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Magnetic fluorinated covalent organic framework material as well as preparation method and application thereof

A technology of covalent organic framework and fluorination, applied in material separation, analytical materials, instruments, etc., can solve the problems of insufficient extraction efficiency of nanoparticles, and achieve strong magnetic response, strong adsorption selectivity, and high separation and enrichment efficiency Effect

Active Publication Date: 2021-11-30
SHANDONG ANALYSIS & TEST CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

MSPE usually utilizes Fe 3 o 4 provides magnetism, however the Fe 3 o 4 The extraction efficiency of nanoparticles is not enough, so the need for Fe 3 o 4 Nanoparticles are modified, and externally modified materials play an important role in enhancing the enrichment efficiency

Method used

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  • Magnetic fluorinated covalent organic framework material as well as preparation method and application thereof
  • Magnetic fluorinated covalent organic framework material as well as preparation method and application thereof
  • Magnetic fluorinated covalent organic framework material as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Example 1 Preparation of Magnetic Fluorinated Covalent Organic Framework Materials:

[0039] Dissolve ferric chloride hexahydrate, trisodium citrate and urea in 30mL of water at a molar ratio of 1:2:3, stir and add 300mg of polyacrylamide, transfer the mixture to a reactor after 1h, react at 200°C for 12h, and react After the end, use an external magnetic field to separate the precipitate from the reaction medium, wash it repeatedly with water and ethanol, and dry to obtain carboxylated Fe 3 o 4 nanoparticles.

[0040] 30 mg carboxylated Fe 3 o 4 Nanoparticles were ultrasonically dispersed in 30 mL of acetonitrile, 0.24 mmol of 2,4,6-tris(4-aminophenyl)-1,3,5-triazine was added, and after shaking at room temperature for 6 h, 0.36 mmol of 2,3, 5,6-Tetrafluoro-p-benzaldehyde and 6 mL of 12 mmol / L acetic acid were shaken at room temperature for 24 hours, magnetically separated, washed repeatedly with acetonitrile, and dried to obtain a magnetic fluorinated covalent o...

Embodiment 2

[0044] Example 2 Optimization of pretreatment conditions using magnetic fluorinated covalent organic framework materials as magnetic solid phase extraction adsorbents:

[0045] Weigh 5 mg of magnetic fluorinated covalent organic framework material into a 50 mL glass bottle, add 25 mL of water and ultrasonically disperse evenly. Add 0.5mL of benzoylurea pesticides, shake and adsorb for a certain period of time, then magnetically separate, and discard the supernatant. Next, add an appropriate amount of desorbent, after ultrasonic desorption for a certain period of time, magnetically separate and collect the eluate. Finally, nitrogen was blown to dryness and reconstituted, and after filtering with a filter membrane, the samples were injected and analyzed by liquid chromatography-mass spectrometry.

[0046] Among them, the liquid chromatography separation adopts C18 chromatographic column (100mm×2.1mm, 2.6μm), the mobile phase is 5mmol / L ammonium acetate water (C) and acetonitr...

Embodiment 3

[0052] Example 3 Cyclic performance of magnetic fluorinated covalent organic frameworks as adsorbents for magnetic solid phase extraction

[0053] Under the optimal pretreatment conditions, using the operation process of Example 2, the magnetic fluorinated covalent organic framework material that completed the first magnetic solid phase extraction process was mixed with 10 mL of methanol and 10 mL of water in sequence, and after ultrasonication for 10 min, magnetic separation was performed. Complete material regeneration. Execute the operation process of embodiment 2, compare the recovery of benzoylurea pesticides after different adsorption-desorption cycles, the results are shown in Figure 5 . After 8 cycles of use, the recovery rate of benzoylurea pesticides did not fluctuate significantly, and remained at about 90%, which indicated that Fe 3 o 4 @TAPT-TFTA-COF not only has good adsorption for benzoylurea pesticides, but also has good stability and recycling performanc...

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Abstract

The invention provides a magnetic fluorinated covalent organic framework material and a preparation method and application thereof. The structural formula of the magnetic fluorinated covalent organic framework material is Fe3O4-coated TAPT-TFTA-COF, and the magnetic fluorinated covalent organic framework material is of a core-shell structure prepared by taking carboxylated Fe3O4 nanoparticles as a core and taking a covalent structure prepared from 2,4,6-tri(4-aminophenyl)-1,3,5-triazine and 2,3,5,6-tetrafluoroterephthalaldehyde as monomers through polycondensation, and the surface of the shell layer is in a sea urchin shape. The magnetic fluorinated covalent organic framework material disclosed by the invention is used for magnetic solid-phase extraction of benzoylurea pesticides, shows strong adsorption selectivity and high separation and enrichment efficiency, and has the remarkable advantages of being small in adsorbent dosage, short in extraction time, capable of being repeatedly used and capable of reducing the detection cost.

Description

technical field [0001] The application relates to the fields of nanomaterial preparation and pesticide residue detection, and specifically relates to a magnetic fluorinated covalent organic framework material and its preparation method and application. Background technique [0002] The information disclosed in this background section is only intended to increase the understanding of the general background of the application, and is not necessarily regarded as an acknowledgment or any form of suggestion that the information constitutes the prior art already known to those skilled in the art. [0003] Benzoylurea pesticides are insect growth regulators that can inhibit the synthesis of chitin in target insects, leading to their death or sterility. They are widely used in corn, cotton, soybeans, rice, wheat, vegetables, fruit trees and Pest control of tea and other crops. However, the extensive use of benzoylurea pesticides leads to their residues in the environment and plants...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G12/08C08K9/04C08K3/22G01N30/02G01N30/06G01N30/08G01N30/14G01N30/72
CPCC08G12/08C08K9/04C08K3/22G01N30/02G01N30/06G01N30/08G01N30/14G01N30/72C08K2003/2275G01N2030/027G01N2030/062G01N2030/146
Inventor 徐桂菊赵汝松候龙飞刘楚晴王晓利刘璐
Owner SHANDONG ANALYSIS & TEST CENT
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