Hollow structured magnetic microsphere coated with mono-dispersed silicon dioxide and its preparation method

A technology of silica and magnetic microspheres, which is applied in the field of magnetic nanomaterials, can solve the problems of poor controllability and uniformity of the particle size of magnetic nanoparticles, no surface modification of the particles, no template removal, etc., and the preparation method is simple and easy Row, uniform number of nuclei, strong acid resistance

Inactive Publication Date: 2007-02-14
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the particle size controllability and uniformity of the synthesized magnetic nanoparticles are poor, the particles are...

Method used

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  • Hollow structured magnetic microsphere coated with mono-dispersed silicon dioxide and its preparation method

Examples

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Embodiment 1

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

[0024] Weigh 1g of FeCl 3 ·6H 2 O and 0.37 g FeCl 2 4H 2 O was dissolved in 20ml of water through nitrogen and deoxygenation to obtain a mixed solution. Take 130ml of water in a 250mL round-bottomed flask, pass nitrogen to remove oxygen, add 12.5ml of concentrated ammonia water with a mass percentage concentration of 25-28%, pour the above-mentioned iron salt mixed solution into it quickly under vigorous stirring, and heat at 80°C Under reaction 1h. After the reaction is completed, use a 0.1T 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 6 to 10 nm. 3 o 4 Nanoparticles.

[0025] Will Fe 3 o 4After the nanoparticles were fixed to a volume of 6 mg / ml, 20 ml was taken out and sonicated for 10 minutes to obtain a ferrite nanoparticle sol for compo...

Embodiment 2

[0026] Example 2 Synthesis of Ferrite Nanoparticles: CoFe 2 o 4 Preparation of nanoparticles

[0027] Weigh 1g of FeCl 3 ·6H 2 O and 0.38 g CoCl 2 4H 2 O was dissolved in 20ml of water through nitrogen and deoxygenation to obtain a mixed solution. Take 130ml of water in a 250mL round-bottomed flask to pass through nitrogen to remove oxygen, add 12.5ml of concentrated ammonia water with a concentration of 25-28% by mass, and quickly pour the above mixed salt solution into it under vigorous stirring. Reaction 1h. After the reaction is completed, use a 0.1T 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 3 to 13 nm. 2 o 4 Nanoparticles.

[0028] CoFe 2 o 4 Nanoparticles are ultrasonically dispersed in water to obtain ferrite nanoparticle sol.

[0029] CoCl can be 2 Change to MnCl 2 or ZnCl 2 get the corresponding MnFe 2 o 4 or ZnFe ...

Embodiment 3

[0030] Example 3 Synthesis of polymer microspheres: Synthesis of polystyrene-acrylic acid (PS-AA) polymer microspheres

[0031] Add 100ml of water and 0.12g of NaHCO into a 250ml three-necked bottle 3 , 5ml styrene (St) and 0.5ml acrylic acid (-AA), pass N 2 After half an hour, it was placed in a water bath at 70° C., 0.05 g of potassium persulfate (KPS) was added and reacted for 10 h under mechanical stirring to obtain polystyrene-acrylic acid microspheres with a particle size of 300 nm.

[0032] If 8g of sodium dodecylbenzenesulfonate is added to the reaction system, polymer microspheres with a particle diameter of 80nm are obtained.

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Abstract

The present invention is monodisperse silica coated hollow magnetic microsphere and its preparation process and belongs to the field of nanometer magnetic material technology. Superparamagnetic nanometer ferrite particle is first prepared in coprecipitatin method and monodisperse polymer microsphere with surface functional radical is synthesized in emulsion polymerization; the superparamagnetic nanometer ferrite particle and the monodisperse polymer microsphere is then compounded by means of coordination effect, and the compound is coated with silica; and the composition particle is finally calcined at 500-700 deg.c for 5-12 hr to produce the silica coated hollow magnetic microsphere. The present invention has simple preparation process and controllability of the granularity and cavity size of the magnetic microsphere, and the magnetic microsphere has high chemical and colloid stability and may be used in biological detection and other fields.

Description

technical field [0001] The invention belongs to the technical field of magnetic nanometer materials, in particular to a superparamagnetic microsphere with a hollow structure coated with monodisperse silicon dioxide and a preparation method thereof. Background technique [0002] Due to its unique properties (no remanence), superparamagnetic nanoparticles have broad application prospects in biomedical fields such as bioseparation, immunoassay, and targeted drugs. However, due to its own chemical stability, colloidal stability, and poor biocompatibility, its surface often needs to be modified with a protective layer, such as polymer or silicon dioxide. Due to the advantages of good chemical and colloidal stability and good biocompatibility, silica is one of the most ideal materials for protecting magnetic particles. The inventor has used ferrite nanoparticles without any surface treatment and ultrasonic treatment for silica coating to obtain ferrite-silica core-shell particles...

Claims

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Application Information

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IPC IPC(8): B01J13/02C04B35/26C04B35/624C04B35/628H01F1/11
Inventor 杨文胜陆子阳王刚
Owner JILIN UNIV
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