Hollow microsphere with superparamagetism Fe3O4 nanocrystallines and preparation method thereof

A superparamagnetic and nanocrystalline technology, which is applied in the field of hollow microspheres and its preparation, can solve the problems of complex and cumbersome process, low efficiency, and long time consumption, and achieve the effect of simple preparation method, good stability and low cost

Inactive Publication Date: 2010-06-09
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method requires pre-prepared template microspheres, which need to be porous, and then can be further used to load ferric oxide nanoparticle

Method used

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  • Hollow microsphere with superparamagetism Fe3O4 nanocrystallines and preparation method thereof
  • Hollow microsphere with superparamagetism Fe3O4 nanocrystallines and preparation method thereof
  • Hollow microsphere with superparamagetism Fe3O4 nanocrystallines and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 12mL 0.5mol / L FeCl 3 Aqueous solution and 6mL 0.5mol / L FeSO 4 The aqueous solution was mixed, and nitrogen gas was passed for 30 minutes to remove oxygen; after the temperature was raised to 55 ° C, 10 mL of 3M NaOH aqueous solution was added dropwise, and then the temperature of the reaction system was raised to 65 ° C, and the reaction was kept for 1 hour; then the temperature was raised to 90 ° C, Keep warm for 30 minutes. After cooling to room temperature, the as-prepared Fe was separated using a magnet 3 o 4 Nanocrystals were washed sequentially with water and ethanol, and dried in vacuum.

[0036] 1g Fe 3 o 4 Disperse nanocrystals in 40mL ethanol, add 0.2mL dodecyltrimethylsilane DTS, pass nitrogen gas for 30 minutes to remove oxygen, then reflux for 6 hours under nitrogen atmosphere; after cooling to room temperature, use magnet to separate nanocrystals, ethanol Washed 3 times and dried in vacuum to obtain DTS-modified Fe 3 o 4 Nanocrystalline, labeled Fe...

Embodiment 2

[0041] 1g Fe 3 o 4 Nanocrystals dispersed at a concentration of 1.0×10 -2 mol / L ethanol solution of phenyltrimethoxysilane (PTS), in N 2 Reflux for 2 h under protection, separate the nanocrystals after cooling to room temperature, wash with ethanol and dry to obtain PTS-modified Fe 3 o 4 Nanocrystalline, labeled Fe 3 o 4 -PTS.

[0042] In 4 mL of methyl methacrylate-styrene copolymer (P(MMA-co-St) with a concentration of 10 g / L in acetonitrile, 100 μL TEOS and 10 mg Fe 3 o 4 -HDTS mixed, sonicated for 10 minutes to make Fe 3 o 4 -PTS is fully dispersed to obtain solution A2. Pour this mixed solution into 16mL with a concentration of 2.0×10 -3 mol / L dodecyltrimethoxyammonium chloride aqueous solution B2. Add 0.4 mL of 28% ammonia water and react for 12 hours. Separation of embedded Fe by magnet 3 o 4 The nanocrystalline composite microspheres were washed with water and ethanol in turn, and dried at 50°C. The composite microspheres were soaked in 5mL of acetonitr...

Embodiment 3

[0045] 1g Fe 3 o 4 Nanocrystals dispersed at a concentration of 1.0×10 -2 mol / L of octyltriethoxysilane (OTS) ethanol solution, in N 2 Under protection, reflux for 10 h, cool to room temperature, separate the nanocrystals, wash with ethanol and dry to obtain the hydrolyzed OTS-modified Fe 3 o 4 Nanocrystalline, labeled Fe 3 o 4 -OTS.

[0046] Add 100 μL TEOS and 20 mg Fe 3 o 4 -OTS mixed, sonicated for 15 minutes to make Fe 3 o 4 -OTS is fully dispersed to obtain solution A3. Pour this mixed solution into 16mL with a concentration of 2.0×10 -3 mol / L of octyltrimethoxyammonium bromide aqueous solution B3. Add 0.4 mL of 28% ammonia water and react for 12 hours. Separation of embedded Fe by magnet 3 o 4The nanocrystalline composite microspheres were washed with water and ethanol in turn, and dried at 50°C. The composite microspheres were soaked in 5mL THF and stirred for 6 hours to dissolve the PS and diffuse out of the microspheres, the magnets separated the micr...

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Abstract

The invention discloses a hollow microsphere with superparamagetism Fe3O4 nanocrystallines and a preparation method thereof. The hollow microsphere takes a silica shell as a casing, the thickness of the silica shell is 10-50nm, and the silica shell contains Fe3O4 nanocrystallines which contains hydrophobicity. The preparation method is as follows: dispersing the hydrophobic Fe3O4 nanocrystallines in an organic solution of silica precursor Si(OR)4 and hydrophobic high molecular by adopting a precipitating-phase separating method; adding water solution containing an surfactant; embedding the Fe3O4 nanocrystallines and the Si(OR)4 to form a compound microsphere by using the quick precipitation of the high molecular; adding ammonia water to catalyze the Si(OR)4 for hydrolytie polycondensation to form a SiO2 shell on the surface of the microsphere; and removing the high molecular by dissolving by a solvent. The hollow microsphere in the invention has superparamagetism, and has wide application prospect in the biomedical field like targeted drug carriers and the like.

Description

technical field [0001] The invention relates to a hollow microsphere and a preparation method thereof, specifically a hollow microsphere with superparamagnetic Fe inside 3 o 4 Nanocrystalline silicon dioxide hollow microspheres and a preparation method thereof. Background technique [0002] Hollow microspheres refer to a class of spherical shell materials with a size ranging from nanometers to micrometers and internal cavities. Compared with dense materials of the same size, hollow microspheres have the characteristics of low density and large specific surface area. In addition, because of its internal cavity structure, its sound insulation and heat insulation properties are good, and it can be loaded with a variety of functional materials. These characteristics make hollow microspheres widely used in scientific research and industrial and agricultural production. Silica has the advantages of high temperature resistance, good mechanical and acid stability, good biocompati...

Claims

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Application Information

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IPC IPC(8): B01J13/02C04B35/624H01F1/11
Inventor 符小艺何新华谢民强
Owner SOUTH CHINA UNIV OF TECH
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