A kind of iridium-containing complex responsive to cu2+ and its preparation method and application
A technology of iridium complexes and ketone compounds is applied in the field of photoelectric phosphorescent materials, which can solve the problems of slow detection speed and high detection price, and achieve the effects of high selectivity, high sensitivity and long emission life.
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Embodiment 1
[0053] With 1-phenothiazinyl-4-phenyloxazine as the main ligand, 2-pyridinecarboxylic acid is the preparation of the iridium-containing complex of the auxiliary ligand, comprising the following steps (such as figure 1 shown):
[0054] (1) Preparation of 4-phenyl-2,3-phthalazin-1-one
[0055] 2-Benzoylbenzoic acid (5.66g, 25mmol) and 2mL85% hydrazine hydrate were placed in a 150mL round-bottomed flask, then 50mL of ethanol was added to it, and heated to reflux for 6h. After the reaction is complete, cool to room temperature, filter under reduced pressure, wash the solid three times with a small amount of ethanol and water mixed solvent, and dry at 60°C for 24 hours to obtain 4-phenyl-2,3-phthalazin-1-one White solid 4.94g, yield 89%; m.p.246-248℃;
[0056] The characterization parameters of 4-phenyl-2,3-naphthyridine-1-one are as follows:
[0057] 1 H-NMR (CDCl 3 ,400MHz)δ10.95(s,1H,N-H),8.51(d,J=8Hz,1H,phthalazinering),7.76(t,J=16Hz,3H,phthalazinering),7.57(d,J=8Hz,2H, p...
Embodiment 2
[0085] Embodiment 1 contains iridium complex at a concentration of 1 × 10 -5 Cu in mol / L acetonitrile solution 2+ Response UV-Vis absorption spectrum test such as figure 2 shown. It can be seen from the spectrum that the absorption peaks of the iridium-containing complexes are mainly concentrated in two regions: a relatively strong absorption peak at 220-350 nm in the near ultraviolet region and a weak absorption peak at 405 nm. In addition, it can also be clearly seen that with Cu 2+ (0~2.0eq), the UV absorption curve of the complex changed significantly, and the absorption peak at 228nm became stronger, indicating that Cu 2+ The addition of the iridium complex has a significant effect on the photophysical properties of the solution, and can be used as a phosphorescent material for detecting copper ions in the environment.
Embodiment 3
[0087] Embodiment 1 contains iridium complex to Cu 2+ The response phosphorescence emission spectrometry test as image 3 shown. In acetonitrile solution, the concentration is 1×10 -5 The emission of mol / L iridium-containing complex is red light, and its maximum emission wavelength is 658nm. With Cu 2+ (0~2.0eq) gradually added, the emission peak intensity at 658nm gradually weakened, and when Cu 2+ When the addition amount of is greater than 2 equivalents, the intensity of this emission peak no longer changes. It shows that the copper ion has the effect of phosphorescent quenching on the iridium complex, and it can be used as a copper ion probe for the sensing of copper ion.
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