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Preparation method of amino-modified molecularly imprinted material of coumarin rodenticide

A coumarin-based, molecularly imprinted technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problem of high selectivity of molecularly imprinted polymers without molecularly imprinted polymers, no reports of molecularly imprinted polymers in literature, and weak enrichment ability. and other problems, to achieve the effect of strong selectivity, simple preparation process and controllable functional group ratio

Inactive Publication Date: 2014-06-11
NINGBO MUNICIPAL CENT FOR DISEASE CONTROL & PREVENTION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Regarding the enrichment and purification of coumarin rodenticides, literatures mainly use polymeric resins such as GDX101, GDX201, GDX301, GDX403, GDX501, and XAD-2 (Tan Jiayi, Jiang Zhaolin, Wu Yuhong. Journal of Analytical Science, 1999, 15, 229.) and mixed Oasis HLB solid-phase extraction cartridges (M.C Jin, X.H Chen, Y. Zhu. J. Chromatogr. A, 2007, 1155: 57), etc., but these enrichment materials do not have molecular Imprinted polymers have specific high selectivity and weak enrichment ability, so their application is limited to a certain extent
However, the preparation of molecularly imprinted polymers for coumarin rodenticides has not been reported in the literature.

Method used

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  • Preparation method of amino-modified molecularly imprinted material of coumarin rodenticide
  • Preparation method of amino-modified molecularly imprinted material of coumarin rodenticide
  • Preparation method of amino-modified molecularly imprinted material of coumarin rodenticide

Examples

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preparation example Construction

[0020] The preparation method of the amino-modified molecularly imprinted material of the coumarin rodenticide of the present invention comprises the following steps:

[0021] 1. Preparation of monodisperse polymer composite microspheres rich in epoxy groups: monodisperse polymer composite microspheres with high epoxy functional group content were prepared by suspension polymerization.

[0022] This step is specifically: successively measure 1.0-20.0mL epoxy functionalized monomer, 2.0-10.0mL polymerized monomer, 0-4.0mL crosslinking agent, and add them to 50.0-500.0mL dispersant, 60 Ultrasonic dispersion at ℃ for 1.0-10.0 minutes; then add 0.5-5.0g initiator, at 60-90℃, stirring speed is 300-900 rpm, mechanical stirring at constant temperature and speed, after reaction for 0.5-5.0 hours, wash with ethanol Several times until the pH is 6-8, and vacuum-dried at 30-90° C. for 1-24 hours to prepare monodisperse polymer composite microspheres rich in epoxy groups.

[0023] The di...

Embodiment 1

[0031](1) Weigh 2.0g of polyvinyl alcohol 217 in 500.0mL of ultrapure water, heat to dissolve, and use it as a dispersant; polymerize monomer methyl methacrylate (4.0mL), functional monomer methacrylic acid to shrink Glyceride (4.0 mL) and cross-linking agent divinylbenzene (2.0 mL) were sequentially added dropwise to the reaction system under stirring, and ultrasonically dispersed at 60°C for 5.0 minutes to make the reaction system evenly dispersed. Dissolve 1.0g of permethoxybenzoyl permethoxybenzoyl initiator in 20.0mL of hot ethanol solution, add it dropwise to the above reaction system at 80°C and 800 rpm, react at constant temperature and speed for 3.0 hours, successively use Washed several times with ultrapure water and ethanol, and vacuum dried at 60°C for 12 hours to prepare epoxy-functionalized polymer composite microspheres.

[0032] (2) Weigh 2.0g of template molecules and 10.0mL of amino functional reagents respectively, and add them to 100.0mL of methanol reactio...

Embodiment 2-16

[0035] Its operating steps are the same as in Example 1, and the raw material, raw material formula and preparation condition parameters of Examples 1-16 are shown in Table 1.

[0036] Table 1: Raw material components and preparation parameters of Examples 1-16 of the present invention

[0037]

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Abstract

The invention discloses a preparation method of an amino-functionalized molecularly imprinted composite material of coumarin rodenticides. According to the invention, a dispersant is dissolved in hot water; a polymerization monomer, a functional monomer, and a cross-linking agent are added into the water, and the mixture is subjected to ultrasonic dispersing; an initiator is added into the mixture, the mixture is heated, and the mixture is stirred for carrying out a reaction, such that monodisperse polymer composite microspheres rich in epoxy groups are obtained; the material is washed until a pH is 6-8, and is dried; a composite reaction liquid of template molecules and an amino-functionalization reagent is added to the obtained material; the mixture is heated, and the mixture is stirred for carrying out a reaction, such that an amino-functionalized molecularly imprinted composite material bonded with the template molecules is obtained; the material is washed until the pH is 6-8, and is dried; the template molecules are removed by ultrasonic elution, such that the target product is obtained. The method provided by the invention is characterized by simple preparation process, controllable functional group proportion, and the like. The material can be used for enriching residual trace-amount coumarin rodenticides in environmental water samples so as to purify the environmental water sample, and can reach a relatively high enriching multiple.

Description

technical field [0001] The invention relates to a preparation method of an amino-functional molecular imprinted composite material with a core-shell structure, in particular to a preparation method of an amino-modified molecular imprinted material of a coumarin rodenticide. Background technique [0002] In recent years, chlorowarfarin [chemical name: 3-(α-p-chlorophenyl-β-acetylethyl)-4-hydroxycoumarin] and warfarin [chemical name: 3-(1-acetonyl Benzyl)-4-hydroxycoumarin], as the first generation of anticoagulant rodenticide, is still popularized and used in many places because of its high efficiency, broad spectrum, and good palatability. At the same time, the extensive use of rat poison has caused varying degrees of surface water pollution, but there is still a lack of efficient and selective enrichment and purification methods for coumarin-based rodenticides such as chlorowarfarin and warfarin . In view of this, the research on the enrichment and purification technology...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/14C08F212/08C08F220/32C08F212/36C08F222/38C08F2/20C08F8/32C08J9/26B01J20/26B01J20/30
Inventor 金米聪陈晓红赵永纲
Owner NINGBO MUNICIPAL CENT FOR DISEASE CONTROL & PREVENTION