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Preparation method of iridium complex-containing phosphorescence material and its application in cobalt ion detection

A technology of iridium complexes and phosphorescent materials, applied in luminescent materials, fluorescence/phosphorescence, material excitation analysis, etc., can solve the problems of limited fluorescent probes and methods, high background, poor selectivity, etc., and achieve large stoke transfer, The effect of high sensitivity and high selectivity

Inactive Publication Date: 2012-04-11
ANHUI UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the fluorescent probes and methods suitable for cobalt detection are very limited, and most fluorescent probes respond to cobalt ions only in the presence of oxidizing reagents, such as hydrogen peroxide, and in alkaline media.
In addition, many of these probes are poorly selective and have high background
Therefore, it is still a challenge to find new cobalt ion fluorescent probes with low cost, fast response, easy implementation, application in natural environment, food and biological system, and obvious detection phenomenon.

Method used

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  • Preparation method of iridium complex-containing phosphorescence material and its application in cobalt ion detection
  • Preparation method of iridium complex-containing phosphorescence material and its application in cobalt ion detection
  • Preparation method of iridium complex-containing phosphorescence material and its application in cobalt ion detection

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Experimental program
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Effect test

Embodiment 1

[0035] Embodiment 1: The preparation steps of this embodiment are as follows:

[0036] (1) Preparation of 3, 4-diphenylcinnoline (dpci):

[0037] Dissolve 2g of 2-aminobenzophenone (10mmol) in 60mL of anhydrous diethyl ether, and then add dropwise therein the The Grignard reagent solution was refluxed for 45 minutes after the dropwise addition, and excess methanol and ammonium nitrate were added to quench the reaction. After washing with water and drying, the solvent was evaporated, and methanol recrystallized to obtain 2.7 g of light yellow prismatic crystal amino alcohol product, with a yield of 93%. m.p.149-150℃.

[0038] Add 0.75g (2.6mmol) of the product from the previous step into 20mL of 20% (volume ratio) sulfuric acid, heat at 100°C for 45min, adjust to weak alkalinity with aqueous ammonia, distill off the solvent after extraction with ether, add 5mL of acetic acid and 3.5 mL of concentrated hydrochloric acid After dissolving completely, add 2.5% sodium nitrite aque...

Embodiment 2

[0044] Embodiment 2: based on iridium complex Ir(dpci) 2 (dafbc)PF 6 Phosphorescence emission spectroscopy tests of phosphorescence chemical sensors responding to cobalt ions such as figure 1 Shown, in the mixed solution of dimethylformamide and water, Ir(dpci) 2 (dafbc)PF 6 The emission is pure red, and its maximum emission peak is at 673nm. With Co 2+ Gradually added, the intensity of the emission peak of 673 gradually weakened, while the peak at 721nm decreased slowly, and gradually emerged, and finally became the largest peak.

Embodiment 3

[0045] Embodiment 3: adding different metal ions (2.0 × 10 -4 mol / L), the iridium complex Ir(dpci) 2 (dafbc)PF 6 In dimethylformamide-water solution (1.0×10 -4 mol / L) changes in the emission spectrum such as figure 2 shown. It can be seen that the emission peak of the solution without adding metal ions is at 673nm; adding Li + , Na + , K + , Ca 2+ , Ba 2+ , Mg 2+ , Hg 2+ , Ag + , Cu 2+ , Fe 2+ , Ni 2+ , Zn 2+ , Cr 3+ , Pb 2+ and Cd 2+ After plasma, there is little change in peak intensity and no change in peak position. While joining Co 2+ The spectrum of the complex changed a lot, the peak at 673nm gradually weakened, and the peak at 721nm gradually appeared, and finally became the largest peak. This comparative experiment shows that Co 2+ The addition of complex Ir(dpci) 2 (dafbc)PF 6 The photophysical properties of the solution have obvious effects, and the complex has a strong effect on Co 2+ There is excellent selectivity.

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Abstract

Belonging to the technical field of photoelectric phosphorescence materials, the invention discloses a preparation method of an iridium complex-containing phosphorescence material and its application in cobalt ion detection. With a general structural formula as shown in formula I, the iridium complex-containing phosphorescence material of the invention can be used for Co<2+> detection and comprises a main ligand and an auxiliary ligand, wherein, the main ligand is a derivative of 3, 4-disubstituted cinnoline, and the auxiliary ligand is a derivative of 15 crown-5 ether dipyridine. By means of the influence of Co<2+> on photo-physical and sensing properties of the iridium complex, the phosphorescence chemical sensor can observe the change of its phosphorescence emission spectrum so as to reach the Co<2+> detection purpose. The phosphorescence chemical sensor of the invention has the advantages of rapid phosphorescence response speed, easy differentiation from a fluorescence background, large range, high identification sensitivity to Co<2+>, good stability, and applicability for Co<2+> detection in various environments, and small interference from other positive ions, etc. Formula I is shown as the following.

Description

technical field [0001] The invention belongs to the technical field of photoelectric phosphorescent materials, and in particular relates to a preparation method of an iridium-containing complex phosphorescent material, which can be used for the detection of cobalt ions. Background technique [0002] Cobalt is a natural metal element. It is the twenty-seventh element in the periodic table. It belongs to the transition metal element and has relatively active chemical properties. It exists in the state of various compounds in nature and is widely distributed in rocks, soil, and water. It is one of the essential trace elements for all multicellular organisms, and it is enriched in the liver, bones and kidneys in the human body. Cobalt can stimulate the hematopoietic system of human bone marrow, promote the synthesis of hemoglobin and increase the number of red blood cells. Vitamin B 12 Participate in physiological functions in the body in the form of The mechanism of cobalt s...

Claims

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Application Information

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IPC IPC(8): C07F15/00C09K11/06G01N21/64
Inventor 童碧海梅群波杨子郑明东张小勇余谟鑫
Owner ANHUI UNIVERSITY OF TECHNOLOGY
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