Organic-inorganic heteropolyacid-based rare earth derivative as well as preparation method and application thereof

A derivative and organic technology, applied in the field of preparation of polyacid-based fluorescent probe materials, can solve the problems of low water solubility and limit metal ions, and achieve the effect of preventing hydrolysis

Active Publication Date: 2019-06-07
HENAN UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the low water solubility of organic molecules, its application as a fluorescent probe material to detect metal ions in aqueous solution is limited to a certain extent.

Method used

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  • Organic-inorganic heteropolyacid-based rare earth derivative as well as preparation method and application thereof
  • Organic-inorganic heteropolyacid-based rare earth derivative as well as preparation method and application thereof
  • Organic-inorganic heteropolyacid-based rare earth derivative as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] An example of organic-inorganic hybrid multi-acid-based rare earth derivatives, the molecular formula of the multi-acid-based rare earth derivatives is [N(CH 3 ) 4 ] 3 K 2 [Eu(C 7 h 5 o 3 )(H 2 O) 2 (α-PW 11 o 39 )]·7H 2 O.

[0035] The preparation method of the above-mentioned organic-inorganic hybrid polyacid-based rare earth derivatives specifically comprises the following steps:

[0036] 1) EuCl 3 ∙6H 2 O (0.228 g, 0.600 mmol), ligand p-hydroxybenzoic acid (0.280 g, 0.200 mmol), polyacid precursor K 14 [P 2 W 19 o 69 (H 2 O)]∙24H 2 Add O (2.120 g, 0.465 mmol) into 30 mL of distilled water, stir until completely dissolved, adjust the pH value to 4.5±0.2 with 3 mol / L KOH aqueous solution, and stir at room temperature for 25 min;

[0037] 2) Put the solution obtained in step 1) into a water bath at 60°C, stir and heat for 2 hours, then add tetramethylammonium chloride (0.110 g, 1.000 mmol) while it is hot and stir for 25 minutes. After the reaction i...

Embodiment 2

[0045] Detect the solution concentration of compound 1 at the optimum fluorescence intensity:

[0046] 1) Compound 1 was formulated to a concentration of 1.0±0.1×10 -2 mol / L, 7.5±0.1×10 -3 mol / L, 5.0±0.1×10 -3 mol / L, 2.5±0.1×10 -3 mol / L, 1.0±0.1×10 -3 mol / L, 7.5±0.1×10 -4 mol / L, 5.0±0.1×10 -4 mol / L, 2.5±0.1×10 -4 mol / L, 1.0±0.1×10 -4 mol / L, 7.5±0.1×10 -5 mol / L, 5.0±0.1×10 -5 mol / L, 2.5±0.1×10 -5 mol / L, 1.0±0.1×10 -5 mol / L solution;

[0047] 2) The concentration of test compound 1 is 1.0±0.1×10 -3 Fluorescence emission spectrum and fluorescence excitation spectrum at mol / L, to determine the characteristic excitation peak and emission peak of compound 1, and optimize the detection conditions;

[0048] 3) Under the same test conditions, the test concentration is 1.0±0.1×10 -2 mol / L, 7.5±0.1×10 -3 mol / L, 5.0±0.1×10 -3 mol / L, 2.5±0.1×10 -3 mol / L, 1.0±0.1×10 -3 mol / L, 7.5±0.1×10 -4 mol / L, 5.0±0.1×10 -4 mol / L, 2.5±0.1×10 -4 mol / L, 1.0±0.1×10 -4 mol / L, 7.5±0.1×10...

Embodiment 3

[0052] Take 2.0 mL with a concentration of 7.5±0.1×10 -4 The mol / L compound 1 solution was placed in a quartz cuvette, and its time-resolved spectrum was tested under the excitation light of 330nm. The results are shown in Figure 9 .

[0053] Figure 9 The concentration of compound 1 solution is 7.5±0.1×10 -4 Time-resolved spectra under 330nm excitation light at mol / L. It can be seen from the figure that at 108 μs, a strong fluorescence emission peak at 440 nm is attributed to the fluorescence emission of the p-hydroxybenzoic acid ligand; at 112 μs, weak fluorescence emission peaks at 592 and 619 nm are attributed to Eu 3+ Characteristic fluorescence emission of ions; weak fluorescence emission peaks at 580, 650 and 700 nm at 115 μs are also attributed to Eu 3+ The characteristic fluorescence emission of the ion; the fluorescence emission of the p-hydroxybenzoic acid ligand gradually decreases with time, and the Eu 3+ The fluorescence emission of the ion's characteristic...

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Abstract

The invention belongs to the technical field of preparation of polyacid-based fluorescent probe materials and provides an organic-inorganic heteropolyacid-based rare earth derivative. The molecular formula of the heteropolyacid-based rare earth derivative is [N(CH3)4]3K2[Eu(C7H5O3)(H2O)2(alpha-PW11O39)]7H2O. The preparation method comprises the following steps: proportionally mixing EuCl3.6H2O, ap-hydroxybenzoic acid ligand and a polyacid precursor K14[P2W19O69(H2O)]24H2O, dissolving the mixture in water, and performing a reaction under a water bath condition. The fluorescent emission behavior of the polyacid-based rare earth derivative in a water solution is explored, and it is found that organic ligands in the material can effectively absorb energy and sensitize Eu <3+> ions to emit light. In addition, the fluorescence emission behavior of the polyacid-based rare earth derivative in Cr <3+> metal ion water solutions with different concentrations is detected, and the phenomenon of fluorescence intensity quenching is found. The polyacid-based rare earth derivative can be used as a fluorescent probe material to detect the concentration of Cr <3+> metal ions in an aqueous solution.

Description

technical field [0001] The invention belongs to the technical field of preparation of polyacid-based fluorescent probe materials, and specifically relates to an organic-inorganic hybrid polyacid-based rare earth derivative, a preparation method and its use as a fluorescent probe and in detecting metal Cr in water. 3+ Applications in ion concentration. Background technique [0002] Heavy metal elements (such as: Pb 2+ , Hg 2+ , Cr 3+ etc.) have been widely used in industrial production and life, however, heavy metal pollution has become an increasingly severe challenge facing countries all over the world, especially the pollution of drinking water and irrigation water, leading to a series of foreseeable and unforeseen diseases The occurrence of serious threat to human life safety (see A.Gaeta, R. C. Hider, Br. J. Pharmacol. 2005, 146, 1041‒1059). For example: chromium is widely used in leather manufacturing, paint processing, steel manufacturing and other industrial fiel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/06G01N21/64
Inventor 马鹏涛武贺臣陈寒寒王敬平牛景杨
Owner HENAN UNIVERSITY
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