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Preparation method for superparamagnetism ferroferric oxide sub-micron hollow microsphere

A ferroferric oxide and superparamagnetic technology, which is applied in the direction of iron oxide/iron hydroxide, magnetic properties of inorganic materials, ferrous oxides, etc., can solve the problems of low saturation magnetization, poor biocompatibility, easy collapse, etc. problems, to achieve the effect of excellent oxidation resistance, high saturation magnetization, and cost minimization

Inactive Publication Date: 2014-03-26
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, there have been many reports on the preparation of superparamagnetic ferric oxide submicron hollow microspheres. For example, Peng and Sun (Angew Chem2007,46,4155) synthesized microspheres with superparamagnetic ferric oxide, but the dispersion It is not good and the saturation magnetization is low; Yu et al. and Wang et al. used Dodecylamine (DDA) and 1,6-hexanediamine as surfactants respectively, and prepared micelles as soft templates to prepare tetroxide Tri-iron hollow magnetic microspheres, but this kind of soft template often needs to rely on a large amount of organic substances, which is easy to form pollution and has poor biocompatibility, which is not conducive to biomedical applications; Huang et al. used hydrophilic modified polystyrene (Polystyzene, PS ) spheres as hard templates, and ferroferric oxide mesoporous microspheres were prepared by deposition-calcination. This hard template method is easy to popularize, universal and relatively easy to control, but the disadvantage is that it needs to undergo multi-step complex operations and the obtained microspheres Poor spherical shape, easy to collapse, low saturation magnetization

Method used

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  • Preparation method for superparamagnetism ferroferric oxide sub-micron hollow microsphere
  • Preparation method for superparamagnetism ferroferric oxide sub-micron hollow microsphere
  • Preparation method for superparamagnetism ferroferric oxide sub-micron hollow microsphere

Examples

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Embodiment 1

[0020] 8mmol trisodium citrate, 4mmolFeCl 3 .6H 2 O, 12 mmol NH 4 HCO 3 Dissolve in 80ml of distilled water, stir to dissolve with a magnet, add 2×10 -4 mmol polyacrylamide (PAM) and 1×10 -4 mmol polyethylene glycol (PEG). After the dissolution is complete, move it into a 100ml reaction kettle, react in an oven at 220°C for 8 hours, cool to room temperature and age, then wash twice with distilled water and absolute ethanol, centrifuge, and place in a vacuum oven at 50°C Dry to obtain the product.

[0021] The ferric iron tetroxide submicron hollow microsphere of the present invention is subjected to X-ray powder diffraction (XRD), and the result is obtained by figure 1 It can be seen that all diffraction peaks are related to Fe 3 o 4 (JCPDS79-0419) corresponds, Fe does not appear 2 o 3 The characteristic diffraction peaks (110), (210), (211), etc., indicate that the product is pure Fe 3 o 4 . Scanning electron microscopy (SEM) and transmission electron microscopy ...

Embodiment 2

[0023] 10mmol trisodium citrate, 4mmol FeCl 3 .6H 2 O, 8 mmol NH 4 Dissolve AC in 60ml of distilled water, stir and dissolve with a magnet, add the same amount of PAM and PEG as the surfactant in the above Example 1, and after the dissolution is complete, transfer it into a 100ml reactor, and react in an oven at 220°C for 8 hours , cooled to room temperature and aged, then washed twice with distilled water and absolute ethanol, centrifuged, and dried in a vacuum oven at 50°C to obtain the product. The morphology and properties of the obtained product are similar to Example 1.

Embodiment 3

[0025] 8mmol trisodium citrate, 4mmol FeCl 3 .6H 2 O. Dissolve 6 mmol of urea in 60 ml of distilled water, stir and dissolve with a magnet, add the same amount of PAM and PEG as the surfactant in Example 1 above, and after the dissolution is complete, transfer it to a 100 ml reaction kettle and react in an oven at 180°C , reacted for 8 hours, cooled to room temperature and aged, then washed twice with distilled water and absolute ethanol, centrifuged, and dried in a vacuum oven at 50°C to obtain the product. The morphology and properties of the obtained product are similar to Example 1.

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Abstract

The invention relates to a preparation method for a superparamagnetism ferroferric oxide sub-micron hollow microsphere. The preparation method comprises the following steps: 1) taking a reducing agent, an iron source and an alkali source, and dissolving into distilled water; 2) dissolving a surfactant into a solution obtained from step 1); 3) introducing a solution obtained from step 2) into a reaction kettle, reacting in a drying oven, performing natural cooling to room temperature for seasoning, water washing, alcohol washing, and drying in a vacuum drying box, so that the superparamagnetism ferroferric oxide sub-micron hollow microsphere is obtained. The preparation method has the following good effects: 1) according to the invention, the ferroferric oxide sub-micron hollow microsphere is compounded, and has superparamagnetism, high saturation magnetization and excellent oxidation resistance; 2) dispersing agents such as PEG (polyethylene glycol) and PVP (polyvinylpyrrolidone) are adopted to solve the problem of magnetic microsphere agglomeration, so that the ferroferric oxide sub-micron hollow microsphere with uniform particle size is obtained; 3) according to the invention, adopted raw materials is cheap, so that cost is minimized.

Description

technical field [0001] The invention relates to a preparation method of superparamagnetic iron ferric oxide submicron hollow microspheres. Background technique [0002] As a kind of magnetic material, ferroferric oxide has biocompatibility, hydrophilicity, magnetic responsiveness, non-toxicity and good chemical stability, and is widely used in biomedicine (such as magnetic targeting, bioseparation, Tumor magnetic hyperthermia, MRI contrast agent, immune detection, etc.). People use chemical co-precipitation method, organic pyrolysis method, microemulsion method, etc. to prepare ferroferric oxide microspheres with various shapes, among which the hollow ferroferric oxide microspheres have low density, high specific surface characteristics, and high saturation Magnetization, and its hollow part can accommodate a large number of guest molecules and large-sized guests, making it have important application prospects in many technical fields such as microwave absorbing materials a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/08H01F1/11
Inventor 戴红莲许文艳韩颖超李世普
Owner WUHAN UNIV OF TECH
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