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Boric acid type magnetic COFs (covalent organic frameworks) material, preparation method and application

A magnetic and boric acid technology, applied in the field of separation technology and functional material preparation, to achieve the effects of good selectivity, large adsorption capacity and improved separation efficiency

Active Publication Date: 2019-01-25
NORTHWEST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, as far as the inventors know, it has not been reported that boric acid-type monomers are bonded to the COFs substrate to prepare boric acid-type magnetic COFs materials

Method used

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  • Boric acid type magnetic COFs (covalent organic frameworks) material, preparation method and application
  • Boric acid type magnetic COFs (covalent organic frameworks) material, preparation method and application
  • Boric acid type magnetic COFs (covalent organic frameworks) material, preparation method and application

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preparation example Construction

[0037] The preparation method of the above-mentioned boric acid type magnetic COFs material comprises the following steps:

[0038] (1) Synthesis of Fe by solvothermal method 3 o 4 Nanoparticles, washed repeatedly with ethanol and distilled water for later use;

[0039] (2) Amination of the surface of the solid phase matrix: the Fe 3 o 4 Nanoparticles were reacted with tetraethyl orthosilicate (TEOS) dispersed in absolute ethanol to obtain Fe 3 o 4 @SiO 2 , and then heated to reflux with 3-aminopropyltriethoxysilane (APTES) in anhydrous toluene, washed and dried to obtain Fe 3 o 4 @SiO 2 -NH 2 ;

[0040] (3) Functionalization of the surface of the solid-phase matrix: the solid-phase matrix Fe 3 o 4 @SiO 2 -NH 2 Schiff base reaction with monomer 1,3,5-triformylphloroglucinol (Tp) to give Tp-functionalized Fe 3 o 4 -Tp;

[0041] (4) In situ growth synthesis of core-shell Fe 3 o 4 @TpBD(NO 2 ) 2 Nanoparticles: Optimizing the solvent conditions for synthesis, ...

Embodiment 1

[0047] According to literature [1] Synthesis of 1,3,5-triformylphloroglucinol (Tp)

[0048] Synthetic Magnetic Fe 3 o 4 Nanoparticles:

[0049] Weigh 1.35g FeCl 3 ·6H 2 Add O and 0.45g sodium citrate into 30mL ethylene glycol, ultrasonically disperse for 5min, then heat to dissolve; cool to room temperature, add 2.4g sodium acetate, add magnets, and magnetically stir for 30min; add the above mixture into the reaction kettle , heated and reacted at 200°C for 12h; cooled to room temperature, the product was separated with a magnet, and washed alternately with water and ethanol three times.

[0050] Synthesis of amino-functionalized magnetic silica nanoparticles (Fe 3 o 4 @SiO 2 -NH 2 ):

[0051] (1) 864mgFe 3 o 4 After the nanoparticles were washed with distilled water, 1M HCl, distilled water, and 20% sodium citrate in sequence, the particles were dispersed in 144mL distilled water, transferred to a 1000mL three-neck flask, 600mL absolute ethanol was added, ultrason...

Embodiment 2

[0062] Example 2: Selective adsorption of cis-ortho-dihydroxy species by boric acid-type magnetic COFs materials

[0063] With NH at pH=9.0 3 -NH 4 Cl buffer (containing sodium metabisulfite 2g / L) was used to prepare a mixed solution of 5.0 μg / mL dopamine and 5-hydroxytryptamine (interfering substance), catechol and hydroquinone (interfering substance), and 5 mL of dopamine and 5 - Add the mixed solution of serotonin, catechol and hydroquinone into a centrifuge tube containing 10.0 mg of boron affinity adsorbent, and disperse it ultrasonically, shake and adsorb on a constant temperature shaker for 1 h, and then use NH of pH=9.0 3 -NH 4 Rinse with Cl buffer, rinse with water, and finally wash with 1.0mL 5% H 2 After the O-HAc eluent was eluted for 30 min, the eluate was collected, passed through a membrane, and detected by reverse-phase high-performance liquid chromatography (HPLC-UV). Figure 9 It shows that the material has good adsorption selectivity to substances contai...

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Abstract

The invention discloses a boric acid type magnetic COFs (covalent organic frameworks) material, a preparation method and application. The boric acid type magnetic COFs material comprises nanoparticleswith core-shell structures, wherein a core is an Fe3O4 nanoparticle; a shell is COFs; the COFs are modified by boric acid groups, so as to obtain the boric acid type magnetic COFs material. The preparation method comprises the following steps of synthesizing the core-shell Fe3O4@TpBD(NO2)2 nanoparticle by a solvent thermal method via in situ growth, and modifying the function groups on a surfaceby a monomer containing phenylboronic acid groups, so as to obtain the novel boric acid type magnetic COFs material. The separation material has the characteristics that the adsorption capacity is high, and the stability and selectivity are good;material, can be used for the separation and enrichment and content analysis of a trace monoamine type neurotransmitter substance in urine, the interference of a complicated matrix can be eliminated, and the separation and enrichment efficiency is improved.

Description

technical field [0001] The invention belongs to the field of separation technology and preparation of functional materials, and relates to a boric acid type magnetic COFs material, a preparation method and an application thereof. Background technique [0002] Covalent organic frameworks (COFs) are emerging porous organic materials, which have many advantages such as permanent porosity, low density, large specific surface area, good stability, tunable pore size and structure, etc. These excellent properties make COFs materials have excellent potential in various application fields. [0003] Magnetic solid-phase extraction (MSPE) based on magnetic or magnetically modified adsorbents has been developed into one of the promising techniques in enrichment and separation. The development of new functionalized and efficient adsorbents is the key to MSPE technology. It is of great significance to introduce COFs into magnetic nanoparticles to construct new nanocomposites with increa...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/28B01J20/30B01D15/08
CPCB01D15/08B01J20/226B01J20/28009B01J20/30
Inventor 王超展王延萍吴少平申纪伟卫引茂
Owner NORTHWEST UNIV
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