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Preparation method of magnetic fluorescence dual-function silicon oxide hollow microspheres

A hollow microsphere, dual-function technology, applied in the direction of microsphere preparation, chemical instruments and methods, microcapsule preparation, etc., can solve the problems of low saturation magnetization of microspheres, poor magnetic responsiveness, and limited biomedical applications, etc. Achieve the effects of narrow particle size distribution, stable fluorescence characteristics, and low raw material cost

Active Publication Date: 2013-02-13
SUZHOU WIN BIO TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chen et al [Chen Y., et al., 2010 3RD INTERNATIONAL NANOELECTRONICS CONFERENCE, 2010, 1, 959-960.] reported the use of vacuum impregnation technology to fill the magnetic nanoparticles into the pre-prepared silicon oxide medium through the surface channel structure. In the hollow structure of holes, however, the silica hollow microspheres with magnetic particles prepared by these methods will be limited by the size and quantity of the magnetic nanoparticles loaded by the hollow microspheres, so the prepared The saturation magnetization of microspheres is generally small, and the magnetic response is not good
Yuan et al. [Yuan J., et al., J. Magn. Magn. Mater., 2010, 322, 2172-2176.] on the surface of silica hollow microspheres modified with sulfonic acid groups, By adsorbing 2 and 3 valent iron salts, and then promoting the co-precipitation reaction of iron salts to nucleate and grow on the surface of silica hollow microspheres, a hollow structure with magnetic nanoparticles wrapped in a silica shell is obtained. This structure has good magnetic responsiveness, but The silica shell cannot be further surface-modified because it is not exposed, so this material system is difficult to be used as a carrier for biomolecular connection, which limits subsequent biomedical applications

Method used

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  • Preparation method of magnetic fluorescence dual-function silicon oxide hollow microspheres
  • Preparation method of magnetic fluorescence dual-function silicon oxide hollow microspheres
  • Preparation method of magnetic fluorescence dual-function silicon oxide hollow microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1. 24 g FeCl 3 ·6H 2 O and 9.82 g FeCl 2 ·7H 2 Dissolve O in an appropriate amount of water, add an appropriate amount of ammonia water, pass N 2 Gas, heated at 80°C for 30min, then added 3.76 g of oleic acid, continued to heat and stir for 1h, then stopped passing through N 2 , volatilize ammonia water until a large amount of black precipitate appears after stopping stirring, then the reaction can be stopped. Under magnetic separation, the precipitate is washed with deionized water to neutrality, and then washed with deionized water and ethanol three times respectively, and the obtained magnetic Particles, ultrasonically disperse the magnetic particles in an appropriate amount of n-octane, and then evaporate the n-octane to dryness by rotary evaporation, and set aside; dissolve 0.092 g SDS in 40 g deionized water, dissolve 8 g styrene monomer, 0.4 g hexadecane , 1 g TEOS, and 55 mg magnetic particle dispersion were mixed and ultrasonicated to form a uni...

Embodiment 2

[0029] Example 2. 24 g FeCl 3 ·6H 2 O and 9.82 g FeCl 2 ·7H 2 Dissolve O in an appropriate amount of water, add an appropriate amount of ammonia water, pass N 2 Gas, heated at 80°C for 30min, then added 3.76 g of oleic acid, continued to heat and stir for 1h, then stopped passing through N 2 , volatilize ammonia water until a large amount of black precipitate appears after stopping stirring, then the reaction can be stopped. Under magnetic separation, the precipitate is washed with deionized water to neutrality, and then washed with deionized water and ethanol three times respectively, and the obtained magnetic Particles, ultrasonically disperse the magnetic particles in an appropriate amount of n-octane, then evaporate the n-octane to dryness by rotary evaporation, and set aside; dissolve 0.12 g SDBS in 40 g deionized water, mix 8 g styrene monomer, 0.4 g hexadecane , 2 g of methyl orthosilicate, and 80 mg of magnetic particle dispersion were mixed and ultrasonicated ...

Embodiment 3

[0030] Example 3. 24 g FeCl 3 ·6H 2 O and 9.82 g FeCl 2 ·7H 2 Dissolve O in an appropriate amount of water, add an appropriate amount of ammonia water, pass N 2 Gas, heated at 80°C for 30min, then added 3.76 g of oleic acid, continued to heat and stir for 1h, then stopped passing through N 2 , volatilize ammonia water until a large amount of black precipitate appears after stopping stirring, then the reaction can be stopped. Under magnetic separation, the precipitate is washed with deionized water to neutrality, and then washed with deionized water and ethanol three times respectively, and the obtained magnetic Particles, ultrasonically disperse the magnetic particles in an appropriate amount of n-octane, then evaporate the n-octane to dryness by rotary evaporation, and set aside; dissolve 0.23 g of SDS in 40 g of deionized water, mix 8 g of styrene monomer, 0.4 g of cetyl alcohol , 1 g TEOS, and 55 mg magnetic particle dispersion were mixed and ultrasonicated to form ...

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Abstract

The invention relates to a preparation method of magnetic fluorescence dual-function silicon oxide hollow microspheres, comprising the steps of: preparing magnetic nanometer particles by a coprecipitation method; diffusing the magnetic nanometer particles in long-chain alkane after the surfaces of the magnetic nanometer particles are modified by oleic acid; mixing the oil phase composed of alkane dispersion consisting of a styrene monomer, a superhydrophobic agent and magnetic nanometer particles, and the orthosilicic acid alkyl ester with water phase in which a surface active agent is dissolved; pre-emulsifying and finely emulsifying the mixture to obtain a fine emulsion drop system; when the drops are in free radical polymerization, adding an alkali catalyst to control the generation of silicon oxide and the phase separation of the organic and inorganic components of the system; in the reaction process, adding proper ammonia water and a silane coupling agent which is marked by fluorescein to obtain the hollow compound microspheres which are different in sizes, inorganic shell thicknesses and magnetic particle solid content and have stable fluorescence signals. The preparation method disclosed by the invention is simple, the raw materials are low in cost and easy to obtain; and the obtained fluorescence dual-functional hollow silicon oxide microspheres are narrow in size distribution, high in magnetic substance content and stable in fluorescence performance.

Description

field of invention [0001] The invention belongs to the technical field of preparation of magnetic composite functional materials, and in particular relates to a preparation method of silicon oxide magnetic composite hollow microspheres with fluorescence characteristics and high magnetic substance content. Background technique [0002] Silica hollow microspheres with magnetic cores can be widely used in biomedicine such as cell separation, enzyme immunomagnetic analysis, drug controlled release carrier, etc. Therefore, it has attracted the attention of researchers and has become a new research hotspot. The idea of ​​preparing silica magnetic hollow microspheres by the traditional method is basically the same as that of non-magnetic pure silica hollow microspheres. It is basically prepared by the template-assisted method. There are many kinds of materials constituting the template, including polymer microspheres, Micelles composed of surfactant molecules (Ren Yi, Liu Kailang,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J13/02H01F1/11C09K11/06
Inventor 王祎龙马方陈炳地张兵波郭方方时东陆
Owner SUZHOU WIN BIO TECH CO LTD
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