Magnetic ordered mesoporous carbon-based or polymer-based core-shell structural microsphere and preparation method thereof

A polymer-based, core-shell structure technology, applied in the preparation of microspheres, microcapsule preparations, chemical instruments and methods, etc., can solve the problems of poor dispersion of composite materials, disordered pore distribution, and poor magnetic response effects. Achieve the effects of controllable hydrophilicity and hydrophobicity, simple and rapid method, and strong magnetic response

Active Publication Date: 2019-08-02
FUDAN UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0004] However, so far, the synthesis of core-shell nanocomposite microspheres with magnetic nanoparticles as the core and ordered mesoporous polymer framework or carbon framework as the shell has been rarely reported.
The currently synthe

Method used

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  • Magnetic ordered mesoporous carbon-based or polymer-based core-shell structural microsphere and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Evenly disperse 100 mg of magnetic iron ferric oxide particles with a particle size of about 50 nm in 80 mL of ethanol, 40 mL of deionized water and 1 mL of concentrated ammonia water (28 wt%), add 0.3 g of tetraethyl orthosilicate (TEOS), stirred magnetically at room temperature for 8 h, and obtained magnetic composite microspheres with a layer of silicon dioxide deposited on the surface. The product was separated by a magnet and washed with a mixed solution of ethanol and water. After washing, the product was dried at room temperature before use;

[0028] (2) Ultrasonic disperse the magnetic ferroferric oxide composite microspheres deposited with a layer of dense silica on the surface in a mixed solvent containing 50 mL ethanol, 50 mL deionized water, and 1 g F127, and then 1.0 mL1,3 , 5-Trimethylbenzene (TMB) was ultrasonically dispersed into the above solution, and then 1.0 g of dopamine hydrochloride was added to it, stirred for 20 min to make the solution unifo...

Embodiment 2

[0031] (1) Disperse 100 mg of magnetic γ-iron sesquioxide particles with a particle size of about 200 nm in 60 mL of ethanol, 60 mL of deionized water and 1 mL of concentrated ammonia water (28 wt%), and add 0.25 g of orthosilicate Ethyl ester (TEOS), magnetically stirred at room temperature for 8 hours to obtain a magnetic composite microsphere with a layer of silicon dioxide deposited on the surface, the product was separated by a magnet and washed with a mixed solution of ethanol and water, and the product was dried at room temperature after washing and then used;

[0032] (2) Ultrasonic disperse the magnetic Fe3O4 composite microspheres deposited with a layer of dense silica on the surface in a solution containing 40 mL ethanol, 80 mL deionized water, 40 mL tetrahydrofuran, 1 g PEO- b -PS (M n = 26544 g mol −1 ), then 0.6 mL of 1,3,5-trimethylbenzene (TMB) was ultrasonically dispersed into the above solution, and then 0.6 g of dopamine hydrochloride was added to it, stir...

Embodiment 3

[0035] (1) 100 mg magnetic NiFe with a particle size of about 450 nm 2 o 4 The particles were uniformly dispersed in 80 mL ethanol, 40 mL deionized water and 1 mL concentrated ammonia water (28 wt%), added 0.4 g tetraethyl orthosilicate (TEOS), and stirred magnetically for 8 h at room temperature to obtain a layer deposited on the surface Magnetic composite microspheres of silicon dioxide, the product is separated by a magnet and washed with a mixed solution of ethanol and water, and the product is dried at room temperature after washing for use;

[0036] (2) Ultrasonic disperse the magnetic Fe3O4 composite microspheres deposited with a layer of dense silica on the surface in a mixed solvent containing 50 mL of ethanol, 50 mL of deionized water, and 0.5 g of F127, and then add 0.6 mL of n-hexane Ultrasonic disperse into the above solution, then add 1.6 g dopamine hydrochloride into it, stir for 20 min to make the solution uniform, add 1.2 mL of concentrated ammonia water drop...

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Abstract

The invention belongs to the technical field of advanced nano materials, and specifically relates to a magnetic ordered mesoporous carbon-based or polymer-based core-shell structural composite microsphere and a preparation method thereof. According to the preparation method, magnetic nanoparticles are adopted as seeds, and the surface of the magnetic nanoparticles is coated with a dense silica protective layer with a sol-gel method; a macromolecular surfactant/polymer layer composite material of an ordered mesostructure is deposited on the surface of silicon dioxide by adopting an interface co-assembly technique and using a large molecular weight block copolymer as a templating agent; and finally, a magnetic mesoporous carbon-based composite microsphere having a strong surface hydrophobicity is obtained by calcination and carbonization in nitrogen, or a surface functionalized magnetic mesoporous polymer-based composite microsphere is obtained by removing the templating agent on the surface of the macromolecular with a solvent extraction method. The composite microsphere provided by the invention has the characteristics of strong magnetic responsiveness, relatively large ordered mesoporous passages, regular and ordered shell core structure, controllable hydrophilia and hydrophobicity and easy material transport and diffusion, and has important application prospects in the fieldof adsorption and separation.

Description

technical field [0001] The invention belongs to the technical field of advanced nanometer materials, and specifically relates to a magnetically ordered mesoporous carbon-based or polymer-based core-shell structure composite microsphere and a preparation method thereof. Background technique [0002] In recent years, magnetic carbon framework or polymer framework nanomaterials have broad application prospects in the analysis and separation of food and pollutants, enzyme catalysis, and disease diagnosis due to their magnetic response characteristics and low biological toxicity. Magnetic MOF materials have excellent microporous surface structure and ultra-high specific surface area, but due to the small pore size, it is difficult for guest molecules such as biological enzymes or organic macromolecules to be adsorbed and enriched into the pores of the material, making it difficult to make full use of the microporous shell. The huge specific surface area, so the overall enrichment...

Claims

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Application Information

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IPC IPC(8): B01J13/02B01J20/30B01J20/26B01J20/28B01J23/745B01J23/755
CPCB01J13/02B01J20/06B01J20/103B01J20/20B01J20/26B01J20/28009B01J23/745B01J23/755B01J35/0033B01J2220/42B01J2220/445B01J2220/4806B01J2220/4812
Inventor 邓勇辉潘盼盼于蕾
Owner FUDAN UNIV
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