Simple method for synthesizing porous magnetic ferroferric oxide (Fe3O4) microspheres

A technology of magnetic microspheres and ferric iron, applied in the direction of iron oxide/hydroxide, iron oxide, etc., can solve the problems of high energy consumption and high equipment requirements, and achieve low production cost, simple equipment, and high production efficiency. high rate effect

Inactive Publication Date: 2012-06-20
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Nevertheless, the thermal reduction method still requires high temperature and high pressure to be realized, which not only consumes a lot of energy in industrial production, but also requires relatively high equipment requirements.

Method used

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  • Simple method for synthesizing porous magnetic ferroferric oxide (Fe3O4) microspheres
  • Simple method for synthesizing porous magnetic ferroferric oxide (Fe3O4) microspheres
  • Simple method for synthesizing porous magnetic ferroferric oxide (Fe3O4) microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 3.5mmol of PVA (polymerization degree: 1700) and 35ml of secondary water into the three-necked bottle, heat to dissolve and cool down, add 40mmol of urea, seal, pump-fill with N 2 Four times to make the system completely free of oxygen, then add 5mmol FeCl 3 .6H 2 O and 2.5 mmol FeCl 2 .4H 2 O, after the solid is completely dissolved, in N 2 Heated to 85°C under protection, and reacted at this temperature for 48 hours to obtain a black precipitate, which was washed with water and absolute ethanol respectively, and dried under vacuum at 40-60°C overnight to obtain dry black Fe 3 o 4 The yield of solids was 95.8%. The product is about 100nm magnetic microspheres.

[0018] Under the same conditions, the amount of PVA was changed to 0.52mmol, 0.7mmol and 1.75mmol respectively to obtain magnetic microspheres with particle diameters of 280nm, 230nm and 150nm. That is, as the amount of PVA increases, the particle size of the magnetic microspheres becomes smaller.

Embodiment 2

[0020] Add 1.75mmol (calculated as repeating units, the same below) of PVA (polymerization degree: 1700) and 35ml of secondary water into the three-neck flask, heat to dissolve and then cool, add 40mmol of urea, seal, pump-fill with N 2 Four times to make the system completely free of oxygen, then add 5mmol FeCl 3 .6H 2 O, 2.5mmol FeCl 2 .4H 2 O and 3.5mmol acetic acid, after the solid is completely dissolved, in N 2 Heated to 85°C under protection, and reacted at this temperature for 48 hours to obtain a black precipitate, which was washed with water and absolute ethanol respectively, and dried under vacuum at 40-60°C overnight to obtain dry black Fe 3 o 4 The yield of solids was 97.2%. The product is loose and porous magnetic microspheres with a diameter of about 250 nm.

[0021] Under the same conditions, the amount of acetic acid was changed to 1.75mmol and 7mmol to obtain magnetic microspheres with a particle size of 210nm and 300nm, respectively, that is, the parti...

Embodiment 3

[0023] Add 1.75mmol of PVA (polymerization degree is 1700), 35ml of secondary water into the three-necked bottle, heat to dissolve and cool, add 40mmol of urea, seal, pump-fill with N 2 Four times to make the system completely free of oxygen, then add 5mmol FeCl 3 .6H 2 O, 2.5mmol FeCl 2 .4H 2 O and 3.5mmol acetic acid, after the solid is completely dissolved, in N 2 Heated to 80°C under protection, and reacted at this temperature for 72 hours to obtain a black precipitate, which was washed with water and absolute ethanol respectively, and dried in vacuum at 40-60°C overnight to obtain dry black Fe 3 o 4 The yield of solids was 93.4%. The product is loose and porous magnetic microspheres with a diameter of about 250 nm.

[0024] Compared with Example 2, it can be seen that the lower the reaction temperature, the slower the decomposition of urea, and the formed Fe 3 o 4 The larger the particle size of the magnetic microspheres.

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Abstract

The invention relates to a simple method for synthesizing porous magnetic ferroferric oxide (Fe3O4) microspheres. The porous magnetic Fe3O4 microspheres are formed by making ferrous ion salt and ferric ion salt as ferrum raw materials react in aqueous solution at 80-95 DEGC for 20-72h under the protection of N2, wherein the urea is used as the alkaline precipitating agent, and the polyvinyl alcohol and the acetic acid are used as the stabilizing agents. By changing the addition amount of the polyvinyl alcohol and the acetic acid, the grain size of the Fe3O4 microspheres can be effectively controlled. The porous magnetic Fe3O4 microspheres can disperse stably in water for 2 days and has good application prospect in the biomedical filed. The simple method for synthesizing the porous magnetic Fe3O4 microspheres has the advantages of cheap and readily available raw materials, mild reaction condition, good repeatability, high yield and simple equipment, is green and pollution-free and is easy to realize large-scale production.

Description

【Technical field】 [0001] The invention relates to a method for synthesizing porous ferroferric oxide magnetic microspheres, belonging to the technical field of inorganic material preparation technology. 【Background technique】 [0002] Magnetic nanomaterials have always been one of the hot research topics of researchers, and they are widely used in many fields such as catalysis, bioseparation, magnetic resonance imaging and targeted drug delivery. while Fe 3 o 4 Magnetic nanoparticles have attracted much attention due to their unique properties such as good biocompatibility, stability and low toxicity. Currently, the most commonly used synthetic Fe 3 o 4 The methods of magnetic nanoparticles mainly include alkaline co-precipitation method and thermal decomposition method of organometallic complexes. These methods can obtain Fe with relatively uniform particle size. 3 o 4 Magnetic nanoparticles, but the obtained nanoparticles tend to be smaller in size and weaker in magn...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/08
Inventor 阎虎生杨婵
Owner NANKAI UNIV
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