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Magnetic COF-TbPa for enrichment of triazole pesticide and preparing method and application of magnetic COF-TbPa

A technology for enriching triazoles and pesticides, applied in chemical instruments and methods, other chemical processes, ion exchange, etc., can solve the problems of harsh reaction conditions, poor stability, and inability to mass-produce, and achieves simple operation and reaction. Mild conditions, good enrichment effect

Inactive Publication Date: 2019-10-11
ZHEJIANG ACADEMY OF AGRICULTURE SCIENCES
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  • Abstract
  • Description
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Problems solved by technology

The whole process of solvothermal synthesis of COFs is carried out in a closed reaction vessel, which cannot be used for real-time observation and sampling research, and the yield is generally low
In addition, the solvothermal synthesis process of some COFs materials requires operations such as liquid nitrogen flash freezing and flame sealing (such as "Magnetic covalent organic framework material: Synthesis and application as a sorbent for polycyclic aromatic hydrocarbons", Xuexiang Shi, 2018), and there are special types of The synthesis of COFs materials such as triazine COFs needs to be reacted in high-temperature molten zinc chloride, and the reaction conditions are relatively harsh.
Therefore, the COF preparation method has harsh conditions and cannot be mass-produced, which hinders the wide application of COF materials.
In addition, covalent organic frameworks have poor stability and difficult separation, which further limit the application of covalent organic frameworks in the enrichment of triazole pesticide residues.

Method used

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  • Magnetic COF-TbPa for enrichment of triazole pesticide and preparing method and application of magnetic COF-TbPa
  • Magnetic COF-TbPa for enrichment of triazole pesticide and preparing method and application of magnetic COF-TbPa
  • Magnetic COF-TbPa for enrichment of triazole pesticide and preparing method and application of magnetic COF-TbPa

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preparation example Construction

[0022] The present invention provides a magnetic COF-TbPa for enriching triazole pesticides (COF is the abbreviation of covalent organic material, Tb is the English name of 1,3,5-tris(p-formylphenyl)benzene 1,3,5-Tris (p-formylphenyl) benzene abbreviation, Pa is the abbreviation of the English name p-Phenylenediamine of p-phenylenediamine) preparation method, comprises the steps:

[0023] (1) Mix 1,3,5-tris(p-formylphenyl)benzene, aminated magnetic beads and ethanol, and perform the first aldehyde-amine condensation reaction to obtain aldehyded magnetic beads;

[0024] (2) Add the solution of p-phenylenediamine to the dispersion of the formylated magnetic beads, then add the solution of 1,3,5-tris(p-formylphenyl)benzene, and then add dropwise aqueous acetic acid to carry out The second aldehyde-amine condensation reaction yields magnetic COF-TbPa for enrichment of triazole pesticides.

[0025] In the invention, 1,3,5-tris(p-formylphenyl)benzene, aminated magnetic beads and et...

Embodiment 1

[0054] Mix 0.13g of 1,3,5-tris(p-formylphenyl)benzene with 75mL of ethanol, and ultrasonically homogenize to obtain a solution of 1,3,5-tris(p-formylphenyl)benzene; aminate 0.5g Mix magnetic beads (with a particle size of 0.148~0.720μm) with 25mL ethanol, and ultrasonically uniformly obtain a dispersion of aminated magnetic beads; mix the solution of 1,3,5-tris(p-formylphenyl)benzene with aminated The bead dispersion was mixed and reacted at 50°C for 1.5 h; after the reaction, when the temperature dropped to room temperature, the formylated magnetic beads were separated by adding a magnet, then soaked and washed with ethanol for 3 times (50 mL each time), and washed The liquid becomes clear, and formaldehyde magnetic beads are obtained;

[0055] The formylated magnetic beads were mixed with 25mL mixed solvent (1,4-dioxane and trimethylbenzene were obtained by mixing in a ratio of 1:1 by volume), and ultrasonicated to obtain a dispersion of formylated magnetic beads ; 0.064g p...

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Abstract

The invention provides magnetic COF-TbPa for enrichment of triazole pesticide and a preparing method and application of the magnetic COF-TbPa, and belongs to the technical field of adsorption materials. The preparing method of the magnetic COF-TbPa comprises the following steps of (1) mixing 1,3,5-tris(p-formylphenyl)benzene, amination magnetic beads and ethyl alcohol, and carrying out a first aldimine condensation reaction to obtain formylation magnetic beads; (2) adding a solution of p-phenylenediamine into a dispersion solution of the formylation magnetic beads, then adding a solution of the 1,3,5-tris(p-formylphenyl)benzene, then dropwise adding an aqueous solution of acetic acid, and carrying out a second aldimine condensation reaction to obtain the magnetic COF-TbPa for enrichment ofthe triazole pesticide. The material obtained by means of the preparing method has excellent adsorbability on the triazole pesticide, is high in stability, has high superparamagnetism, and can be directly separated and recycled from a solution medium through magnetic separation; moreover, the preparing method is easy to operate, and the reaction condition is mild.

Description

technical field [0001] The invention relates to the technical field of adsorption materials, in particular to a magnetic COF-TbPa for enriching triazole pesticides, a preparation method and application thereof. Background technique [0002] Covalent Organic Frameworks (COFs for short) are a class of pure organic porous materials with ordered structures and controllable functions, which are connected by covalent bonds of light elements such as C, H, B, O, and N. It has many advantages such as highly ordered structure, large specific surface area, good chemical stability and thermal stability, and is mainly used in the fields of optoelectronics, catalysis, gas adsorption storage, and sensing. However, there are few reports on the application of covalent organic framework materials in the enrichment detection of pesticide residues, and there is no COF with good enrichment ability for triazole pesticide residues. [0003] The current common synthesis methods of COFs materials i...

Claims

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Application Information

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IPC IPC(8): B01J20/26B01J20/28C08G12/08B01D15/08B01J20/30
CPCB01D15/08B01J20/264B01J20/28009B01J20/28019C08G12/08
Inventor 齐沛沛王新全林祥萍王娇赵慧宇
Owner ZHEJIANG ACADEMY OF AGRICULTURE SCIENCES
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