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A class of metal-organic frameworks based on ratiometric fluorescence detection of mercury ions

An organic framework and ratiometric fluorescence technology, which is applied in the fields of luminescent materials, fluorescence/phosphorescence, material excitation analysis, etc., can solve the problems of restricted probe structure design and synthesis, mercury ion probes are urgent, and are not conducive to extensive promotion and research. Ease of large-scale preparation, low cost, and easy-to-prepare effects

Inactive Publication Date: 2018-06-08
XUZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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, so 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 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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  • A class of metal-organic frameworks based on ratiometric fluorescence detection of mercury ions
  • A class of metal-organic frameworks based on ratiometric fluorescence detection of mercury ions
  • A class of metal-organic frameworks based on ratiometric fluorescence detection of mercury ions

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Example 1 (Synthesis of organic linking ligand)

[0032] Weigh 2.1 g of dimethyl 5-hydroxyisophthalate and 3.3 g of anhydrous potassium carbonate in the flask, add 40 mL of acetonitrile, stir for a few minutes, and slowly add 1.0 g of 1,2-dibromoethyl to the above system. Alkane, constant temperature 80 ℃, reaction 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 Methyl ester.

[0033] Weigh 2.39 g of 5,5'-(ethane-1,2-disubstituted dioxo) dimethyl isophthalate and 0.65 g of sodium hydroxide into a single-necked flask, add 40 mL of ethanol / water (v / v=4 / 1) Mixed solvent, constant temperature of 80°C, reaction for 4 hours under stirring. Rotate the above reaction liquid, acidify with dilute hydrochloric acid, filter with suction and wash with water to obtain a colorless solid, which is dried to obtain the t...

Embodiment 2

[0034] Example 2 (Synthesis of metal-organic framework materials)

[0035] Weigh 3.9 mg 5,5'-(ethane-1,2-disubstituted dioxo)diisophthalic acid (H 4 EDDA) (0.01mmol), 4.2 mg Cd(ClO 4 ) 2 ·6H 2 O (0.01 mmol) is placed in a 10 mL glass sample bottle, and 7 mL of water is added as a solvent. Then the glass sample bottle is placed in a hydrothermal synthesis reactor, and then the hydrothermal synthesis reactor is placed in an electric blast drying box , Constant temperature 120 ℃, reaction for three days. After the reaction is over, it is cooled to obtain colorless massive crystals, filtered, washed, and dried, which is the metal-organic framework material Cd-EDDA. Its three-dimensional structure is shown in figure 1 As shown, the yield: 80%. Cd 1.5 (C 18 H 10 O 10 )·(H 2 O) 3 :C 35.50; H 2.65; O 34.16. Found: C, 35.55; H, 2.45; N, 34.21.

Embodiment 3

[0036] Example 3 (Stability test of materials)

[0037] Weigh 5 parts of the material Cd-EDDA in Example 2 and add them to the aqueous solutions with pH values ​​of 2.0, 4.2, 7.0, 10.3 and 12.2, stir for 24 hours, filter, and vacuum dry at room temperature and test their PXRD respectively. Test results see 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 type of metal-organic framework material based on ratio fluorescence detection of mercury ions. Background technique [0002] As a global environmental pollutant, mercury has teratogenic and carcinogenic effects and is a cumulative 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 harm is serious. Therefore, the development of effective, highly sensitive and specific mercury ion probe materials has clinical and physiological and medical significance. [0003] However, designing and synthesizing a detection technology with high selectivity and effective identification of mercury ions is currently a very challenging subject. After decades of unremitting efforts by scientists, tradi...

Claims

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Application Information

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