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Polystyrene mercury ion fluorescence recognition materials and preparation method thereof

A polystyrene and fluorescence recognition technology, applied in the fields of luminescent materials, fluorescence/phosphorescence, material excitation analysis, etc., can solve the problems of fluorescent recognition materials that can only be detected but cannot be separated, fluorescence quenching signal amplification, and detection materials that cannot be reused.

Inactive Publication Date: 2015-08-19
NANHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a functionalized polystyrene Hg 2+ Fluorescence identification material solves the problems in the prior art that the fluorescence identification material can only be detected but not separated; the detection material cannot be reused and the fluorescence quenching signal is amplified

Method used

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  • Polystyrene mercury ion fluorescence recognition materials and preparation method thereof
  • Polystyrene mercury ion fluorescence recognition materials and preparation method thereof
  • Polystyrene mercury ion fluorescence recognition materials and preparation method thereof

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preparation example Construction

[0037] The invention provides a functionalized polystyrene Hg 2+ The preparation method of the fluorescent recognition material is specifically implemented according to the following steps:

[0038] Step 1, preparation of amino-2-(4'-hydroxyl-3'-(di-(2"-ethylthioethyl)amino)phenyl-benzo[d]oxazole (BOS, VII), the specific The synthetic route is shown in the following formula 1 - formula 4

[0039]

[0040] Specifically follow the steps below:

[0041] Step 1.1, the preparation of two-(2-ethylthioethyl)amine (Ⅲ)

[0042] Add diethanolamine (Compound I) into chloroform, slowly add thionyl chloride at -5°C-5°C, wherein the molar volume ratio (mol / ml) of diethanolamine to chloroform is 1:500-1:700 ; The molar ratio of diethanolamine to thionyl chloride is 1:3-1:5; After reacting at room temperature for 1.5h-2.5h, heat up to reflux for 2.5h-3.5h, cool, add ethanol to the reaction solution to remove excess Thionyl chloride. The solvent was distilled off under reduced pressure...

Embodiment 1

[0069] A functionalized polystyrene Hg 2+ The preparation method of the fluorescent recognition material is specifically implemented according to the following steps:

[0070] Step 1, preparation of 5-amino-2-(4'-hydroxyl-3'-(two-(2"-ethylthioethyl) amino)phenyl-5-aminobenzo[d]oxazole (BOS, VII);

[0071] A. Preparation of Di-(2-Ethylthioethyl)amine (Ⅲ)

[0072] Add 5.25g (0.05mol) of di-ethanolamine compound 1 into 30mL of chloroform, slowly add 23.8g of thionyl chloride at 0°C, react at room temperature for 2.0h, heat up to reflux for 3h, cool, and add Ethanol removes excess thionyl chloride. The solvent was distilled off under reduced pressure, and then a small amount of chloroform and diethyl ether were added to produce a white solid. After suction filtration, the solid was washed several times with diethyl ether and dried in vacuo to obtain 8.4 g of a white solid, i.e., di-(2-chloroethyl)amine salt acid salt, the yield was 95.2%.

[0073] Under the protection of nitr...

Embodiment 2

[0090] Step 1, preparation of amino-2-(4'-hydroxyl-3'-(two-(2"-ethylthioethyl) amino)phenyl-benzo[d]oxazole (BOS, VII), specifically according to The following steps are implemented:

[0091] Step 1.1, the preparation of di-(2-ethylthioethyl)amine (Ⅲ), specifically: adding diethanolamine (compound I) into chloroform, slowly adding thionyl chloride at -5°C-5°C , wherein, the molar volume ratio (mol / ml) of diethanolamine and chloroform is 1:500; The molar ratio of diethanolamine and thionyl chloride is 1:3; After reacting at room temperature for 2.5h, heat up to reflux reaction for 3.5h, cool , Ethanol was added to the reaction solution to remove excess thionyl chloride. Remove the solvent by distillation under reduced pressure, then add chloroform and diethyl ether, the molar volume ratio (mol / mL / mL) of diethanolamine, chloroform and diethyl ether is 1:40:120, a white solid is produced, suction filtered, and the solid is washed several times with diethyl ether , and dried in ...

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Abstract

The invention discloses polystyrene mercury ion fluorescence recognition materials. The structural formula of the polystyrene mercury ion fluorescence recognition materials is as follows. The invention also discloses a preparation method of the functionalized polystyrene mercury ion fluorescence recognition materials. The preparation method comprises the following specific implementation steps of, preparing 5-amino-2-(4'-hydroxy-3'-(2-(2''-ethylsuleenyl ethyl) amino) phenyl-5-amino benzo [d] oxazole (VII), preparing aldehyde polystyrene microspheres (IX) and performing reaction preparation on the compounds (VII) and (IX) obtained through preparation to obtain the functionalized polystyrene mercury ion fluorescence recognition materials (X). The detection sensitivity of the polystyrene mercury ion fluorescence recognition materials is greatly improved due to the molecular wire effect of a polymer and the detection limit is 0.006 micromole every liter. The polystyrene mercury ion fluorescence recognition materials can enter cells and can be applied to the detection on mercury ions in the cells.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, in particular to a polystyrene Hg 2+ Fluorescence recognition material, the present invention also relates to a kind of polystyrene Hg 2+ A method for preparing a fluorescent recognition material. Background technique [0002] Heavy metal ions can enter the human body through the food chain and other channels, and accumulate in the human body to cause great harm to human health. especially Hg 2+ It is a carcinogen, and its extremely low concentration can cause organ lesions such as kidneys and digestive system. Therefore, the detection and pollution control of heavy gold ions, such as Pb 2+ , Cd 2+ , Hg 2+ , Cu 2+ , Ag + etc. are the hotspots of current research. Fluorescence detection technology is widely used in chemical detection, biological imaging, drug screening and antibody detection due to its advantages of high sensitivity, good selectivity, simple operation, suitabilit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/06C08F12/08C08F8/34C08F8/26C08F8/24G01N21/64
Inventor 王宏青罗傲恒王榆元黄乔张勤
Owner NANHUA UNIV
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