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Chlorophenol graphene-based molecularly imprinted solid-phase extraction column and preparation method and application thereof

A solid-phase extraction cartridge, molecular imprinting technology, applied in separation methods, chemical instruments and methods, preparation of samples for testing, etc., can solve the problems of few polymer adsorption sites, single detection object, lack of application significance, etc. Achieve high selectivity and enrichment capacity, large adsorption capacity and strong selectivity

Inactive Publication Date: 2016-06-22
NINGBO MUNICIPAL CENT FOR DISEASE CONTROL & PREVENTION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The invention has the advantages of simple preparation process and good selectivity to 2,4,6-trichlorophenol, but the polymer is only specific to 2,4,6-trichlorophenol, and the detection object is single, while environmental water samples are generally simultaneously There are a variety of chlorophenol compounds, and a single solid-phase extraction material lacks practical application significance, and the polymer has fewer adsorption sites and poor enrichment efficiency, so it is not effective when applied to the detection of trace chlorophenol compounds. good

Method used

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  • Chlorophenol graphene-based molecularly imprinted solid-phase extraction column and preparation method and application thereof
  • Chlorophenol graphene-based molecularly imprinted solid-phase extraction column and preparation method and application thereof
  • Chlorophenol graphene-based molecularly imprinted solid-phase extraction column and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Preparation of chlorophenol graphene-based molecularly imprinted nanoparticles:

[0031] (1.1) Preparation of monodisperse core-shell magnetic polymer microspheres with high magnetic response: by solvothermal method, 2.5g FeCl 3 ·6H 2O, 80g ethylene glycol, 6.5g sodium acetate and 2.0g polyethylene glycol were mixed, stirred and dissolved at 50°C for 0.5h, then the mixed solution was added to a polytetrafluoroethylene autoclave and reacted at 200°C for 8h to obtain magnetic tetrafluoroethylene Ferric oxide microspheres. Then weigh 80 mg of magnetic ferric oxide microspheres, add 100 mL of acetonitrile to ultrasonically disperse for 0.5 h, then add 0.6 g of divinylbenzene (DVB), 0.6 g of glycidyl methacrylate (GMA) as polymerized monomers and 0.02 g of Nitroisobutyronitrile (ABIN) was used as an initiator to prepare monodisperse core-shell magnetic polymer microspheres with high magnetic response by precipitation polymerization at 80°C for 2 hours.

[0032] (1.2) ...

Embodiment 2

[0039] (1) Preparation of chlorophenol graphene-based molecularly imprinted nanoparticles:

[0040] (1.1) Preparation of monodisperse core-shell magnetic polymer microspheres with high magnetic response: using solvothermal method, 1.0g FeCl 3 ·6H 2 O, 80g ethylene glycol, 5g sodium acetate and 2.0g polyethylene glycol were mixed, stirred and dissolved at 50°C for 1h, then the mixed solution was added to a polytetrafluoroethylene autoclave and reacted at 200°C for 4h to obtain magnetic trioxide Iron microspheres. Then weigh 80 mg of magnetic ferric oxide microspheres, add 100 mL of acetonitrile to ultrasonically disperse for 0.5 h, then add 0.6 g of divinylbenzene (DVB), 0.6 g of glycidyl methacrylate (GMA) as polymerized monomers and 0.09 g of diisocyanate Azodiisobutyronitrile (ABIN) was used as an initiator to prepare monodisperse core-shell magnetic polymer microspheres with high magnetic response by precipitation polymerization at 80°C for 4.5 hours.

[0041] (1.2) Acti...

Embodiment 3

[0048] (1) Preparation of chlorophenol graphene-based molecularly imprinted nanoparticles:

[0049] (1.1) Preparation of monodisperse core-shell magnetic polymer microspheres with high magnetic response: using solvothermal method, 3.5g FeCl 3 ·6H 2 O, 70g of ethylene glycol, 6g of sodium acetate and 2.0g of polyethylene glycol were mixed, stirred and dissolved at 50°C for 0.5h, and then the mixed solution was added to a polytetrafluoroethylene autoclave at 200°C for 6h to obtain magnetic tetraoxide Tri-iron microspheres. Then weigh 70 mg of magnetic ferric oxide microspheres, add 100 mL of acetonitrile to ultrasonically disperse for 0.5 h, then add 0.6 g of divinylbenzene (DVB), 0.2 g of glycidyl methacrylate (GMA) as polymerized monomers and 0.08 g of diisocyanate Nitroisobutyronitrile (ABIN) was used as an initiator to prepare monodisperse core-shell magnetic polymer microspheres with high magnetic response by precipitation polymerization at 80°C for 3.5 hours.

[0050] (...

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Abstract

The invention relates to a chlorophenol graphene-based molecularly imprinted solid-phase extraction column, which comprises an empty column, a sieve plate and a filling material. The filling material is formed by mixing chlorophenol graphene molecularly imprinted nanoparticles and a conventional solid-phase extraction packing at the mass ratio of 1: 1-10. According to the chlorophenol graphene molecularly imprinted nanoparticles, a magnetic Fe3O4 high-molecular material is supported on the surface of graphene as a function unit, and a target chlorophenol compound to be adsorbed is used as template molecule. Meanwhile, the invention also relates to a preparation method and an application of the chlorophenol graphene-based molecularly imprinted solid-phase extraction column. The chlorophenol graphene-based molecularly imprinted solid-phase extraction column has large specific surface area, many adsorption sites, strong specific selectivity and good enrichment effect, can be used in enrichment of residual trace amount of chlorophenol compounds in an environmental water sample, and can achieve high enrichment factor and can remarkably reduce matrix effects. Meanwhile, the preparation method of the molecularly imprinted solid-phase extraction column is simple, technological conditions are stable, and production cost is low.

Description

technical field [0001] The invention relates to the technical field of environmental monitoring and treatment, in particular to a chlorophenol graphene-based molecularly imprinted solid-phase extraction column and a preparation method and application thereof. Background technique [0002] Chlorophenol compounds (such as: 2-chlorophenol, 2,4-dichlorophenol, 2,4,6-trichlorophenol and pentachlorophenol) are widely used in industries such as pesticides, medicines and synthetic materials, and are aromatic compounds A class of compounds with the widest application, the greatest toxicity and serious pollution. Because chlorophenols have a certain solubility in water, and because of their large octanol / water partition coefficient (lgKow is 2.17-5.01), they have obvious fat solubility and can accumulate in the biosphere through the food chain, thereby greatly exacerbating their toxicity. Pollution. Currently, chlorophenols have been detected in waste, sludge, sediment, soil, ground...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D15/20B01J20/26B01J20/30G01N1/34G01N1/40
Inventor 潘胜东金米聪陈晓红赵永纲
Owner NINGBO MUNICIPAL CENT FOR DISEASE CONTROL & PREVENTION
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