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A magnetic mesoporous SIO with a core-shell-shell structure 2 Preparation method of nanoparticles

A magnetic nanoparticle and nanoparticle technology, which is applied in the preparation of microspheres, chemical instruments and methods, pharmaceutical formulations, etc., can solve the problem of invisible pore structure and other problems, and achieve clearly visible pore structure, uniform particle size distribution, and dispersibility. Good results

Active Publication Date: 2020-12-11
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Magnetic mesoporous SiO prepared by existing methods 2 Nanoparticles do not have a complete and uniform pore structure, and there are many deficiencies in both morphology and application (Document 1: Wang Miaomiao, et al. Mesoporous SiO 2 / Fe 3 o 4 Laccase Immobilization of Hollow Magnetic Microspheres[J]. Chemical Journal of Chinese Universities, 2013(2): 299~305., Literature 2: WeiweiZhao.et.al Novel Method To Investigate the Interaction Force between Etoposide and APTES-Functionalized Fe 3 o 4 @nSiO 2 @mSiO 2 Nanocarrier for DrugLoading and Release Processes.Phys.Chem.C 2015,119,4379~4386)

Method used

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  • A magnetic mesoporous SIO with a core-shell-shell structure <sub>2</sub> Preparation method of nanoparticles
  • A magnetic mesoporous SIO with a core-shell-shell structure <sub>2</sub> Preparation method of nanoparticles
  • A magnetic mesoporous SIO with a core-shell-shell structure <sub>2</sub> Preparation method of nanoparticles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1: Magnetic mesoporous nanoparticle Fe 3 o 4 @SiO 2 @mSiO 2 - Preparation of EDPS

[0021] Will Fe 3 o 4 Take 100 mg of magnetic nanoparticles and ultrasonically disperse them in a mixture of 160 mL of ethanol and 40 mL of water for 40 minutes, and add 2 mL of NH under vigorous mechanical stirring. 3 ·H 2 O, then add 2.5mL TEOS dropwise within 10min, continue stirring at 35°C for 6h, wash with ethanol and deionized water three times, magnetically separate, and vacuum dry at 40°C for 10h to obtain SiO 2 Coated Fe with uniform size and core-shell structure 3 o 4 @SiO 2 magnetic microspheres.

[0022] Take 80mg Fe 3 o 4 @SiO 2 The magnetic microspheres were dispersed in a mixed solution containing 95mL water, 43mL ethanol, 2.5mL ammonia water and 0.3g CTAC by ultrasonication for 30min. Subsequently, 2.5 mL of TEOS was mixed in 6 mL of ethanol and added dropwise to the reaction system with stirring. After 15 minutes of reaction, the particles were ...

Embodiment 2

[0026] Embodiment 2: large-aperture magnetic mesoporous Fe 3 o 4 @SiO 2 @mSiO 2 - Preparation of EDPS nanoparticles

[0027] Fe 3 o 4 @SiO 2 The preparation method of the magnetic microspheres is the same as in Example 1.

[0028] Take 80mg Fe 3 o 4 @SiO 2 The magnetic microspheres were dispersed in a mixed solution containing 95mL water, 49mL ethanol, 2.5mL ammonia water, 0.18mL triethylamine (TEA) and 0.3g CTAC by ultrasonication for 30min. Subsequently, 2.5 mL of TEOS was dissolved in 6 mL of cyclohexane and added dropwise to the reaction system with stirring. After 15 minutes of reaction, the particles were formed, and 2.5mL EDPS was also added dropwise to the system. After 18 hours of reaction at room temperature, the product was collected by magnetic separation and washed three times with ethanol and water. Finally, the nanoparticles were redispersed in 60 mL of acetone, and refluxed at 70 °C for 12 h to remove CTAC. To ensure the complete removal of CTAC, thi...

Embodiment 3

[0042] Embodiment 3: Magnetic mesoporous nanoparticle Fe 3 o 4 @SiO 2 @mSiO 2 - Preparation of EDPS

[0043] Will Fe 3 o 4 Disperse 80 mg of magnetic nanoparticles in a mixture of 160 mL of ethanol and 40 mL of water by ultrasonication for 40 minutes, and add 3 mL of NH 3 ·H 2 O, then add 4mL TEOS dropwise within 10min, continue to stir at 35°C for 6h, wash with ethanol and deionized water three times, magnetically separate, and vacuum dry at 40°C for 10h to obtain SiO 2 Coated Fe with uniform size and core-shell structure 3 o 4 @SiO 2 magnetic microspheres.

[0044] Take 80mg Fe 3 o 4 @SiO 2 The magnetic microspheres were dispersed in a mixed solution containing 95mL water, 43mL ethanol, 4mL ammonia water and 0.3g CTAC by ultrasonication for 30min. Subsequently, 2 mL of TEOS was mixed in 7.5 mL of ethanol and added dropwise to the reaction system with stirring. After 15 minutes of reaction, the particles were formed, and 2.5mL EDPS was added dropwise to the sys...

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Abstract

The invention discloses a preparation method of magnetic mesoporous SiO2 nanoparticles with a core-shell-shell structure. According to the method, Fe3O4 is used as a magnetic carrier; tetraethoxysilane is used as a silicon source; hexadecyl trimethyl ammonium chloride is used as a surfactant; the radial Fe3O4@SiO2@mSiO2 mesoporous nanoparticles with a mesoporous form and a core-shell-shell three-layer structure is obtained; and at the same time, N-[3-(trimethoxysilyl)propyl]ethylenediamine is used as an amino silane coupling agent for loading amino groups in the surfaces and the pore channelsof the mesoporous nanoparticles. In addition, according to the invention, triethylamine and cyclohexane are used as organic swelling agents, so that a mesoporous layer with a larger pore diameter is obtained. The magnetic mesoporous SiO2 nanoparticles prepared by the method disclosed by the invention have good magnetism, high dispersity and unique pore channel structure, and have a wide application prospect in the aspects of medicine release, biology, material science and the like.

Description

technical field [0001] The invention belongs to the field of preparation of mesoporous materials, in particular to magnetic mesoporous SiO with a core-shell-shell structure 2 Methods for the preparation of nanoparticles. Background technique [0002] Mesoporous SiO 2 Nanoparticles are nanomaterials with radial vertical channels on the surface. Due to mesoporous SiO 2 Microspheres have a larger specific surface area and a unique pore structure, making them widely used in composite materials, biology, medicine and other fields, especially in adsorption applications and drug release. Magnetic Mesoporous SiO 2 Nanoparticles are magnetic particles embedded in mesoporous SiO 2 Inside, a core-shell two-layer structure is formed, making it magnetic while maintaining a unique pore structure. The core-shell-shell three-layer structure has a larger particle size and a more complete spherical structure, and more molecules can be loaded on the surface and in the pores. [0003] Ma...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J13/06B01J20/22B01J20/28B01J20/30A61K9/51
CPCA61K9/0009A61K9/5115A61K9/5123B01J13/06B01J20/223B01J20/28009B01J20/28016B01J20/28054
Inventor 董伟盛伟潘夕郝陈琦左淦丞
Owner NANJING UNIV OF SCI & TECH
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