Molecularly imprinted polymeric microspheres for phenol, preparation method thereof and use thereof

A technology of molecular imprinting and polymers, which is applied in chemical instruments and methods, analytical materials, material separation, etc., can solve the problems of column efficiency reduction, chromatographic peak tailing, and influence on separation effect, and achieve fast selective adsorption speed and simple preparation , The effect of strong selective adsorption performance

Inactive Publication Date: 2009-12-30
RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Secondly, the use and selection of commonly used functional monomers, cross-linking agents and polymerization methods have relatively large limitations, so for specific template molecules, such as 2,4,6-trichlorophenol in the present invention, 2 , the imprinted polymer microspheres of 4-dichlorophenol or 4-chlorophenol molecules have not been reported in the prior art, which makes molecular imprinting technology far from meeting the needs of practical applications
[0013] At the same time, when the existing molecularly imprinted polymer microspheres are prepared, the polymeric precursor cannot be uniformly dispersed in the dispersant, so the particle size of the obtained polymer microspheres is not uniform. Therefore, when MIP is used as a high-performance liquid chromatography (HPLC) When the stationary phase detects the monomer to be tested, the chromatographic peak is often too broad and tailed, which reduces the column efficiency and affects the separation effect

Method used

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  • Molecularly imprinted polymeric microspheres for phenol, preparation method thereof and use thereof
  • Molecularly imprinted polymeric microspheres for phenol, preparation method thereof and use thereof
  • Molecularly imprinted polymeric microspheres for phenol, preparation method thereof and use thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0054] With 1 mole of 2,4,6-trichlorophenol as a template molecule and 4 moles of methacrylic acid as a functional monomer, dissolve in 4ml of acetonitrile solvent to obtain a mixed solution; add 2,4,6 - Divinylbenzene with 20 times the molar weight of trichlorophenol as a crosslinking agent and azobisisobutyronitrile with 0.66 times the molar weight of 2,4,6-trichlorophenol are mixed evenly as an initiator, and nitrogen deoxidation is carried out for 10 minutes to remove Oxygen dissolved in the mixed solution. Take 3mL of the above solution and add it into 12mL of liquid paraffin, mix well, and put it under the irradiation of ultraviolet light for polymerization reaction for 24 hours. The reaction mixture was centrifuged at 3500 rpm for 20 min, the supernatant was discarded, and the solid was extracted by Soxhlet with an acetonitrile-acetic acid mixed solution (90:10, v / v) until there was no 2,4,6-tris in the extraction solution. Chlorophenols were detected. Dry the obtaine...

Embodiment 2

[0060] With 1 mole of 2,4,6-trichlorophenol as a template molecule and 4 moles of 4-vinylpyridine as a functional monomer, dissolve in 4ml of acetonitrile solvent to obtain a mixed solution; add 2,4 , L-2-diacrylamido phenylpropanol acrylate with 20 times the molar amount of 6-trichlorophenol as crosslinking agent and azobisisobutyronitrile with 0.8 times the molar amount of 2,4,6-trichlorophenol as The initiators were mixed evenly, and nitrogen deoxidation was performed for 10 minutes to remove dissolved oxygen in the mixed solution. Take 3mL of the above solution and add it into 27mL of liquid paraffin, mix well, and put it under the irradiation of ultraviolet light for polymerization reaction for 24 hours. The reaction mixture was centrifuged at 3500 rpm for 20 min, the supernatant was discarded, and the solid was extracted by Soxhlet with an acetonitrile-acetic acid mixed solution (90:10, v / v) until there was no 2,4,6-tris in the extraction solution. Chlorophenols were de...

Embodiment 3

[0062]With 1 mole of 2,4,6-trichlorophenol as a template molecule and 6 moles of methacrylic acid as a functional monomer, dissolve in 4ml of propionitrile solvent to obtain a mixed solution; add 2,4, Ethylene glycol dimethacrylate of 30 times the molar weight of 6-trichlorophenol is used as crosslinking agent and azobisisobutyronitrile of 0.5 times the molar weight of 2,4,6-trichlorophenol is mixed uniformly as an initiator, and the Nitrogen deoxygenation for 10 minutes to remove dissolved oxygen in the mixed solution. Take 3mL of the above solution and add it into 18mL of liquid paraffin, mix well and put it under the irradiation of ultraviolet light for polymerization reaction for 24 hours. The reaction mixture was centrifuged at 3500 rpm for 20 min, the supernatant was discarded, and the solid was extracted by Soxhlet with an acetonitrile-acetic acid mixed solution (90:10, v / v) until there was no 2,4,6-tris in the extraction solution. Chlorophenols were detected. The obt...

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Abstract

The invention provides molecularly imprinted polymeric microspheres for phenol. The polymeric monomer of the polymeric microspheres is methacrylic acid or 4-vinylpyridine and the specific surface area of the polymeric microspheres is 23.08-62.33m<2>/g. The invention also provides a method for preparing the polymeric microspheres and the use of the polymeric microspheres in collection or detection of phenol compounds. In addition, the invention also provides a chromatographic column and a solid phase extraction cartridge filler. The filler is the molecularly imprinted polymeric microspheres. The molecularly imprinted polymeric microspheres are simple and convenient in preparation, have an adsorption selectivity of 8.25 to 44.55 mg/g, reach a balance within 6 hours and have the advantages of high absorption selectivity and high absorption speed.

Description

technical field [0001] The invention relates to a molecularly imprinted polymer microsphere for phenol, its preparation method and application. The invention belongs to the technical field of environmental monitoring and processing. Background technique [0002] Molecularly imprinted polymers (molecularly imprinted polymer, MIP) is a technology in which under the action of a cross-linking agent, template molecules and functional monomers produce chemoselective bonding sites. The substrate to be tested is identified by conforming to the template molecular polymer in terms of shape, size and positioning of functional groups. MIP can be combined with analytical techniques such as liquid chromatography, capillary electrophoresis, capillary electrochromatography, and solid phase extraction. In recent years, the application of highly selective MIPs in the analysis of pharmaceutical, biochemical and environmental samples has become a booming new topic. [0003] Molecularly impri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/06C08F226/06C08F2/44C08J9/26G01N30/08B01J20/281B01D11/02
Inventor 林金明冯钦忠赵利霞郭宝元
Owner RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI
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