Preparation method and application of ZnS quantum dot silica-based surface molecular imprinting sensor

A technology of surface molecular imprinting and quantum dots, which is applied in the direction of material excitation analysis, fluorescence/phosphorescence, etc., can solve the problems of long reaction time, complicated operation, poor selectivity, etc., achieve the improvement of sensitivity and selectivity, increase the reaction rate, and benefit The effect of desorption and recombination

Inactive Publication Date: 2014-12-24
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The purpose of the present invention is to overcome the defects of complex detection of 2,4-dichlorophenol existing in the prior art, long reaction time, poor selectivity, etc., and to provide a preparation method and application of a ZnS quantum dot silicon-based surface molecularly imprinted phosphorescent sensor

Method used

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  • Preparation method and application of ZnS quantum dot silica-based surface molecular imprinting sensor
  • Preparation method and application of ZnS quantum dot silica-based surface molecular imprinting sensor
  • Preparation method and application of ZnS quantum dot silica-based surface molecular imprinting sensor

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Embodiment 1

[0036] (1) In a 500 mL flask, add 100 mL of ethanol, 40 mL of deionized water and 15 mL of ammonia water. After vigorous magnetic stirring, add 10 mL of tetraethyl orthosilicate (TEOS), and stir for 2 h, the reaction produces SiO 2 , washed and precipitated, centrifuged, vacuum dried, and set aside. Take 1 g of SiO prepared above 2 Put it into a 100ml flask, add 45 mL of toluene, ultrasonically disperse, then add 1 mL of 3-(methacryloyloxy)propyltrimethoxysilane (KH570) dropwise under constant stirring, and heat up to 85 o C reflux for 20 hours. Centrifuge to get KH570 modified SiO 2 , washed with ethanol and dried for later use.

[0037] (2) In a 100 mL three-neck flask, add 1.797 g ZnSO 4 ·7H 2 O, 0.059 g MnCl 2 4H 2 O, add distilled water until completely dissolved, the resulting mixed solution was stirred at room temperature for 15 min under nitrogen, then added 5 mL containing 1.501 g Na 2 S·9H 2 O in water and stirred for 18 hours. Centrifuge to obtain Mn-dope...

Embodiment 2

[0041] (1) In a 500 mL flask, add 120 mL of ethanol, 60 mL of deionized water and 25 mL of ammonia water. After vigorous magnetic stirring, add 10 mL of tetraethyl orthosilicate (TEOS), and stir at room temperature for 2 h. SiO produced by reaction 2 , washed and precipitated, centrifuged, vacuum dried, and set aside. Take 1 g of SiO prepared above 2 Add 55 mL of toluene to a 100 mL flask, ultrasonically disperse, then add 3 mL of 3-(methacryloyloxy)propyltrimethoxysilane (KH570) dropwise under constant stirring, and heat up to 95 o C reflux for 28 hours. Centrifuge to get KH570 modified SiO 2 , washed with ethanol and dried for later use.

[0042] (2) In a 100 mL three-neck flask, add 1.797 g ZnSO 4 ·7H 2 O, 0.118 g MnCl 2 4H 2 O, add distilled water until completely dissolved, the resulting mixed solution was stirred at room temperature for 30 min under nitrogen, then added 5 mL containing 1.501 g Na 2 S·9H 2 O in water and stirred for 24 hours. Centrifuge to obt...

Embodiment 3

[0046] (1) In a 500 mL flask, add 110 mL of ethanol, 50 mL of deionized water and 20 mL of ammonia water. After vigorous magnetic stirring, add 10 mL of tetraethyl orthosilicate (TEOS), and stir at room temperature for 2 h. SiO produced by reaction 2 , washed and precipitated, centrifuged, vacuum dried, and set aside. Take 1 g of SiO prepared above 2 Add 50 mL of toluene to a 100 mL flask, ultrasonically disperse, then add 2 mL of 3-(methacryloyloxy)propyltrimethoxysilane (KH570) dropwise under constant stirring, and heat up to 90 o C reflux for 24 hours. Centrifuge to get KH570 modified SiO 2 , washed with ethanol and dried for later use.

[0047] (2) In a 100 mL three-neck flask, add 1.797 g ZnSO 4 ·7H 2 O, 0.1 g MnCl 24H 2 O, add distilled water until completely dissolved, the resulting mixed solution was stirred at room temperature for 20 min under nitrogen, then added 5 mL containing 1.501 g Na 2 S·9H 2 O in water, stirred for 20 hours. Centrifuge to obtain Mn...

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Abstract

The invention provides a preparation method and application of a ZnS quantum dot silica-based surface molecular imprinting sensor, belonging to the technical field of environmental function material preparation. The preparation method comprises the following steps: hydrolyzing silicon tetraacetate in a mixed solution of alkaline ethanol and water to prepare SiO2, and meanwhile adding a water solution of sodium sulphide hydrate in the water solution of zinc sulfate heptahydrate and tetrahydrate manganese chloride to prepare Mn-ZnS quantum dot; then respectively performing vinyl modification on the obtained SiO2 and Mn-ZnS quantum dot by using 3-methacryloxypropyltrimethoxysilane; and synthesizing the quantum dot phosphorescence surface molecular imprinting polymer through a precipitation polymerization method by using 2,4-dichlorophenol as a template molecule, acrylamide as functional monomer, Mn-ZnS-KH570 as an auxiliary monomer, SiO2-KH570 as a host material, ethylene dimethacrylate as a cross-linking agent, 2,2'-azobis(2-methylpropionitrile) as an initiator, and acetonitrile as solvent. The prepared phosphorescence surface molecular imprinting polymer has good optical and pH stability and has the capability of selectively recognizing 2,4-dichlorophenol.

Description

technical field [0001] The invention relates to a preparation method and application of a ZnS quantum dot silicon-based surface molecularly imprinted phosphorescence sensor, which belongs to the technical field of environmental functional material preparation. Background technique [0002] Molecular imprinting technology (MIT) is an emerging polymerization technology that can specifically recognize a specific molecule in recent years. The polymers prepared by this method are called molecularly imprinted polymers (Molecularly imprinted polymers). , MIPs). The preparation method is generally that when there is a template molecule in the system, the functional monomer can be polymerized to fix the template molecule in a complementary manner in the presence of a cross-linking agent. After the polymerization, the template molecules can be removed, so in this process, the "snapshot" of the system changes can be "taken" or recorded, so that the obtained molecular assembly can ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/64
Inventor 卫潇郝桐帆李洪吉徐叶青高林周志平闫永胜
Owner JIANGSU UNIV
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