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Superparamagnetism mesoporous silicon dioxide composite ball and preparing method thereof

A mesoporous silica and superparamagnetic technology, applied in the direction of magnetic properties of silica, silica, inorganic materials, etc., can solve the problems of low saturation magnetization, wide size distribution of silica composite particles, irregular shape, etc. , to achieve the effect of high content of magnetic substances, low equipment requirements, and strong external magnetic field responsiveness

Inactive Publication Date: 2012-07-25
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the magnetic mesoporous silica composite particles prepared by the methods in the prior art have the disadvantages of wide size distribution, irregular shape, and low saturation magnetization.

Method used

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  • Superparamagnetism mesoporous silicon dioxide composite ball and preparing method thereof
  • Superparamagnetism mesoporous silicon dioxide composite ball and preparing method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Example 1: Fe 3 o 4 Preparation of nanoparticles

[0024] 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 concentration of 25% to 28% by mass, and quickly pour the above iron salt mixed solution into it under vigorous stirring. Reaction 1h. After the reaction is completed, use a 0.4T 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

[0025] Example 2: γ-Fe 2 o 3 Preparation of nanoparticles

[0026] 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 concentration of 25% to 28% by mass, and quickly pour the above 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 0.4T 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

[0027] Example 3: CoFe 2 o 4 Preparation of nanoparticles

[0028] Weigh 14g of CoCl 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 concentration of 25% to 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 0.4T 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 CoFe with a particle size of 7 to 12 nm. 2 o 4 Nanoparticles.

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Abstract

A superparamagnetism mesoporous silicon dioxide composite ball of the present invention and manufacture method thereof belong to nucleocapsid type technology field of magnetic nano particle. The shape of the composite ball is global; inner core being made of magnetic ferrite nano particle cluster, shell coating layer being made of mesoporous silicon dioxide; quality ratio of magnetic ferrite nanoparticle in particulate being 40-80%. Method of manufacturing has that producing magnetic ferrite nano particle is by using coprecipitation method; executing surface modification by adding oleic acidstirring; ultrasonic forming oil-in-water emulsion in the mix solution of ethyl orthosilicate and cyclohexane, cetyl trimethyl ammonium bromide as surfactant; ethyl orthosilicate hydrolytic condensation forming mesoporous silicon dioxide coating layer by adding ammonia spirit; finally taking off molding plate and getting products. Product of the invention has bigger specific surface area and stronger magnetic separation capacity, and has good dispersancy in water, and is further functionalization after being decorated at surface. The method of the present invention has simple process, and lower equipment requirement.

Description

technical field [0001] The invention belongs to the technical field of core-shell magnetic nanoparticles and a preparation method thereof; in particular, it relates to a superparamagnetic mesoporous silica composite sphere with high saturation magnetization 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 ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01F1/11B22F1/02C04B35/628C01B33/18
Inventor 杨文胜滕兆刚赵锐李军
Owner JILIN UNIV
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