Magnetic nanosphere with mesoporous shell and quick preparation method thereof

A technology of magnetic nanospheres and nanospheres, applied in the field of magnetic nanospheres, can solve the problems of complex process of magnetic nanospheres, small specific surface area of ​​magnetic nanospheres, long preparation time, etc. The effect of separating costs

Inactive Publication Date: 2013-12-25
BEIJING UNIV OF CHEM TECH
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Problems solved by technology

Fe can also be synthesized relatively quickly by this method. 3 o 4 Core surface coated with dense SiO 2 Shell magnetic nanospheres (Anne-Laure Morel, Sergei I. Nikitenko, Karine Gionnet, Alain Wattiaux, Josephine Lai-Kee-Him Christine Labrugere, Bernard Chevalier, Gerard Deleris, Cyril Petibois, Alain Brisson, Monique Simonoff. Sonochemical approach to the synthesis of Fe 3 o 4 SiO 2 core-shell nanoparticles with tunable properties.ACSnano, 2008, 2, 847-856), but synthesized Fe 3 o 4 Core surface coated with dense SiO 2 The magnetic nanospheres of the shell layer should use more expensive tetraethyl orthosilicate as Fe 3 o 4 Core surface coated with dense SiO 2 layer of Si source, especially Fe 3 o 4 Core surface coated with dense SiO 2 The specific surface area of ​​the magnetic nanosphere prepared by the layer is small, and it has certain limitations as a catalyst support.
[0005] In view of the above problems such as complex preparation of magnetic nanospheres and long preparation time, the present invention adopts FeCl 3 ·6H 2 O to prepare Fe with superparamagnetism 3 o 4 core, with cheap sodium silicate as superparamagnetic Fe 3 o 4 Core surface coated with SiO 2 The silicon source of the shell, using hexadecyltrimethylammonium bromide as a template, adopts the method of ultrasonic wave, in superparamagnetic Fe 3 o 4 Rapid formation of a layer of mesoporous SiO on the surface of the core 2 The shell layer, prepared a kind of mesoporous SiO 2 Magnetic SiO with shell and large specific surface area 2 Fe 3 o 4 nanosphere

Method used

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  • Magnetic nanosphere with mesoporous shell and quick preparation method thereof

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Embodiment 1

[0018] (1) Weigh 13.4g FeCl 3 ·6H 2 O was dissolved in 86.6g of deionized water to make a solution, and 4.1g of sodium acetate was weighed and dissolved in 45.9g of ethylene glycol to make a solution. At the temperature of a water bath at 30°C and under stirring conditions, it was added dropwise to the solution containing N 2 In the protected reactor, after the dropwise addition, the mixed solution was put into an autoclave, crystallized at 180°C for 8 hours, then cooled naturally, washed with deionized water and ethanol three times, and dried in vacuum at 60°C for 8 hours. The obtained magnetic Fe 3 o 4 particles.

[0019] (2) Weigh the prepared magnetic Fe 3 o 4 Add 5.8g of granules to 44.2g of ethanol, add dropwise 20g of sodium silicate solution with a mass concentration of 5% and cetyltrimethyl bromide with a mass concentration of 0.2% at the same time at a water bath temperature of 30°C under stirring conditions Ammonium chloride (CTAB) ethanol solution 5g, after t...

Embodiment 2

[0021] (1) Weigh 20.3g FeCl 3 ·6H 2 O was dissolved in 79.7g of deionized water to make a solution, and 6.2g of sodium acetate was weighed and dissolved in 43.8g of ethylene glycol to make a solution. At the temperature of a water bath at 30°C and under stirring conditions, it was added dropwise to the solution containing N 2 In the protected reactor, after the dropwise addition, the mixed solution was put into an autoclave, crystallized at 180°C for 8 hours, then cooled naturally, washed with deionized water and ethanol three times, and dried in vacuum at 60°C for 8 hours. The obtained magnetic Fe 3 o 4 particles.

[0022] (2) Weigh the prepared magnetic Fe 3 o 4 Add 6.9g of granules to 43.1g of ethanol, add 20g of sodium silicate solution with a mass concentration of 10% and hexadecyltrimethyl bromide with a mass concentration of 0.2% at the same time under stirring conditions at a water bath temperature of 30°C Ammonium chloride (CTAB) ethanol solution 10g, after the ...

Embodiment 3

[0024] (1) Weigh 27.0g FeCl 3 ·6H 2 O was dissolved in 73.0g deionized water to make a solution, and 8.2g of sodium acetate was weighed and dissolved in 41.8g of ethylene glycol to make a solution, which was added dropwise at the temperature of a water bath at 30°C under stirring conditions 2 In the protected reactor, after the dropwise addition, the mixed solution was put into an autoclave, crystallized at 180°C for 8 hours, then cooled naturally, washed with deionized water and ethanol three times, and dried in vacuum at 60°C for 8 hours. The obtained magnetic Fe 3 o 4 particles.

[0025] (2) Weigh the prepared magnetic Fe 3 o 4 Add 9.3g of granules to 40.7g of ethanol, add dropwise 15g of sodium silicate solution with a mass concentration of 15% and cetyltrimethyl bromide with a mass concentration of 0.2% at the same time at a water bath temperature of 30°C under stirring conditions Ammonium chloride (CTAB) ethanol solution 15g, after the dropwise addition, ammonia so...

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Abstract

The invention relates to a magnetic nanosphere with a mesoporous shell and a quick preparation method thereof, which belongs to the technical field of magnetic nanospheres. A Fe3O4 core with superparamagnetism is prepared from FeCl3.6H2O, then a mesoporous SiO2 shell is quickly formed on the surface of the magnetic Fe3O4 core with an ultrasonic wave method by taking hexadecyl trimethyl ammonium bromide as a template agent and taking low-cost sodium silicate as a silicon source for wrapping the SiO2 shell on the surface of the magnetic Fe3O4, and finally, the template agent is removed by roasting under the protection of N2, thus obtaining the magnetic SiO2@Fe3O4 nanosphere with the mesoporous SiO2 shell and large specific surface area. The magnetic nanosphere has good application prospects in the aspects of magnetic adsorption, precious metal recovery, target administration carriers, bioprotein separation and the like.

Description

technical field [0001] The invention relates to a magnetic nanosphere with a mesoporous shell and a rapid preparation method thereof, belonging to the technical field of magnetic nanospheres. Background technique [0002] Magnetic nanomaterials are widely used in magnetic fluids, microwave absorption, adsorption and removal of water pollutants, precious metal recovery, catalysis, targeted drug delivery carriers, biological protein separation, etc. (Ji Junhong, Ji Shengfu, Yang Wei, Li Chengyue. Magnetic Fe 3 o 4 Preparation and application of nanocrystals. Advances in Chemistry, 2010,22(8):1566-1574), such as superparamagnetic Fe 3 o 4 Cu / Fe prepared for nuclei 3 o 4 SiO 2 Magnetic catalyst, which can realize the catalytic conversion of low concentration formaldehyde to hydrogen production (Junhong Ji, Penghui Zeng, Shengfu Ji, Wei Yang, Hongfei Liu, Yingyi Li. Catalytic activity of core–shell structured Cu / Fe 3 o 4 SiO 2 microsphere catalysts.Catalysis Today, 2010,1...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/02
Inventor 季生福杨浩刘鸿飞
Owner BEIJING UNIV OF CHEM TECH
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