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Holmium nitrilotriacetate complex used as cadmium ion fluorescent probe and preparation method thereof

A fluorescent probe, nitrilotriacetic acid technology, applied in the preparation of organic compounds, cyanide reaction preparation, fluorescence/phosphorescence, etc., to achieve good selective recognition effect

Active Publication Date: 2018-12-11
HENAN UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The invention relates to a holmium nitrilotriacetate complex used as a fluorescent probe for cadmium ions. When a certain amount of Cd is added 2+ ion, the fluorescence of the complex is significantly enhanced, with high sensitivity and selectivity, and has the characteristics of simple and quick operation, non-toxicity, environmental friendliness and high selectivity. 2+ Ionic fluorescent probes have not been reported in the literature

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  • Holmium nitrilotriacetate complex used as cadmium ion fluorescent probe and preparation method thereof
  • Holmium nitrilotriacetate complex used as cadmium ion fluorescent probe and preparation method thereof
  • Holmium nitrilotriacetate complex used as cadmium ion fluorescent probe and preparation method thereof

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Embodiment 1

[0021] The synthesis of embodiment 1 complex:

[0022] 0.2mmol of H 3 NTA and 0.6mmol Ho(NO 3 ) 3 .6H 2 O was dissolved in 10mL of water, the pH of the mixture was adjusted to 5, stirred at room temperature for 30 minutes, transferred to a 25mL polytetrafluoroethylene liner, and put into a reaction kettle, at 160°C The reaction was carried out at room temperature for 96 hours, cooled to room temperature naturally, and the obtained product was washed twice with anhydrous ether (1 mL / time) to obtain pale pink crystals with a yield of 66.1%.

Embodiment 2

[0023] Example 2 Structural characterization of complexes:

[0024] The crystal structure adopts Bruker Smart CCD X-ray single crystal diffractometer at 296(2)K, and the selected size is 0.49×0.41×0.32mm 3 crystals, using graphite monochromatized MoKα rays As the incident radiation source, the diffraction points were collected by ω / 2θ scanning, the unit cell parameters were refined by the least square method, and the collected data were corrected for absorption with the SADABS program. The structure of the complex was solved by the direct method, the coordinates of non-hydrogen atoms and the anisotropy temperature factor were refined by the full-matrix least-squares method, and all calculations were completed by the SHELXTL program. The detailed crystallographic parameters are listed in Table 1. Holmium nitrilotriacetate complex [Ho(NTA)(H 2 O)] n The crystal structure diagram, two-dimensional planar structure and three-dimensional pore structure of figure 1 , figure 2 a...

Embodiment 3

[0028] Example 3 Fluorescent properties of complexes:

[0029] Using the F-7000FL fluorescence spectrometer, the fluorescence properties of the complex were measured at room temperature, and the fluorescence spectrum of the complex in distilled aqueous solution is shown in Figure 4 As shown, the excitation light wavelength is 326nm, and the emission peak is located at 496nm. When Cd 2+ When the concentration of ions added is the same as that of the complex, the same as the complex blank sample (without adding Cd 2+ ions), the position of the emission peak of the complex does not shift (emission wavelength 496nm, excitation wavelength 326nm), but the intensity of the emission peak increases with the Cd 2+ Significantly enhanced by the addition of ions (the fluorescence intensity can be increased by about 5 times); same as the above experiment, adding Cu 2+ , Hg 2+ , Pb 2+ , Ca 2+ and Zn 2+ Compared with the fluorescence intensity of the complex blank sample, the fluores...

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Abstract

The invention discloses a nitrilotriacetic acid holmium complex used as a cadmium ion fluorescent probe and a preparation method thereof. The chemical formula of the complex is [Ho(NTA)(H2O)]n, wherein the NTA is nitrilotriacetic acid, and is of a two-dimensional plane structure; the distance between adjacent planes is 3.0 angstroms; the adjacent planes are constructed into a three-dimensional mesh structure through hydrogen bonds. When the nitrilotriacetic acid holmium complex is used as the cadmium ion fluorescent probe, the fluorescence emission peak intensity of the holmium complex is positively correlated with the concentration of Cd<2+> (the maximal enhancement extent can reach about 5 times, the emission wavelength is 496 nm, and the excitation wavelength is 326 nm), and the existence of the Cd<2+> cannot affect the position of the fluorescence emission peak of the nitrilotriacetic acid holmium complex; after Cu<2+>, Hg<2+>, Pb<2+>, Ca<2+> and Zn<2+> are respectively added, the emission peak position of the fluorescence intensity of the holmium complex does not displace and the intensity does not change greatly by comparing the fluorescence intensity of the holmium complex with the fluorescence intensity of a blank sample. The nitrilotriacetic acid holmium complex can be used as a fluorescent probe for the Cd<2+>, and has a potential application prospect in the fields of environment monitoring and life sciences.

Description

technical field [0001] The present invention relates to a kind of as cadmium ion (Cd 2+ ) a holmium nitrilotriacetate complex of a fluorescent probe and a preparation method thereof, the fluorescent probe has potential application prospects in the fields of environmental monitoring and life sciences. technical background [0002] Metal-carboxylic acid coordination polymers are complexes with highly regular and infinite network structures formed by self-assembly between organic ligands and metal ions. They have large specific surface areas and very high porosity. And the function tends to be diversified, and it has a wide range of applications in the fields of gas adsorption and separation, magnetic materials, biological activity, selective catalysis, molecular recognition, ion exchange, photoelectric materials [Zhou HC et al., Chem.Rev., 2(2012) 673]. This type of complex usually has a controllable microporous structure, which is one of the main reasons for its excellent f...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C229/76C07C227/18C09K11/06G01N21/64
CPCC07C227/18C07C229/76C09K11/06C09K2211/182G01N21/6428G01N21/6486
Inventor 杨立荣练晨刘流张怀敏邵彩云张武
Owner HENAN UNIVERSITY
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