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A kind of triazole molecularly imprinted polymer microsphere and its preparation method and application

A molecular imprinting and triazole technology, applied in alkali metal compounds, chemical instruments and methods, preparation of samples for testing, etc., can solve the problems of large polymer particle size and poor specific adsorption effect, and achieve particle size The effect of small size, single particle size distribution and good specific adsorption capacity

Active Publication Date: 2020-02-14
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the particle size of the polymer prepared by this method is relatively large, about 2 μm, and the specific adsorption effect is poor.

Method used

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  • A kind of triazole molecularly imprinted polymer microsphere and its preparation method and application
  • A kind of triazole molecularly imprinted polymer microsphere and its preparation method and application
  • A kind of triazole molecularly imprinted polymer microsphere and its preparation method and application

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preparation example Construction

[0030] The invention provides a method for preparing triazole molecularly imprinted polymer microspheres, comprising the following steps:

[0031] 1) After mixing the triazole compound template molecules, functional monomers and porogens, self-assembly is carried out after ultrasonication in an oxygen-free environment to obtain a self-assembly mixture;

[0032] 2) Prepolymerizing the self-assembly mixture liquid obtained in step 1) with an acrylate crosslinking agent and an azo initiator to obtain a prepolymerization reaction liquid; the temperature of the prepolymerization is 20-40° C.;

[0033] 3) The pre-polymerization reaction liquid obtained in step 2) is heated up to perform a polymerization reaction to obtain a polymer; the heating rate is 0.5-1.2°C / min, and the polymerization temperature is 35-60°C;

[0034] 4) eluting the triazole compound template molecules in the polymer obtained in step 3) to obtain triazole molecularly imprinted polymer microspheres;

[0035] The...

Embodiment 1

[0092] Add 0.2mmol triadimefon, 0.6mmol methacrylic acid (MAA) and 50mL acetonitrile in sequence to a 100mL borosilicate glass bottle, mix well, and ultrasonically pass through N at 25°C. 2 After 10 minutes, place in a constant temperature air bath shaker at 25°C for self-assembly for 10 hours, then add 25 mg of azobisisobutyronitrile (AIBN) and 3 mmol of ethylene glycol dimethacrylate (EGDMA), mix well, and pass through N 2 After 10 minutes, place in a constant temperature water bath shaker at 25°C for pre-polymerization for 2 hours, then raise the temperature to 40°C at a rate of 0.5°C / min, and polymerize for 18 hours. After the polymerization is over, let it stand to room temperature, then separate the polymer with a high-speed centrifuge (rotating speed is 10000rpm), pour off the supernatant, put it into a Soxhlet extractor after the polymer is dried, and use methanol:acetic acid=6:1 (V / V) was used as the eluent to repeatedly elute the template molecule until no triadimefo...

Embodiment 2

[0104] The MIPs obtained in Example 1 are used as solid-phase extraction fillers, and are applied to triadimefon, myclobutanil, tebuconazole, hexaconazole, diniconazole, propiconazole, tricyclazole, imine in spiked tobacco leaves Detection of recovery rate of azole and flusilazole. The specific process is:

[0105] 1) The tobacco leaf control sample was crushed with a high-speed multifunctional pulverizer for 1 min, passed through a 40-mesh sieve, and then transferred to a constant temperature vacuum drying oven at 50°C to dry to constant weight. Weigh several 1g samples of the above-mentioned dried tobacco leaves, place them in 10mL centrifuge tubes, add 1mL of mixed standard solutions of nine kinds of triazole fungicides with different concentrations of pesticide residues, and the spiked concentrations are 0.01, 0.05, 0.1, 0.5μg / g, and then vortexed for 5 minutes to make it fully mixed, left at room temperature overnight, and then placed in 50 ° C for 2 hours of vacuum dry...

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Abstract

The invention provides a preparation method of triazole molecularly imprinted polymeric microspheres and belongs to the technical field of molecularly imprinted polymers. The preparation method comprises the following steps that triazole compound template molecules, a functional monomer and a pore-foaming agent are mixed, then the mixture is subjected to ultrasound in an oxygen-free environment and then is self-assembled, the self-assembled mixed liquid is mixed with an acrylic cross-linking agent and an azo-initiator, the mixture is prepolymerized, and the obtained prepolymerized reaction liquid is heated and then performs polymerization reaction under the oscillation condition to obtain a polymer; the triazole compound template molecules in the obtained polymer are eluted to obtain the triazole molecularly imprinted polymeric microspheres. The prepared triazole molecularly imprinted polymeric microspheres are single in particle diameter and has good specific adsorption capacity to template molecules and their structural analogues.

Description

technical field [0001] The invention relates to the technical field of molecularly imprinted polymers, in particular to a triazole molecularly imprinted polymer microsphere and a preparation method thereof. Background technique [0002] Triazole fungicides refer to compounds containing 1,2,4-triazole rings, which are widely used in the control of diseases and insect pests such as fruits, vegetables, and rice due to their advantages of low toxicity, strong systemic absorption, and long-lasting effect . Phillips McDougall made statistics on the sales of the top 15 fungicides in the world in 2015, including 5 triazole fungicides, which shows its important position. However, with the widespread application of triazole pesticides, their residues in agricultural products and the environment have gradually attracted people's attention. [0003] Molecular imprinting technology refers to the technology of preparing a polymer synthetic material that can specifically recognize target...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F222/14C08F220/06C08J9/28B01J20/26B01J20/28B01J20/30G01N1/28
CPCB01J20/268B01J20/28021B01J20/3057C08F222/1006C08F222/102C08J9/28C08J2335/02G01N1/28C08F220/06
Inventor 顾丽莉李志君韩毅彭建陶军孔光辉师君丽吴玉萍
Owner KUNMING UNIV OF SCI & TECH
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