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Magnetic covalent organic framework material, and preparation method and application thereof in detection of perfluorinated compounds

A covalent organic framework and magnetic technology, applied in the field of environmental inspection, can solve the problems of low separation efficiency of PFCs, long preparation time, harsh reaction conditions, etc., and achieve the effects of rapid enrichment and separation, simple synthesis steps, and mild reaction conditions.

Inactive Publication Date: 2020-05-08
QILU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the inventors of the present invention found that the current magnetic adsorption materials have defects such as long preparation time, harsh reaction conditions, and low separation efficiency for PFCs.

Method used

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  • Magnetic covalent organic framework material, and preparation method and application thereof in detection of perfluorinated compounds
  • Magnetic covalent organic framework material, and preparation method and application thereof in detection of perfluorinated compounds
  • Magnetic covalent organic framework material, and preparation method and application thereof in detection of perfluorinated compounds

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Embodiment approach

[0053] The third embodiment of the present invention provides an application of the above-mentioned magnetic covalent organic framework material for detecting perfluorinated compounds.

[0054] In one or more examples of this embodiment, the perfluoro compound is PFBS (perfluorobutane sulfonate), PFHpA (perfluoroheptanoic acid), PFOA, PFHxS (perfluorohexyl sulfonic acid), PFNA (Perfluorononanoic acid), PFDA (perfluorodecanoic acid), PFOS, PFUdA (perfluoroundecanoic acid), PFDoA (perfluorododecanoic acid).

[0055] The fourth embodiment of the present invention provides a method for enriching perfluorinated compounds in wastewater. The magnetic covalent organic framework material is added to wastewater containing perfluorinated compounds, and after shaking for a period of time, hysteresis separation is performed , The separated magnetic covalent organic framework material is eluted.

[0056] In one or more embodiments of this embodiment, the eluent is methanol, ethanol, acetone or ac...

Embodiment 1

[0062] Synthesis of 2,5-bis(2-(2-azidoethoxy)ethoxy)-1,4-phthalaldehyde.

[0063] (1) Add 2-(2-chloroethoxy)ethanol (4g, 32mmol), deionized water (20mL) to a 50mL round-bottom flask, and then add sodium azide (5.2g, 80mmol, 2.5eq). Stir at 80°C for 18 hours under nitrogen protection, then pour into 35 mL sodium hydroxide solution (5% (W / V)) and extract with ethyl acetate (3×35 mL). The organic phase was dried with anhydrous sodium sulfate and spin-dried to obtain 2-(2-azidoethoxy)ethanol as an oil.

[0064] (2) Under the protection of nitrogen, add 2-(2-azidoethoxy)ethanol (2g, 15.3mmol) and dry dichloromethane (20mL) to a 100mL round bottom flask, and then add to the above solution Add triethylamine (2.7mL, 18.4mmol, 1.5eq), cool to 0°C, add p-toluenesulfonyl chloride (3.48g, 18.4mmol, 1.2eq). The reaction mixture was stirred at 0°C for 1 hour, warmed to room temperature and stirred for 17 hours until the reaction was complete. Then it was washed with sodium bicarbonate soluti...

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Abstract

The invention discloses a magnetic covalent organic framework material, and a preparation method and application thereof in detection of perfluorinated compounds. The preparation method comprises thesteps: taking 1,3,5-tri(4-aminophenyl)benzene, terephthalaldehyde and a terephthalaldehyde intermediate as raw materials, and performing covalent linkage on the surfaces of ferroferric oxide nanoparticles under the catalytic action of acetic acid to obtain a covalent organic framework material precursor layer containing azido; reducing the azido of the covalent organic framework material precursorlayer into a primary amine group to generate a magnetic covalent organic framework material containing the primary amine group, wherein the terephthalaldehyde intermediate is terephthalaldehyde of which a benzene ring is connected with the azido through a chemical bond. The magnetic covalent organic framework material provided by the invention can be quickly synthesized at room temperature, and efficient separation and enrichment of PFCs are realized in a magnetic solid-phase extraction manner.

Description

Technical field [0001] The invention relates to a magnetic covalent organic frame material, a preparation method and application for detecting perfluorinated compounds, and belongs to the technical field of environmental inspection. Background technique [0002] Disclosure of the background information is only intended to increase the understanding of the overall background of the present invention, and is not necessarily regarded as an acknowledgement or in any form suggesting that the information constitutes the prior art known to those of ordinary skill in the art. [0003] Perfluorinated compounds (PFCs) refer to a class of fluorine-containing chemicals formed by replacing all hydrogen atoms connected to all or more of the carbon atoms in the carbon chain of aliphatic hydrocarbons by fluorine atoms. It has good thermal and chemical stability, can resist photolysis, hydrolysis, OH radical oxidation and biodegradation, has significant environmental persistence, and has a strong b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/28C02F1/28G01N30/02B01J20/30
CPCB01J20/226B01J20/28009C02F1/285G01N30/02
Inventor 王磊磊卢元月赵汝松王晓利王霞高永超
Owner QILU UNIV OF TECH
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