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Metal-organic framework material for detecting mercury ions on basis of ratio fluorescence

An organic framework, ratiometric fluorescence technology, applied in luminescent materials, fluorescence/phosphorescence, material excitation analysis, etc., can solve the problems of limited probe structure design and synthesis, mercury ion probe urgent, and unfavorable widespread promotion and research, etc. The effect of easy large-scale preparation, low price and easy preparation

Inactive Publication Date: 2016-02-03
XUZHOU NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0005] 1. Most small molecule probes based on organic dyes are generally limited by their solubility and are suitable for organic solvent systems or organic / water mixed systems. Therefore, the development of probes that can detect mercury ions in pure water systems is still in the current research. needs improvement
[0006] 2. The mechanism of action of most highly selective mercury ion probes is not yet completely clear. Most of the known ones are designed using the mechanism of Hg-S reaction, which is limited by the design and synthesis of the probe structure, which is not conducive to practical significance Extensive research on
[0007] 3. Some of the reported probe materials are often limited by other heavy metal ions, such as Cd 2+ , Pb 2+ Interference to the recognition process, design and easy preparation of specificity are urgent for mercury ion probes, which are of great significance

Method used

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  • Metal-organic framework material for detecting mercury ions on basis of ratio fluorescence
  • Metal-organic framework material for detecting mercury ions on basis of ratio fluorescence
  • Metal-organic framework material for detecting mercury ions on basis of ratio fluorescence

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Example 1 (Synthesis of organic linker ligands)

[0032] Weigh 2.1g of dimethyl 5-hydroxyisophthalate and 3.3g of anhydrous potassium carbonate in a flask, add 40mL of acetonitrile, stir for a few minutes, slowly add 1.0g of 1,2-dibromoethane to the above system, and keep the temperature 80°C, react for 24 hours. Suction filtration, rotary evaporation, extraction with water and dichloromethane, drying with anhydrous sodium sulfate, rotary evaporation to obtain 5,5'-(ethane-1,2-disubstituted dioxo)diisophthalic acid di methyl ester.

[0033] Weigh 2.39g of 5,5'-(ethane-1,2-disubstituted dioxo)dimethyl diisophthalate and 0.65g of sodium hydroxide in a single-necked bottle, add 40mL of ethanol / water (v / v=4 / 1) mixed solvents, kept at a constant temperature of 80°C, and reacted for 4 hours under stirring. The above reaction solution was rotary evaporated, acidified with dilute hydrochloric acid, and washed with water after suction filtration to obtain a colorless solid...

Embodiment 2

[0034] Example 2 (Synthesis of Metal-Organic Frameworks)

[0035] Weigh 3.9 mg of 5,5'-(ethane-1,2-disubstituted dioxo)diisophthalic acid (H 4 EDDA ) (0.01mmol), 4.2mgCd(ClO 4 ) 2 ·6H 2 O (0.01mmol) in a 10mL glass sample vial, add 7mL of water as a solvent, then place the glass sample vial in a hydrothermal synthesis reaction kettle, and then place the hydrothermal synthesis reaction kettle in an electric blast drying oven at constant temperature 120°C, react for three days. After the reaction is over, cool to obtain colorless blocky crystals, filter, wash, and dry, which is the metal-organic framework material Cd– EDDA , whose three-dimensional structure is shown in figure 1 As shown, the yield: 80%. Cd 1.5 (C 18 h 10 o10 )?(H 2 O) 3 :C35.50;H2.65;O34.16.Found:C,35.55;H,2.45;N,34.21.

Embodiment 3

[0036] Example 3 (Material Stability Test)

[0037] Take by weighing 5 parts of material Cd in embodiment 2- EDDA , were added to aqueous solutions with pH values ​​of 2.0, 4.2, 7.0, 10.3, and 12.2, stirred for 24 hours, filtered, and tested for PXRD after vacuum drying at room temperature. The test results are shown in figure 2 shown.

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Abstract

The invention provides a method for realizing detection of mercury ions in pure water solution in a ratio fluorescence form on the basis of a metal-organic framework material. According to the method, 5,5minute-(ethane-1,2-disubstituted bis(oxy)) m-phthalic acid is used as a ligand, and takes a hydrothermal reaction with hexahydrate cadmium perchlorate to obtain a three-dimensional metal-organic framework material; the material has dual fluorescence emission functions, i.e., a fluorescence emission peak based on the ligand and a charge transfer emission peak based on ligand-metal ions charge transfer are respectively included; the detection of the mercury ions by the metal-organic framework material in the ratio fluorescence form can be realized; the specificity on the mercury ion detection in alkali metal, alkaline-earth metal, transition metal and other heavy metal ions is shown; through much characterization, the mechanism of the material on the mercury ion detection is specific. Therefore the material provides a method for mercury ion ratio fluorescence detection on the basis of the metal-organic framework material, and the method has the advantages that the sensitivity is high, and the operation is simple.

Description

technical field [0001] The invention relates to a metal-organic framework material for detecting mercury ions in an aqueous solution, in particular to a class of metal-organic framework materials for detecting mercury ions based on ratiometric fluorescence. Background technique [0002] As a global environmental pollutant, mercury has teratogenic and carcinogenic effects, and is an accumulative poison. The harm to the human body mainly involves the central nervous system, digestive system and kidneys. In addition, it also has certain effects on the respiratory system, skin, blood and eyes. The danger is serious. Therefore, it is of clinical and physiological significance to develop effective, highly sensitive and specific mercury ion probe materials. [0003] However, designing and synthesizing a detection technology with high selectivity and effective recognition of Hg ions is currently a very challenging subject. After decades of unremitting efforts by scientists, tradit...

Claims

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Application Information

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IPC IPC(8): C08G83/00C09K11/06G01N21/64
Inventor 王健李阳蒋敏史颖武鹏彦
Owner XUZHOU NORMAL UNIVERSITY
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