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Silica-magnetic composite micropartical and preparation method thereof

A technology of mesoporous silica and composite particles, applied in the field of magnetic materials, can solve the problems of reducing the specific surface area of ​​magnetic particles, weak magnetic response ability, and inability to achieve magnetic separation, and achieve strong external magnetic field response ability and strong oxidation resistance , The effect of low equipment requirements

Inactive Publication Date: 2009-07-08
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the limited specific surface area of ​​magnetic particles poses great challenges to their application in many technical fields
Even for very small magnetic particles (such as: 30nm), its specific surface area is only 40m 2 / g, further reducing the size of the magnetic particles to increase the specific surface area of ​​the particles cannot achieve ideal results, because the magnetic response ability depending on the particle size will become so weak that it cannot achieve the purpose of magnetic separation, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1: Fe 3 o 4 Preparation of nanoparticles

[0020] Weigh 13.73g of FeCl 3 ·6H 2 O and 5.1 g FeCl 2 4H 2 O, dissolved in 100mL of water that has passed through nitrogen and deoxygenated to obtain a mixed solution. Take 400mL of water in a 1L three-necked bottle to pass through nitrogen to remove oxygen, add 25mL of concentrated ammonia water with a mass percentage concentration of 25-28%, and quickly pour the above-mentioned iron salt mixed solution into it under vigorous stirring. Reaction 1h. After the reaction is completed, use a 0.2T permanent magnet to separate the black solid from the reaction solution, and wash the obtained solid with high-purity water for 3 to 5 times to obtain Fe with a particle size of 7 to 12 nm. 3 o 4 Nanoparticles.

Embodiment 2

[0021] Embodiment 2: γ-Fe 2 o 3 Preparation of nanoparticles

[0022] Weigh 13.73g of FeCl 3 ·6H 2 O and 5.1 g FeCl 2 4H 2 O, dissolved in 100mL of water that has passed through nitrogen and deoxygenated to obtain a mixed solution. Take 400mL of water in a 1L three-necked bottle to pass through nitrogen to remove oxygen, add 25mL of concentrated ammonia water with a mass percentage concentration of 25-28%, and quickly pour the above-mentioned iron salt mixed solution into it under vigorous stirring. Reaction 1h. Oxygen was then introduced into the reaction solution for 2 h. After the reaction is completed, use a 0.2T permanent magnet to separate the red solid from the reaction solution, and wash the obtained solid with high-purity water for 3 to 5 times to obtain γ-Fe with a particle size of 7 to 12 nm. 2 o 3 Nanoparticles.

Embodiment 3

[0023] Example 3: CoFe 2 o 4 Preparation of nanoparticles

[0024] Weigh 14g of CoCl 3 ·6H 2 O and 5.1 g FeCl 2 4H2 O, dissolved in 100mL of water that has passed through nitrogen and deoxygenated to obtain a mixed solution. Take 400mL of water in a 1L three-necked bottle to remove oxygen through nitrogen, add 25mL of concentrated ammonia water with a concentration of 25-28% by mass, quickly pour the above mixed salt solution into it under vigorous stirring, and react at 50°C 1h. After the reaction is completed, use a 0.2T permanent magnet to separate the black solid from the reaction solution, and wash the obtained solid with high-purity water for 3-5 times to obtain CoFe with a particle size of 7-12nm. 2 o 4 Nanoparticles.

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PUM

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Abstract

The mesoporous silicon dioxide-magnetic composite particles and the preparation method thereof belong to the technical field of magnetic materials. The inner core of the particle is superparamagnetic nanometer ferrite particles coated with silicon dioxide, the outer shell is mesoporous silicon dioxide, the particle has a multi-core structure, and the specific surface area is 180-210m2 / g. The preparation method comprises preparing ferrite particles by a co-precipitation method; then directly dispersing the washed ferrite particles into an aqueous solution of water-soluble inorganic salt containing SiO2 to coat the inorganic silicon source; Ammonium bromide was used as a template, and tetraethyl orthosilicate was used as a silicon source for mesoporous silica coating. The process and required equipment of the invention are simple, and the composite particles have the characteristics of high magnetic substance content, strong external magnetic field response ability, high specific surface area, strong magnetic separation ability, good dispersibility in water, and easy further functionalization. The particle is suitable for separation and purification in the fields of biological materials and pharmaceutical products.

Description

technical field [0001] The invention belongs to the technical field of magnetic materials, in particular to a mesoporous silicon dioxide-magnetic composite particle and a preparation method thereof. Background technique [0002] Since the researchers of Mobil Corporation synthesized mesoporous silica, this kind of mesoporous molecular sieve has brought infinite vitality to the synthesis and application of mesoporous solid materials. For example: Mesoporous materials can be used as microreactors for nanoparticles due to their adjustable nanoscale pore structure. In addition, due to its huge specific surface area and uniform pore size, mesoporous solid materials have important applications in catalysis, especially in catalyzing reactions involving large-volume molecules, mesoporous materials show better performance than zeolite molecular sieves. catalytic activity. Since the surface effect, quantum confinement effect and small size effect of mesoporous solids may be signific...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01F1/11B22F1/02C04B35/628
Inventor 杨文胜滕兆刚王刚李军
Owner JILIN UNIV
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