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Preparation method for mesoporous silicon oxide hollow microspheres with magnetic nanoparticles embedded in shell layers

A technology of magnetic nanoparticles and mesoporous silica, which is applied in the preparation of microspheres, silica and microcapsules, etc., can solve the problems of limited content of magnetic nanoparticles, uneven distribution, difficult operation, etc., and achieve a narrow particle size distribution. , low cost of raw materials, simple method

Active Publication Date: 2012-06-20
SUZHOU WIN BIO TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has strict requirements on the condition control of each step in the preparation, is not easy to operate and has limited output, or the content of magnetic nanoparticles in the composite material is limited and the distribution is uneven.
[0004] In order to solve the above problems, we proposed a ternary composite material based on a nested core-shell structure of silica / magnetic hybrid shell / polymer core, combined with a simple and feasible sol-gel method, and selected different types of porogens, The porogen and the polymer core are removed in one step by thermal ablation or solvent dissolution, and a mesoporous silica hollow microsphere with magnetic nanoparticles embedded in the shell is prepared. This method can overcome the above shortcomings; the material has regular The pore structure and cavity of the inorganic mesoporous silica material evenly embed a lot of magnetic nanoparticles, and there is no similar report at home and abroad.

Method used

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  • Preparation method for mesoporous silicon oxide hollow microspheres with magnetic nanoparticles embedded in shell layers
  • Preparation method for mesoporous silicon oxide hollow microspheres with magnetic nanoparticles embedded in shell layers
  • Preparation method for mesoporous silicon oxide hollow microspheres with magnetic nanoparticles embedded in shell layers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 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 3.86 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 Nanoparticles, 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 0.104 g of SDS in 40 g of deionized water, dissolve 9 g of styrene monomer, 0.4 g of sixteen The dispersion of alkane, 1 g TEOS, and 55 mg magnetic particles was mixed and ultras...

Embodiment 2

[0030] Example 2. The co-precipitation method was used to prepare the oleic acid-modified magnetic nano-particles, and the magnetic particles dispersed by n-octane and then evaporated to dryness were prepared. Dissolve 0.12 g SDBS in 40 g deionized water, mix 8 g styrene monomer, 0.4 g hexadecane, 2 g orthomethyl orthosilicate, and 80 mg magnetic particles into a homogeneous oil phase , and then mixed with an aqueous solution of surfactant, and ultrasonically finely emulsified at 500 W for 10 min. Add 1.0% potassium persulfate relative to styrene monomer, stir at room temperature and pass N 2 After 30 min, the reaction system was transferred to a water bath at a temperature range of 70 °C to initiate polymerization. After the polymerization was carried out for 90 min, 0.1 mL of ammonia water was added, and the reaction was carried out at 70 °C for 6 h; the product was used under the assistance of magnetic separation. Wash with deionized water repeatedly 2-3 times. Dispers...

Embodiment 3

[0031] Example 3. The co-precipitation method was used to prepare the oleic acid-modified magnetic nano-particles, and the magnetic particles dispersed by n-octane and then evaporated to dryness were prepared. 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 of TEOS, and 55 mg of magnetic particles into a homogeneous oil phase, and then mix with the surface The aqueous solutions of the active agents were mixed and ultrasonically finely emulsified at 500 W for 10 min. Add 1.0% AIBN relative to styrene monomer, stir at room temperature and pass N 2 After 30 min, the reaction system was transferred to a water bath at a temperature range of 70 °C to initiate polymerization. After the polymerization was carried out for 60 min, 0.05 mL of 1% sodium hydroxide aqueous solution was added, and the reaction was carried out at 70 °C for 6 h; Wash with deionized water repeatedly 2-3 times with assistance. Disperse the template ...

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Abstract

The invention relates to a preparation method for mesoporous silicon oxide hollow microspheres with magnetic nanoparticles embedded in shell layers. In the invention, the magnetic nanoparticles are prepared by using a coprecipitation method, are subjected to oleic acid surface modification and then are dispersed in normal octane; an oil phase constructed by styrene monomer, cetane, normal octane dispersion of the magnetic nanoparticles, alkoxysilane and a silane coupling agent is mixed with a water phase which dissolves a surfactant; a fine emulsion liquid droplet system is obtained through pre-emulsification and fine emulsification processes; controlling formation of silicon oxide and phase separation of organic and inorganic components in the system to obtain a template with a nested structure during free radial polymerization of the liquid droplets by adding a base catalyst; based on the template, generating a raw material by taking long-chain alkyl silane coupling agent and alkoxysilane as mesoporous silicon oxide; performing one-step ablation to remove an inner core of a polymer and a pore forming agent; or by taking a cationic surfactant as the pore forming agent, removing the pore forming agent and the inner core of the polymer through a solvent dissolving method and obtaining the magnetic / mesoporous silicon oxide hollow composite microspheres. The composite microspheres have large specific surface area and good magnetic operability and can be used for application fields of biomedicine, environment, water treatment and the like.

Description

field of invention [0001] The invention belongs to the technical field of preparation of inorganic nanocomposite materials, and in particular relates to a preparation method of mesoporous silicon oxide hollow microspheres embedded with magnetic nanoparticles in a shell layer. Background technique [0002] As an emerging material, mesoporous materials have very important applications in the fields of photochemistry, catalysis, environmental water treatment, bioseparation and drug loading, and are one of the hotspots of current research. Mesoporous materials refer to porous materials with a pore size of 2.0-50 nm, such as aerogel, columnar clay, M41S, and SBA series materials. Due to its large specific surface area, extremely uniform and adjustable pore size, and the characteristics of ordered dimensions, it has unique advantages in application compared with some traditional materials. In recent years, great progress has been made in the synthesis of mesoporous silica materia...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/02C01B33/113H01F1/11
Inventor 王祎龙唐玉霖王方英凯
Owner SUZHOU WIN BIO TECH CO LTD
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