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Method for preparing magnetic meso-porous silica composite microspheres via weak hydrolysis system

A mesoporous silica and hydrolysis system technology, which is applied in the fields of magnetic materials, magnetic objects, inductors/transformers/magnets, etc., can solve the problems of complex synthesis and low coating efficiency, and achieve simple preparation steps and comprehensive synthesis methods. The effect of stability and easy access to raw materials

Inactive Publication Date: 2019-06-28
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the invention first needs to check the amorphous silica to coat the mesoporous silica on its outer layer, and the synthesis is complicated.
Organic alkanes and water two-phase mixed solution solvent system, using strong TEOS hydrolysis catalysts such as ammonia water, TEOS hydrolysis is fast, easy to nucleate alone, forming mesoporous silica microspheres that are not coated with magnetic nanoparticles, and the coating efficiency is low

Method used

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  • Method for preparing magnetic meso-porous silica composite microspheres via weak hydrolysis system
  • Method for preparing magnetic meso-porous silica composite microspheres via weak hydrolysis system

Examples

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Effect test

Embodiment 1

[0029] (1) Evenly disperse 50mg of magnetic iron ferric oxide particles with a size of about 300nm in 100ml of water, 1.5g of 1,3,5-trimethylbenzene, 0.05g of L-arginine and 0.5g of hexadecyltrimethylbenzene After stirring for 30 minutes, 0.5g tetraethyl orthosilicate (TEOS) was added dropwise to a solution of ammonium chloride (CTAC), and stirred at 50°C for 24 hours to obtain magnetic nanoparticles / containing pore-enlarging agent and The silica core-shell composite microspheres of the surfactant, the thickness of the pore expander / surfactant / silica composite coating layer is 60nm; the product is collected with a magnet, and washed 3 times with absolute ethanol and water;

[0030] (2) The above-mentioned washed magnetic nanoparticles / silica core-shell composite microspheres containing pore expanders and surfactants were calcined at 400°C for 3 hours in an air atmosphere to obtain ferric oxide@mesoporous silica core Shell composite microspheres.

[0031] The magnetic nanopart...

Embodiment 2

[0034] (1) Evenly disperse 50mg of γ-iron sesquioxide particles with a size of about 60nm in 100ml of water, 0.5g of 1,3,5-trimethylbenzene, 1g of L-lysine and 0.5g of Brij35 (C 12 h 25 EO 23 ) solution, after stirring for 30 minutes, add 2 g of tetraethyl orthosilicate (TEOS) dropwise, and stir at 50°C for 24 hours to obtain magnetic nanoparticles / silica containing pore-enlarging agent and surfactant Core-shell composite microspheres, the thickness of the pore expander / surfactant / silica composite coating layer is 100nm; the product is collected with a magnet, and washed three times with 0.6wt% ammonium nitrate ethanol solution;

[0035] (2) The above-mentioned washed magnetic nanoparticles / silica core-shell composite microspheres containing pore expanders and surfactants were calcined at 200°C for 9 hours in an air atmosphere to obtain γ-ferric oxide@mesoporous dioxide Silicon core-shell composite microspheres.

Embodiment 3

[0037] (1) 50mg of CoFe with a size of about 600nm 2 o 4 The particles are uniformly dispersed in 100ml of water, 1.5g of 1,3,5-trimethylbenzene, 0.05g of triethanolamine and 1g of small molecule Brij56 containing polyether (C 16 h 33 EO 10 ) solution, after stirring for 30 minutes, add 0.5g of sodium silicate dropwise, and stir at 80°C for 12 hours to obtain magnetic nanoparticles / silica core-shell composite microspheres containing pore expanders and surfactants , the thickness of the pore expander / surfactant / silicon dioxide composite coating layer is 20nm; the product is collected with a magnet, and washed three times with a hydrochloric acid ethanol solution with a pH greater than 1.0;

[0038] (2) Calcining the above-mentioned washed magnetic nanoparticles / silica core-shell composite microspheres containing pore expanders and surfactants at 500 °C for 1 h in an air atmosphere to obtain CoFe 2 o 4 @Mesoporous silica core-shell composite microspheres.

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Abstract

The invention provides a method for preparing magnetic meso-porous silica composite microspheres via a weak hydrolysis system, relates to the technical field of advance nanocomposite materials, and solves the problems that traditional meso-porous silica microspheres are relatively small in the meso-porous size, limited in the loading object and hard to bear micro-molecule protein as enzyme. The method comprises the following steps that magnetic nanoparticle, a surfactant, a hole reaming agent and a hydrolysis catalyst are uniformly dispersed in a hydrosolvent, a silicon source precursor is added, reaction is carried out for 12-48h at 10-80 DEG C, and a product is burned for 1-9 h at 200-500 DEG C in the air atmosphere to obtain the magnetic meso-porous silica composite microspheres. The preparation method is simple in steps, raw materials are easy to obtain, and a synthesis method is suitable and suitable for large-scale industrial production; and the prepared magnetic meso-porous silica composite microspheres includes the meso-structure in the aperture of 5-30nm, substances as enzyme and DNA can be born, the center of the magnetic meso-porous silica composite microsphere includesa relatively large magnetic nanoparticle magnetic core, and a good magnetic separation effect is realized.

Description

technical field [0001] The invention relates to the technical field of advanced nanocomposite materials, in particular to a method for preparing magnetic mesoporous silica composite microspheres in a weak hydrolysis system. Background technique [0002] In recent years, with the application of mesoporous materials in the fields of adsorption, catalysis, drug delivery and sensors, more and more researchers pay attention to mesoporous materials, especially mesoporous silica materials based on their high specific Excellent properties such as surface area, uniform mesopore, macropore volume, rich mesopore structure and biocompatibility are considered to be ideal supports for enzyme immobilization. Due to the convenient operation of magnetic separation and recovery, magnetic nanomaterials have attracted many researchers' interest in catalysis, adsorption and enrichment. Therefore, the application of magnetic nanomaterials and mesoporous silica materials in the biological field ha...

Claims

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Application Information

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IPC IPC(8): H01F1/00H01F41/00
Inventor 胡军蒋晨星黄亮汪晶金洁宁李大权
Owner ZHEJIANG UNIV OF TECH
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