Method for preparing cyhalothrin molecular imprinting polymer microspheres

A technology of cyhalothrin and molecular imprinting, which is applied to the preparation of microspheres, microcapsule preparations, chemical instruments and methods, etc., can solve the problems of poor binding performance, irregular imprinted polymer particles, etc., and achieve easy operation and uniformity Good, easy to control the reaction conditions

Inactive Publication Date: 2011-05-25
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to provide a method for preparing cyhalothrin molecularly imprinted polymer microspheres, so as to solve the problems of irregularity and poor binding properties of the imprinted polymer particles ...

Method used

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  • Method for preparing cyhalothrin molecular imprinting polymer microspheres
  • Method for preparing cyhalothrin molecular imprinting polymer microspheres
  • Method for preparing cyhalothrin molecular imprinting polymer microspheres

Examples

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Embodiment 1

[0026] Example 1. A preparation method of cyhalothrin molecularly imprinted polymer microspheres, followed by the following steps:

[0027] Weigh 0.5mmol of cyhalothrin (as a template molecule) into a 150mL round bottom flask, dissolve it with 50mL of acetonitrile / toluene=3:1 (v / v), add 2mmol of acrylic acid (AA), mix well and shake Let stand for 1h at room temperature. Then add 10mmol of cross-linking agent DVB and 0.44mmol of initiator AIBN and mix well to obtain a mixed solution. First, the mixed solution was ultrasonically degassed (ultrasonic frequency 40KHz) for 10 minutes, and then placed on an ice water bath at 0-4°C, bubbling with nitrogen to remove oxygen for 10 minutes, strictly sealed and placed in a constant temperature oscillator for 24 hours (60°C, 50rpm). After the reaction was stopped, the polymer with white precipitate was collected by centrifugation (10000rpm, 15min), and the white precipitated polymer was re-dispersed in 50mL of methanol / acetic acid=9:1 (v / v)...

Embodiment 2

[0037] Example 2. A method for preparing cyhalothrin molecularly imprinted polymer microspheres, followed by the following steps:

[0038] Weigh 0.5mmol of cyfluthrin into a 150mL round bottom flask, dissolve it with 50mL of acetonitrile / toluene=3:1 (v / v), add 2mmol of 2-hydroxyethyl-methacrylate (HEMA), and mix After shaking evenly, let it stand for 1h. Then add 10mmol of cross-linking agent DVB and 0.44mmol of initiator AIBN and mix well to obtain a mixed solution. First, the mixed solution was ultrasonically degassed for 10 minutes, and then placed on an ice water bath at 0-4°C to bubbling nitrogen to remove oxygen for 10 minutes. After strict sealing, it was placed in a constant temperature oscillator to react for 24 hours (60°C, 50rpm). After the reaction was stopped, the polymer with white precipitate was collected by centrifugation (10000rpm, 15min), and the white precipitated polymer was re-dispersed in 50mL of methanol / acetic acid=9:1 (v / v) extract to obtain the polymer...

Embodiment 3

[0044] Embodiment 3. A method for preparing cyhalothrin molecularly imprinted polymer microspheres, followed by the following steps:

[0045] Weigh 0.5 mmol of cyhalothrin and place it in a 150 mL round bottom flask, dissolve it with 50 mL of acetonitrile / toluene = 3:1 (v / v), add 2 mmol of methacrylic acid (MAA), mix and shake, and then stand for 1 hour. Then add 10mmol of crosslinking agent DVB and 0.44mmol of initiator AIBN and mix well to obtain a mixed solution. First, the mixed solution was ultrasonically degassed for 10 minutes, and then placed on an ice water bath at 0-4°C to bubbling with nitrogen to remove oxygen for 10 minutes. After strict sealing, it was placed in a constant temperature oscillator for 24 hours (60°C, 50rpm). After the reaction was stopped, the polymer with white precipitate was collected by centrifugation (10000rpm, 15min), and the white precipitated polymer was re-dispersed in 50mL of methanol / acetic acid=9:1 (v / v) extract to obtain the polymer susp...

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Abstract

The invention discloses a method for preparing cyhalothrin molecular imprinting polymer microspheres, which comprises the following steps of: 1) dissolving cyhalothrin and functional monomer serving as template molecules into a pore forming solvent; 2) adding cross linker and initiator into the obtained solution, introducing nitrogen to remove oxygen and sealing, and then placing the solution in an oscillator for heating reaction; 3) centrifuging the obtained reaction product, and re-dispersing the collected polymer in an extract in a volume ratio of methanol to acetic acid of 8.5-9.5: 1; 4) ultrasonically extracting the polymer suspension, centrifuging, and repeatedly washing and centrifuging the obtained sediment in turn; and 5) washing the template molecule-free polymer obtained in the step 4) to be neutral by using methanol, performing suction-filtration, and performing vacuum drying to obtain the cyhalothrin molecular imprinting polymer microspheres. The polymer microspheres obtained by the method have good selective identification function and high bonding capacity for the cyhalothrin.

Description

Technical field [0001] The invention relates to a method for directly preparing cyhalothrin molecularly imprinted polymer microspheres by a precipitation method. Background technique [0002] Cyhalothrin (trade name: Lambda-cyhalothrin) is (S)-alcohol-(Z)-1R-cis-acid and (R)-alcohol-(Z)-1S-cis-acid [1: 1] The mixture, as a typical second-generation pyrethroid pesticide, has the characteristics of fast insecticidal action, long lasting period, high efficiency, low toxicity and low residue. It is the current domestic and foreign agricultural and forestry insecticide and acaricide One of the main varieties. It is mainly used for contact killing and stomach poisoning. It has permeability and no systemic effect. It can effectively control Lepidoptera, Hemiptera, Coleoptera and mites. However, it has high resistance to fish and shrimp and other aquatic animals, silkworms and bees. poison. So far, there have been some reports on the toxicity of cyfluthrin. For example, studies have s...

Claims

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Application Information

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IPC IPC(8): C08F212/36C08F220/06C08F220/28C08F220/56C08F2/06C08J9/28C08J9/26B01J13/14B01J20/285B01J20/30
Inventor 梁晓郭逸蓉王阳阳桂文君刘毅华朱国念
Owner ZHEJIANG UNIV
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