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Magnetic covalent organic framework nano material, preparation method and application

A covalent organic framework and nanomaterial technology, applied in the field of magnetic covalent organic framework nanomaterials and preparation, can solve problems such as human health risks, achieve excellent magnetic separation characteristics, simple and convenient operation, and high adsorption capacity

Active Publication Date: 2022-04-29
NORTHWEST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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  • Magnetic covalent organic framework nano material, preparation method and application
  • Magnetic covalent organic framework nano material, preparation method and application
  • Magnetic covalent organic framework nano material, preparation method and application

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preparation example Construction

[0036] A preparation method of a magnetic covalent organic framework nanomaterial disclosed by the present invention comprises the following steps:

[0037] Step 1, preparation of magnetic Fe 3 o 4 nanoparticles;

[0038] The specific preparation method of the present invention is preferably: FeCl 3 、6H 2 O, Na 3 Cit, 2H 2 O. Dissolve NaAc in ethylene glycol and stir for 20-50 minutes. Among them, FeCl 3 、6H 2 O, Na 3 Cit, 2H 2 The mass ratio of O and NaAc is 2~6:0.5~2:3~7; the resulting mixed solution is placed in an autoclave and reacted at 150°C~200°C for 8~12h, and the obtained product is washed and dried to obtain magnetic Fe 3 o 4 nanoparticles.

[0039] Step 2, the magnetic Fe 3 o 4 Nanoparticles dispersed in ethanol to obtain Fe 3 o 4 Dispersion, preferably, magnetic Fe 3 o 4 The mass of nanoparticles and the volume ratio of absolute ethanol is 0.1~1g:5~50mL; 2,5-dihydroxy terephthalaldehyde is dissolved in ethanol, preferably, 2,5-dihydroxy terephthal...

Embodiment 1

[0053] This embodiment discloses the preparation of a magnetic covalent organic framework nanomaterial, specifically:

[0054] Step 1, Magnetic Fe 3 o 4 Preparation of nanoparticles:

[0055] The raw materials are ferric chloride hexahydrate (FeCl 3 、6H 2 O) 3.4g, dehydrated sodium citrate (Na 3 Cit, 2H 2 O) 1.0 g and sodium acetate (NaAc) 6.0 g. The organic solvent used is ethylene glycol 100mL. FeCl 3 、6H 2 O, Na 3 Cit, 2H 2 O. NaAc was dissolved in ethylene glycol, stirred by ultrasonic to form a homogeneous yellow solution, then transferred to a stainless steel autoclave lined with polytetrafluoroethylene, and reacted at 200°C for 12 hours. The material was taken out, washed repeatedly with ethanol and water, dried at 25°C, and set aside.

[0056] Step 2, functionalization of COFs materials: take 0.5g of magnetic Fe prepared in step 1 3 o 4 Particles were ultrasonically dispersed in 25mL ethanol, 0.07g 2,5-dihydroxyterephthalaldehyde was ultrasonically dissol...

Embodiment 2

[0062] The difference between this embodiment and embodiment 1 is: in step 2, Fe 3 o 4 0.15g and 0.03g of 2,5-dihydroxyterephthalaldehyde.

[0063]The magnetic nanocomposite material Fe prepared in this embodiment 3 o 4 The topography of @COFs is similar to that of Example 1, and will not be given separately here.

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Abstract

The invention discloses a magnetic covalent organic framework nano-material, a preparation method and application, firstly, magnetic Fe3O4 nano-particles are prepared, then the magnetic Fe3O4 nano-particles and a 2, 5-dihydroxy terephthalaldehyde solution are mixed, stirring is conducted for 1-3 h at the temperature of 30-65 DEG C, and Fe3O4 nano-particles modified for the first time are obtained; and mixing the Fe3O4 nanoparticles modified for the first time, 1, 3, 5-tris (4-aminophenyl) benzene and 2, 5-dihydroxy terephthalaldehyde in the most week, adding an acetic acid solution, and stirring and reacting at room temperature to obtain the magnetic covalent organic framework nano material Fe3O4 (at) COFs. The magnetic covalent organic framework nano-material prepared by the invention not only has the excellent properties of large specific surface area, rich adsorption sites and the like of a covalent organic framework, but also inherits the excellent magnetic separation characteristic of a magnetic material, so that the composite material has the characteristics of high adsorption and separation speed and high adsorption capacity, can be repeatedly used for more than 6 times, and has a wide application prospect. And the removal efficiency of ethyl carbamate can still reach 88% or above.

Description

technical field [0001] The invention belongs to the technical field of food safety analysis, and in particular relates to a magnetic covalent organic framework nanomaterial, a preparation method and an application. Background technique [0002] A variety of sample pretreatment methods, such as liquid-liquid extraction, solid-phase extraction, and ultrasound-assisted microextraction, have been reported for the enrichment of target compounds in complex sample matrices. However, magnetic solid phase extraction (MSPE) is an important branch of solid phase extraction. MSPE has the advantages of fast adsorption and separation speed, less amount of adsorbent, and simple operation, and has received extensive attention. Therefore, the development of a magnetic solid phase extraction (MSPE) adsorbent capable of adsorbing ethyl carbamate facilitates the improvement of adsorption performance. [0003] Compared with other COFs, the imine-based COFs materials obtained by the dehydration...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/28G01N1/34G01N30/06B01J20/30
CPCB01J20/06B01J20/22B01J20/28009G01N1/34G01N30/06G01N2030/062
Inventor 盛庆林杨姝英周佳怡何靖怡岳田利
Owner NORTHWEST UNIV
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