Triazole molecularly imprinted polymeric microspheres and preparation method and application thereof

A technology of molecular imprinting and triazoles, which is applied to the preparation of alkali metal compounds, chemical instruments and methods, and test samples, 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: 2018-12-28
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • Triazole molecularly imprinted polymeric microspheres and preparation method and application thereof
  • Triazole molecularly imprinted polymeric microspheres and preparation method and application thereof
  • Triazole molecularly imprinted polymeric microspheres and preparation method and application thereof

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preparation example Construction

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

[0031] 1) Mixing the triazole compound template molecule, the functional monomer and the porogen, and performing self-assembly after ultrasonication in an oxygen-free environment to obtain a self-assembly mixed solution;

[0032] 2) mixing the self-assembly mixed solution obtained in step 1) with an acrylate-based crosslinking agent and an azo-based initiator, and then pre-polymerizing to obtain a pre-polymerization reaction solution; the temperature of the pre-polymerization is 20-40° C.;

[0033] 3) heating the prepolymerized reaction solution obtained in step 2) and performing 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-based compound template molecules in the polymer obtained in step 3) to obtain triazole-based molecul...

Embodiment 1

[0092] Add 0.2 mmol of triazolone, 0.6 mmol of methacrylic acid (MAA) and 50 mL of acetonitrile to a 100 mL borosilicate glass bottle in turn, mix well, and sonicate through N at 25°C. 2 After 10 min, it was placed in a constant temperature gas bath shaker at 25 °C for self-assembly for 10 h, and then 25 mg of azobisisobutyronitrile (AIBN) and 3 mmol of ethylene glycol dimethacrylate (EGDMA) were added, mixed uniformly, and passed through N 2 After 10 min, it was placed in a constant temperature water bath shaker at 25 °C for prepolymerization for 2 h, then the temperature was raised to 40 °C at 0.5 °C / min, and the polymerization was performed for 18 h. After the polymerization, let stand to room temperature, then separate the polymer with a high-speed centrifuge (rotation speed is 10000rpm), pour off the supernatant, put the polymer into a Soxhlet extractor after drying, and use methanol:acetic acid=6:1 (V / V) was repeatedly cycled as eluent to elute template molecules until n...

Embodiment 2

[0104] The MIPs obtained in Example 1 were used as solid-phase extraction fillers, and were applied to spiked tobacco leaves with triazolone, myclobutanil, tebuconazole, hexaconazole, diconazole, propiconazole, tricyclazole, and imine. azole and flusilazole recovery rate detection. 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 and place them in 10mL centrifuge tubes respectively, add 1mL of mixed standard solutions of 9 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 min to make it fully mixed, left standing at room temperature overnight, and then placed in 50° C. for vac...

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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. They are widely used in the control of diseases and insect pests of fruits, vegetables, rice, etc. . Phillips McDougall made statistics on the sales of the top 15 important fungicides in the world in 2015, including 5 kinds of triazole fungicides, which shows its important position. However, with the wide application of triazole pesticides, the problem of their residues in agricultural products and the environment has gradually attracted people's attention. [0003] Molecular imprinting technology refers to the preparation of a polymer synthetic material that can specifically recognize target molecules and their structural analogs. In recent years, this technology has b...

Claims

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Application Information

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Patent Type & Authority Applications(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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