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Ferroferric oxide @ silicon dioxide magnetic single-hole hollow microsphere and preparation method thereof

A technology of fe3o4 and microspheres, which is applied in the direction of microsphere preparation, microcapsule preparation, and magnetic properties of inorganic materials. It can solve the problems of not using high loading capacity, etc., and achieve good chemical stability, good stability, and uniform size of microspheres Effect

Inactive Publication Date: 2014-02-05
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If the microspheres are used as a carrier to carry functional materials, it is not necessary to obtain high loading capacity.

Method used

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  • Ferroferric oxide @ silicon dioxide magnetic single-hole hollow microsphere and preparation method thereof
  • Ferroferric oxide @ silicon dioxide magnetic single-hole hollow microsphere and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Fe 3 o 4 The preparation of nanoparticles adopts the following method: 8.1g FeCl 3 ·6H 2 O and 4.17 g FeSO 4 ·7H 2 O was dissolved in 90 mL of ultra-pure water to form a solution, heated to 55 °C after 30 min of nitrogen gas and kept at a constant temperature, and 50 mL of sodium hydroxide solution (3.0 mol / L) was added dropwise. After the sodium hydroxide solution is added dropwise, adjust the temperature to 65°C, and react at a constant temperature for one hour under a nitrogen atmosphere, then raise the temperature to 90°C, react at a constant temperature for 30 minutes, and finally turn off the heating and cool to room temperature. Separation of Fe using a magnet 3 o 4 Crystal, after the precipitation is complete, pour out the supernatant, and prepare the obtained Fe 3 o 4 transferred to a beaker, washed several times with pure water, and then washed with absolute ethanol, the obtained Fe 3 o 4 The muddy solid was vacuum dried to obtain Fe 3 o 4 Nanopart...

Embodiment 2

[0027] Fe 3 o 4 Preparation of nanoparticles and Fe 3 o 4 The surface modification of nanoparticles adopts the method in Example 1.

[0028] Adopt the method of embodiment 1 to configure DTS-Fe 3 o 4 / THF solution, and adjust its concentration to 1.0g / L.

[0029] Take 0.1mL DTS-Fe 3 o 4 / THF solution was mixed with 0.5mL of polystyrene (PS) THF solution (12.5g / L), and then 3.4mL of THF, 0.1mL of TEOS and 4mL of MeCN were added sequentially, and the mixture was mixed evenly, Quickly add 30mL water, then add CTAB / H 2 O (0.2 mL, 0.01 mol / L), mix well, add 0.5mL ammonia water, and let it stand for one day. Centrifuge to separate the precipitate, then add THF to dissolve the polymer, and finally centrifuge again to obtain Fe 3 o 4 SiO 2 Magnetic single-hole hollow microspheres. Get Fe 3 o 4 SiO 2 The scanning electron micrograph of the magnetic single-hole hollow microsphere is similar to Example 1. The average particle size of the microspheres is 302±65 nm. SiO ...

Embodiment 3

[0031] Fe 3 o 4 Preparation of nanoparticles and Fe 3 o 4 The surface modification of nanoparticles adopts the method in Example 1.

[0032] Adopt the method of embodiment 1 to configure DTS-Fe 3 o 4 / THF solution, and adjust its concentration to 1.0g / L.

[0033] Take 0.5mL DTS-Fe 3 o 4 / THF solution was mixed with 0.25 mL of polystyrene (PS) THF solution (12.5 g / L) and 0.25 mL of polymethyl methacrylate (PMMA) THF solution (12.5 g / L), and then added sequentially 3mL of THF, 0.1mL of TEOS and 4mL of MeCN, after mixing the mixture evenly, quickly add 30mL of water, then add CTAB / H 2 O (0.2 mL, 0.01 mol / L), mix well, add 0.5mL ammonia water, and let it stand for one day. Centrifuge to separate the precipitate, then add THF to dissolve the polymer, and finally centrifuge again to obtain Fe 3 o 4 SiO 2 Magnetic single-hole hollow microspheres. Get Fe 3 o 4 SiO 2 The scanning electron micrograph of the magnetic single-hole hollow microsphere is similar to Example 1. ...

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Abstract

The invention discloses a ferroferric oxide @ silicon dioxide magnetic single-hole hollow microsphere and a preparation method thereof. The ferroferric oxide @ silicon dioxide magnetic single-hole hollow microsphere is characterized in that a hollow microsphere shell is a mixture of silicon dioxide and ferroferric oxide nano particles; the ferroferric oxide nano particles are dispersed in silicon dioxide substrate randomly; the shell is provided with a large hole; an empty chamber which is in an exocentric structure is formed inside the microsphere; the large hole which is formed in the shell is communicated with the microsphere empty chamber; the average grain diameter of the above hollow microsphere is between 200 and 2Mum; the size of the large hole which is formed in the shell is between 16 to 500 nm; a distribution range of the size of the empty chamber is between 50 and 1.5Mum. The preparation method of the ferroferric oxide @ silicon dioxide magnetic single-hole hollow microsphere comprises adding hydrophobization ferroferric oxide nano particles which contain hydrophobic organic polymers and an organic solution of a silicon dioxide precursor into water, mixing with catalyzer, generating into the polymer- ferroferric-oxide nano particle- silicon-dioxide composited microsphere after standing reaction for a period of time, separating the composited microsphere and removing the organic polymers to obtain the ferroferric oxide @ silicon-dioxide magnetic single-hole hollow microsphere. The ferroferric oxide @ silicon dioxide magnetic single-hole hollow microsphere can be used for embedding and conveying macromolecules and nano particles and has vast application prospect in biomedical fields such as targeted drugs and biological macromolecular carriers.

Description

technical field [0001] The invention relates to an inorganic hollow microsphere and a preparation method thereof, in particular to a Fe with a large single hole in the shell wall. 3 o 4 SiO 2 Hollow microsphere and its preparation method. Background technique [0002] Magnetic nanomaterials have unique application value in fields such as industry, biomedicine, and electronic information. In the field of biomedicine, the application range of magnetic nanomaterials includes targeted drug carriers, magnetic hyperthermia, cell screening and separation, magnetic resonance imaging, immunoassay, radioimmunolabeling of magnetic particles, etc. Among them, Fe 3 o 4 Magnetic nanocrystals have the advantages of being non-toxic, degradable and metabolizable in vivo, and can be easily manipulated under a magnetic field. They have been widely used in biomedical research. Combining magnetic nanoparticles with polymers or inorganic oxides can form magnetic microspheres. Compared with...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01F1/11H01F1/36B01J13/02
Inventor 符小艺刘婧婧
Owner SOUTH CHINA UNIV OF TECH
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