CN114778644B - Be used for detecting Hg 2+ Preparation method of iridium (III) complex sensitized NiO photocathode - Google Patents

Be used for detecting Hg 2+ Preparation method of iridium (III) complex sensitized NiO photocathode Download PDF

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CN114778644B
CN114778644B CN202210370754.0A CN202210370754A CN114778644B CN 114778644 B CN114778644 B CN 114778644B CN 202210370754 A CN202210370754 A CN 202210370754A CN 114778644 B CN114778644 B CN 114778644B
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李春香
孔令辉
吕蒙伟
宗成雪
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Qingdao University of Science and Technology
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Abstract

The invention discloses an iridium complex (III) ([ (PM-ppy) 2 Ir(daf‑Rh)]PF 6 ) Preparation method of photocathode for sensitization of NiO for Hg 2+ Is detected. Firstly, an iridium complex (III) photosensitizer with recognition sites is designed and synthesized, and then the iridium complex (III) photosensitizer is assembled on an ITO electrode modified by NiO through chemical bonding, so that the NiO photocathode sensitized by the iridium complex (III) is prepared. When Hg is 2+ Hg, when present 2+ Inducing the opening of rhodamine spiro ring increases the absorption of NiO photocathode to visible light, thereby increasing photoelectric signal and realizing Hg 2+ Is a high sensitivity detection of (1). The invention has the advantages of wide linear range, high sensitivity, good selectivity, high reproducibility and the like.

Description

Be used for detecting Hg 2+ Preparation method of iridium (III) complex sensitized NiO photocathode
Technical Field
The invention belongs to the field of photoelectrochemistry and biochemical analysis of dye sensitization, and particularly relates to a preparation method and application of a cyclometallated iridium (III) complex sensitized NiO photocathode with a recognition function.
Background
Mercury (Hg) is the most common toxic precious metal in nature and is present in water, soil and even food, and even when exposed to low concentrations of mercury, it can damage the nervous system, kidneys, brain and other organs of the human body due to its long-lasting, bioaccumulative and non-biodegradable properties. About 7500 tons of mercury and its compounds are reported to be released into the environment each year, and thus for more powerful monitoring of Hg 2+ The use and the discharge of the mercury ion detection method are established, the selectivity is good, and the sensitivity is high, especially H in the environment and drinking waterg 2+ Is very important and urgent. At present, the detection methods of mercury ions mainly comprise atomic absorption spectrum, cold steam atomic fluorescence spectrum, inductively coupled plasma mass spectrometry and a fluorescence method. These classical methods can achieve the desired performance of Hg 2+ Most methods are complex to operate, and equipment is expensive, especially if not suitable for field-adapted detection. Thus, a simple, inexpensive, particularly field-deployable platform is designed for Hg detection 2+ Has important significance.
Photoelectrochemical (PEC) analysis techniques integrate photochemistry and electrochemistry, with distinct advantages over conventional optical and electrochemical analysis techniques. The photocurrent as an output signal makes PEC analysis instrumentation simpler and less costly than the expensive instrumentation requirements for spectral signals. Furthermore, PEC analysis exhibits low background signal and high sensitivity due to the different energy modes of the excitation light source to the detection signal. For a typical PEC analysis, the photoactive species responsible for photoelectric conversion and the recognition unit controlling the output signal response to the analyte concentration are considered to be two indispensable elements. Basically, the photoelectrode composed of a photoactive material can be classified into a photoanode and a photocathode according to the type of semiconductor. Semiconductor-based n-type photoanode analysis has been dominant in the PEC sensor field over the last two decades. In recent years, photocathode analysis based on p-type semiconductors has been attracting more attention because of its inherent ability to resist interference with the reductive substances coexisting in practical detection systems. Up to now, the most widely used p-type photocathode semiconductor is clearly NiO, which has a bandgap of about 3.5eV, is cost effective, and is easy to prepare nanostructures by various methods. In order to improve the performance thereof, the design of suitable sensitizers has been a focus of attention. The cyclometallated iridium (iii) complexes have been widely used in recent years in the fields of organic electroluminescence, dye-sensitized solar cells, etc., due to their abundant and widely adjustable photophysical properties and electrochemical properties. At present, cathodic photoelectric bioassays are just started, and particularly, a system for bioanalytical by sensitization of NiO by Ir (III) complexes has not been reported yet. The invention develops the iridium (III) with the identification function) The complex is used as a photosensitizer to construct a NiO photocathode to realize Hg 2+ Is a highly sensitive and highly selective assay.
The invention comprises the following steps:
in view of the defects of the prior art, the invention provides an iridium (III) complex photosensitizer with an identification function, and a dye-sensitized NiO photocathode is constructed and used for detecting mercury ions in a water system, and the iridium (III) complex photosensitizer has the characteristics of high sensitivity, good selectivity, low cost and wide linear range.
Based on the above object, the technical scheme of the invention is as follows:
the present invention aims to provide an iridium (III) based complex ([ (PM-ppy) 2 Ir(daf-Rh)]PF 6 ) Preparation method of NiO photocathode sensitized by PM-ppy as main ligand and daf-Rh as auxiliary ligand for detecting Hg 2+ 。[(PM-ppy) 2 Ir(daf-Rh)]PF 6 The structural formula is as follows:
the method comprises the following steps:
(1) Preparation of NiO modified ITO electrode: firstly, the ITO electrode with fixed area is sequentially put into absolute ethyl alcohol, acetone, absolute ethyl alcohol and ultrapure water for cleaning and drying. Fixing the cleaned ITO electrode with a fixed area of 0.5X0.5 cm 2 The electrode was then immersed in a solution containing 0.25M Ni (NO 3 ) 2 ·6H 2 In a mixed solution of O and 0.25M hexamethylenetetramine, the mixture is heated for 60 minutes at 90 ℃ in an electrothermal constant temperature blast drying oven and naturally cooled to room temperature. The ITO electrode was rinsed 3 times with ultrapure water and dried under air. And finally, placing the ITO electrode into a muffle furnace, heating for 30 minutes at 300 ℃, and naturally cooling to room temperature to obtain the modified electrode (NiO/ITO).
(2)[(PM-ppy) 2 Ir(daf-Rh)]PF 6 Assembly of NiO/ITO electrode: soaking the NiO/ITO electrode prepared in the step (1) in [ (PM-ppy) at room temperature 2 Ir(daf-Rh)]PF 6 (1. Mu.M) in solution for 12 hours, the [ (PM-ppy) 2 Ir(daf-Rh)]PF 6 Assembled to the NiO surface. The electrodes are sequentially made of DMF and CH 3 After CN washing, the mixture was dried in air to obtain photocathode [ (PM-ppy) 2 Ir(daf-Rh)]PF 6 /NiO/ITO.
Preferably, the iridium (III) complex [ (PM-ppy) 2 Ir(daf-Rh)]PF 6 The solvent of the solution was DMF.
(3)Hg 2+ Is detected: the photocathode [ (PM-ppy) prepared in the step (2) is subjected to 2 Ir(daf-Rh)]PF 6 Soaking NiO/ITO in a solution containing Hg at different concentrations 2+ In a buffer solution of (0.1M, pH=7.4) for 5 minutes to [ (PM-ppy) 2 Ir(daf-Rh)]PF 6 NiO/ITO was used as the working electrode to record photocurrent. Adopting 570nm light excitation, setting 20s light-on light source once, and realizing Hg with different concentrations, wherein the bias voltage is 0V 2+ Is a signal response of (a).
The invention has the beneficial effects that:
(1) The invention discloses an iridium complex [ (PM-ppy) 2 Ir(daf-Rh)]PF 6 Sensitized NiO photocathode for Hg 2+ Wherein the photosensitizer [ (PM-ppy) 2 Ir(daf-Rh)]PF 6 Has the function of identifying Hg 2+ Is provided.
(2) The photocathode is opposite to Hg 2+ The detection of the (C) has wide linear range and high detection sensitivity, the detection limit is 4.75pM, and the (C) has short response time and excellent selectivity and reproducibility.
Description of the drawings:
FIG. 1[ (PM-ppy) 2 Ir(daf-Rh)]PF 6 Preparation of/NiO/ITO photocathode and detection of Hg 2+ Is a schematic diagram of (a).
FIG. 2[ (PM-ppy) 2 Ir(daf-Rh)]PF 6 Is a composite roadmap of (a).
FIG. 3[ (PM-ppy) 2 Ir(daf-Rh)]PF 6 NiO/ITO photocathode pair with different concentrations of Hg 2+ And photocurrent response and photocurrent of the (c).
FIG. 4[ (PM-ppy) 2 Ir(daf-Rh)]PF 6 NiO/ITO photocathode pair Hg 2+ Linear plot of concentration.
FIG. 5[ (PM-ppy) 2 Ir(daf-Rh)]PF 6 NiO/ITO photocathode pair Fe 3+ 、Ni 2+ 、Zn 2+ 、Al 3+ 、Mg 2+ 、Ag + 、Ba 2+ 、Cu 2+ 、Ca 2+ And (3) interfering with the selectivity experiment of the ions.
Detailed Description
The present invention will be further described with reference to examples, but it should be understood that the following description is only for the purpose of illustrating the invention and is not to be construed as limiting the invention.
1. The dye [ (PM-ppy) in the invention 2 Ir(daf-Rh)]PF 6 The preparation method of (2) comprises the following steps:
(1) Synthesis of rhodamine B hydrazide
Rhodamine B (2 g,4.2 mmol) was dissolved in ethanol (30 mL) and hydrazine hydrate (1.8 mL) was added dropwise. After 3h reflux, the mixture changed from dark purple to light orange and back to colorless. After cooling to room temperature, the mixture was poured into water (30 mL) and extracted with dichloromethane (3×30 mL). The organic phases were combined, dried over anhydrous sodium sulfate, filtered, and the solvent was removed under reduced pressure to give a pink solid product (1.83 g, yield 95%). 1 H NMR(CDCl 3 ,500MHz)δ:7.97–7.92(m,1H),7.43–7.47(m,2H),7.14–7.08(m,1H),6.47(d,J＝8.8Hz,2H),6.43(d,J＝2.4Hz,2H),6.30(dd,J＝8.8,2.4Hz,2H),3.62(s,2H),3.35(q,J＝7.0Hz,8H),1.17(t,J＝7.0Hz,12H).
(2) Synthesis of daf-h
A mixture of 4, 5-diazafluoren-9-one (0.36 g,1.99 mmol), rhodamine B hydrazide (0.91 g,1.99 mmol), phosphorus pentoxide (1.4 g,10.0 mmol), and methanol (20 mL) was heated at 65deg.C for 30 minutes. Cooled to room temperature and then poured into 30mL of water. The organic phases were combined by extraction with dichloromethane (3X 30 mL). Dried over anhydrous sodium sulfate, filtered, and the solvent was removed under reduced pressure. Isolation by column chromatography on silica gel (petroleum ether: ethyl acetate=5:4 (V: V)) afforded the product as a yellow solid (0.94 g, 76% yield).
(3) Synthesis of Daf-Rh
Daf-h (0.81 g,1.30 mmol) and L.complex reagent (0.52 g,1.30 mmol) were dissolved in dry toluene solution (20 mL) and stirred under nitrogen at 120deg.C for 8 hours. After cooling to room temperature, the mixture was poured into 200mL of water and the combined organic phases were extracted with 3×30mL of dichloromethane. The organic phase was washed with brine, dried over anhydrous sodium sulfate and filtered. The solvent was removed under reduced pressure. The crude product was separated by column chromatography on silica gel (eluent: petroleum ether: ethyl acetate=5:4) to give the product as a tan solid (0.58 g, 70% yield).
(4) Synthesis of PM-ppy
4- (2-pyridyl) benzaldehyde (480 mg,2.62 mmol) was dissolved in ethanol (30 mL), followed by addition of NaBH 4 (256 mg,6.92 mmol) was stirred at room temperature for 30 minutes, the solvent was removed under reduced pressure, the residue was dissolved in dichloromethane (30 mL) and water (100 mL), sodium carbonate (1.06 mg,10 mmol) was added, stirring was continued at room temperature for 30 minutes, and extraction was performed using dichloromethane. The combined organic phases were dried, filtered and evaporated under reduced pressure to give a viscous yellow oil (476 mg, 98% yield).
In an ice-water mixture at 0deg.C, the compound ppy-OH (470 mg,2.59 mmol) was dissolved in dichloromethane (30 mL) and 1.5mL of PBr was added dropwise 3 In the above mixed solution. Stir at room temperature overnight. After cooling to 0 ℃, a saturated aqueous sodium carbonate solution is added dropwise, and the temperature is kept below 5 ℃ during the addition. After the solution was made basic, the organic phase was separated and the aqueous phase was extracted with dichloromethane (3X 30 mL). The combined organic phases were then dried over anhydrous magnesium sulfate and the solvent was removed under reduced pressure to give the product as a white powder (430 mg, 67% yield).
The compound ppy-Br (186 mg,0.756 mmol) and triethyl phosphite (400. Mu.L, 2.25 mmol) were dissolved in chloroform (5 mL) and refluxed under nitrogen atmosphere at 80℃for 16 hours. The solvent was removed under reduced pressure, and the crude product was separated by silica gel column chromatography (eluent: ethyl acetate: methanol=10:1) to give PM-ppy as a pale yellow oil (144 mg, yield 63%). 1 H NMR(CDCl 3 ,500MHz)δ:8.69(d,J＝4.1Hz,1H),7.95(d,J＝7.9Hz,2H),7.78–7.71(m,2H),7.42(dd,J＝8.3,2.3Hz,2H),7.26–7.22(m,1H),4.07–4.00(m,4H),3.21(d,J＝21.8Hz,2H),1.25(t,J＝7.1Hz,6H)
(6)[(PM-ppy) 2 Ir(μ-Cl)] 2 Is synthesized by (a)
PM-ppy (470 mg,1.5 mmol) and IrCl 3 3H 2 O(246mg,0.70mmol) was dissolved in a 2-ethoxyethanol/water solution (3:1, 20 mL). The reaction mixture was heated to reflux at 130 ℃ under nitrogen atmosphere for 72 hours. Cooled to room temperature, the solvent was removed under reduced pressure to give CH 2 Cl 2 MeOH (10:1) as eluent, and silica gel column chromatography gave a dark red powder (382 mg, 61% yield). 1 H NMR(CDCl 3 ,500MHz)δ:9.18(d,J＝5.5Hz,4H),7.85(d,J＝8.1Hz,4H),7.76(t,J＝7.8Hz,4H),7.41(d,J＝7.9Hz,4H),6.78(t,J＝6.6Hz,4H),6.72(d,J＝7.9Hz,4H),5.72(s,4H),3.74–3.63(m,16H),2.73(dd,J＝21.7,10.8Hz,8H),0.96(t,J＝7.0Hz,12H),0.91(t,J＝7.0Hz,12H)
(7)[(PM-ppy) 2 Ir(daf-Rh)]PF 6 Is synthesized by (a)
Bridging the chlorine intermediate [ (PM-ppy) 2 Ir(μ-Cl)] 2 (60 mg,0.036 mmol) and daf-Rh (51 mg,0.079 mmol) were dissolved in CH 2 Cl 2 In suspension in MeOH (1:1, 20.0 mL) and the reaction mixture was heated at reflux under nitrogen for 14 h. After cooling the mixture to room temperature, NH dissolved in methanol (10 mL) was added 4 PF 6 (130 mg,0.80 mmol) and stirring was continued for 2 hours at room temperature. The solvent was depressurized and the residue was chromatographed on a silica gel column using CH 2 Cl 2 MeOH (10:1, V/V) as eluent gave a dark red powder (73 mg, 58% yield). 1 H NMR(CDCl 3 ,500MHz):δ9.06(d,J＝7.1Hz,1H),8.27(t,J＝7.1Hz,2H),7.91(t,J＝9.1Hz,2H),7.86–7.72(m,6H),7.69(d,J＝5.5Hz,1H),7.62(t,J＝8.1Hz,2H),7.58(d,J＝7.4Hz,1H),7.56–7.51(m,1H),7.49(dd,J＝7.6,5.5Hz,1H),7.18(d,J＝7.6Hz,1H),7.10(t,J＝6.5Hz,1H),7.05(t,J＝6.6Hz,1H),7.01(t,J＝8.7Hz,2H),6.73(t,J＝9.2Hz,2H),6.39–6.24(m,6H),3.95–3.77(m,8H),3.32(q,J＝6.9Hz,8H),2.95(dd,J＝21.8,9.6Hz,4H),1.16–1.10(m,18H),1.15(td,J＝7.1,2.6Hz,6H).ESI-HRMS:calcd.for C 71 H 74 IrN 8 O 7 P 2 S 1437.4524[M] + ；found 1437.4569[M] + 。
2、[(PM-ppy) 2 Ir(daf-Rh)]PF 6 Preparation of NiO/ITO photocathode
Fixing area of NiO/ITO electrode0.5 cm. Times.0.5 cm, then immersed in a solution containing [ (PM-ppy) 2 Ir(daf-Rh)]PF 6 (1 mM) in a centrifuge tube, immersing for 12 hours at ordinary temperature, and incubating [ (PM-ppy) 2 Ir(daf-Rh)]PF 6 Assembled to the NiO surface. The electrodes are sequentially made of DMF and CH 3 After CN washing, the mixture was dried in air to obtain [ (PM-ppy) 2 Ir(daf-Rh)]PF 6 /NiO/ITO。
3、[(PM-ppy) 2 Ir(daf-Rh)]PF 6 NiO/ITO photocathode pair Hg 2+ Is detected by (a)
[(PM-ppy) 2 Ir(daf-Rh)]PF 6 Sensitized NiO photocathode pair target Hg 2+ Will [ (PM-ppy) 2 Ir(daf-Rh)]PF 6 NiO/ITO photocathode is prepared by mixing Hg with different concentration 2+ The corresponding photocurrent response was recorded in PBS (0.1 m, ph=7.4) for evaluation. Along with Hg 2+ The photocurrent gradually increased due to the increase in Hg due to the increase in concentration 2+ The more, the stronger the absorbance and the better the subsequent sensitization. Increase in photocurrent intensity and Hg 2+ The concentration showed good linearity in the range of 0.01-1000nM, with a limit of detection (LOD) of 4.75pM, about 4 orders of magnitude higher than the iridium (III) complex fluorescent probe.

Claims (2)

1. Be used for detecting Hg 2+ The preparation method of the iridium (III) complex sensitized NiO photocathode, wherein the iridium (III) complex ([ (PM-ppy)) 2 Ir(daf-Rh)]PF 6 ) The structural formula is as follows:
the method comprises the following steps:
(1) Preparation of NiO modified ITO electrode: firstly, sequentially placing the ITO electrode with a fixed area into absolute ethyl alcohol, acetone, absolute ethyl alcohol and ultrapure water in sequence for cleaning and drying; the electrode is then immersed in a solution containing Ni (NO 3 ) 2 ·6H 2 Heating the mixed solution of O and hexamethylenetetramine in an electrothermal constant-temperature blast drying oven, and naturally cooling to room temperature; washing with ultrapure water, and naturally dryingThe method comprises the steps of carrying out a first treatment on the surface of the Finally, placing the ITO electrode in a muffle furnace for quenching to obtain a NiO modified electrode (NiO/ITO);
(2) Preparation of iridium (III) complex sensitized NiO photocathode: soaking the NiO/ITO electrode prepared in the step (1) in iridium (III) complex ([ (PM-ppy) 2 Ir(daf-Rh)]PF 6 ) The solution was stirred for 12 hours with DMF and CH in sequence as electrodes 3 After CN washing, natural drying to obtain iridium (III) complex sensitized NiO photocathode ([ (PM-ppy)) 2 Ir(daf-Rh)]PF 6 /NiO/ITO)；
(3)Hg 2+ Is detected: the photocathode [ (PM-ppy) prepared in the step (2) is subjected to 2 Ir(daf-Rh)]PF 6 Soaking NiO/ITO in a solution containing Hg at different concentrations 2+ In a buffer solution of (0.1M, pH=7.4) for 5 minutes, in [ (PM-ppy) 2 Ir(daf-Rh)]PF 6 Recording photocurrent by using NiO/ITO as a working electrode; the visible light is adopted for excitation, so that different concentrations of Hg can be realized 2+ Is provided.
2. Iridium (III) complex sensitized NiO photocathode prepared by the method according to claim 1 in Hg 2+ Application in detection.
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