo-phenyl)-6-phenyl-pyrimidine

[0040] Take 1-(4-bromo-phenyl)-3-phenyl-β diketone (0.602g, 2mmol) and 10ml of formamide (0.196mol) into a one-necked flask, then stir overnight at 180°C, After cooling to room temperature, it was poured into a large amount of water, extracted with ethyl acetate, the organic phase was washed with water several times, spin-dried and passed through a column with silica gel (petroleum ether: ethyl acetate = 6: 1) to obtain a yellow solid, which was washed with ethanol Recrystallization gave 0.465 g of the product, with a yield of 75%.

Embodiment 3

[0041] Embodiment 3, O, the synthesis of O-dimethyl potassium dithiophosphate

[0042] Weigh phosphorus pentasulfide (11.1g, 50.0mmol) and place it in a round bottom flask, place the round bottom flask in an ice-water bath, weigh potassium hydroxide (5.60g, 0.1mol) and dissolve it in 20ml (0.078mol) of methanol, add A small amount of water to completely dissolve and cool. Use a dropper to drop potassium hydroxide methanol aqueous solution into the flask. During the dropping process, irritating gas is generated, the solid dissolves, and a milky white suspension is produced. After reacting for 3 hours, remove the ice-water bath, let it stand for half an hour, and filter under reduced pressure , washed with ether, and dried to obtain 10.4 g of the product, with a yield of 53.1%.

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Abstract

The invention discloses preparation and an application method for iridium complex phosphorescent materials. A series of dithio compounds such as N,N-disubstituted dithio carbamates, or O,O-disubstituted dithio phosphates and alkoxy-substituted dithio formats are subjected to dissociation of dichloro bridged complex of iridium, and iridium complexes shown as a formula (I), a formula (II) or a formula (III) are generated. The iridium complexes can be used for detecting mercuric ions and acetonitrile; and through influence of Hg2+ on physical, electrochemical and sensing properties of the iridium complexes, the iridium complex phosphorescent materials identify the Hg2+ in high selectivity, high sensitivity and quick response, the turn off phenomenon occurs, and a phosphorescent sensor for detecting the Hg2+ can be manufactured. By changing a solvent for detecting, a turn on phenomenon occurs and a novel sensor for detecting acetonitrile can be manufactured.

Description

technical field [0001] The invention belongs to the technical field of photoelectric materials. Specifically, it relates to a kind of iridium complex phosphorescent material responsive to mercury ions and acetonitrile. Background technique [0002] Mercury is one of the most threatening and toxic metal elements to humans and the environment, due to its persistence, easy migration and high bioaccumulation; and mercury and mercury salts are widely used in industry, based on For the above reasons, the detection of mercury ions in the environment has attracted widespread attention. It is necessary to develop a new type of Hg ion with low cost, fast response, easy implementation, application in natural environment and biological system, and obvious detection. 2+ Detection methods are particularly important. Acetonitrile, also known as methyl nitrile, is a colorless and transparent liquid, highly volatile, has a special odor similar to ether, has excellent solvent performance, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/00C09K11/06G01N21/76
Inventor 梅群波郭远辉黄维童碧海王玲霞翁洁娜范曲立
Owner NANJING UNIV OF POSTS & TELECOMM
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