Method for preparing water-soluble nanometer iron oxide

A ferroferric oxide, water-soluble technology, applied in the field of materials, can solve the problems of easy aggregation of particles, low zeta potential, uneven particle size dispersion, etc., and achieve less surface ligands, simple equipment, and uniform particle size Effect

Inactive Publication Date: 2012-07-11
THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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  • Abstract
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Problems solved by technology

The co-precipitation method refers to the hydrolysis of iron salts under alkaline conditions, and the prepared nanoparticles are water-soluble, but the crystal form is poor, the particle size dispersion is generally uneven, the surface zeta potential is relatively low, and the particles are easy to agglomerate. Together; the high-temperature thermal decomposition method is to decompose iron precursors, such as iron acetylacetonate, iron pentacarbonyl and iron oleate, at high temperature (generally greater than 250°C) in the presence of surfactant oleylamine, etc. etc. The prepared nanoparticles have good crystal form and uniform particle size distribution, but they are oil-soluble and cannot be directly applied in the field of biomedicine. Ligands, it takes a long time to get water-soluble nanoparticles

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  • Method for preparing water-soluble nanometer iron oxide
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  • Method for preparing water-soluble nanometer iron oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1) Add 0.5g of iron(III) acetylacetonate and 20mL of benzyl alcohol solution into a 100mL three-necked reaction flask, stir to dissolve them, in an open system, raise the temperature to 190°C at a rate of 6°C / min, and react for 2h. A black ferric oxide nanoparticle crystal with a mass of about 0.11 g was prepared.

[0029] Such as figure 1 As shown, the X-ray diffraction figure shows that the black solid prepared in the present embodiment is ferric oxide nanocrystal; the transmission electron microscope figure of the magnetic ferric oxide nanocrystal of preparation is as follows figure 2 As shown in A, it can be seen from the transmission electron microscope image that the size distribution of the nanocrystals is relatively uniform, and the diameter is about 6.8 nm.

[0030] 2) Take 1 mL of ferric oxide nanoparticles (about 5 mg) wrapped in benzyl alcohol, use magnetic separation, add appropriate amount of ethanol to wash, and use magnetic separation again, repeat twi...

Embodiment 2

[0035] 1) Add 0.5g of iron(III) acetylacetonate and 20mL of benzyl alcohol solution into a 100mL three-necked reaction flask, stir to dissolve them, pass nitrogen gas to remove oxygen for 30min, and carry out the following reactions under nitrogen atmosphere at 6°C / min The speed was increased to 190° C., and the reaction was carried out for 2 hours to produce black iron ferric oxide nanoparticle crystals with a mass of about 0.11 g and a particle size of about 5 nm.

[0036] 2) Take 1 mL of ferric oxide nanoparticles (about 5 mg) wrapped in benzyl alcohol, use magnetic separation, add appropriate amount of ethanol to wash, and use magnetic separation again, repeat twice.

[0037] 3) Add 5 mL of 0.2M phosphate double salt solution, and ultrasonicate at room temperature for 5 minutes to obtain a uniform and transparent iron ferric oxide nanocolloid solution.

Embodiment 3

[0039] 1) Add 0.5g of iron(III) acetylacetonate and 20mL of benzyl alcohol solution into a 100mL three-necked reaction flask, stir to dissolve them, in an open system, raise the temperature to 190°C at a rate of 6°C / min, and react for 2h. A black iron ferric oxide nanoparticle crystal with a mass of about 0.11 g and a diameter of about 6.8 nm was prepared. .

[0040] 2) Take 1 mL of ferric oxide nanoparticles (about 5 mg) wrapped in benzyl alcohol, use magnetic separation, add appropriate amount of ethanol to wash, and use magnetic separation again, repeat twice.

[0041] 3) Add 5 mL of 0.1 M phosphate double salt solution, and ultrasonicate at room temperature for 5 minutes to obtain a uniform and transparent iron ferric oxide nanocolloid solution.

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Abstract

The invention provides a method for preparing water-soluble nanometer iron oxide. The method comprises the following steps of: pyrolyzing iron acetylacetonate (III) by using alcohol to obtain iron oxide nanoparticles, and adding a ligand aqueous solution at room temperature to obtain the water-soluble nanometer iron oxide. The preparation method is simple, conditions are mild, the required equipment is simple, and batch production can be realized; and the nanoparticles prepared by the method have the size of 5 to 15nm, superparamagnetism, and wide application prospects in the field of biomedicine such as nuclear magnetic resonance imaging, magnetic thermal therapy, catalysis and the like.

Description

technical field [0001] The invention belongs to the field of materials, in particular, the invention relates to a preparation method of water-soluble nano ferric oxide Background technique [0002] Nano-iron ferric oxide is a magnetic nanomaterial with great application value in the field of biomedicine, which is generally prepared by co-precipitation or high-temperature pyrolysis. The co-precipitation method refers to the hydrolysis of iron salts under alkaline conditions, and the prepared nanoparticles are water-soluble, but the crystal form is poor, the particle size dispersion is generally uneven, the surface zeta potential is relatively low, and the particles are easy to agglomerate. Together; the high-temperature thermal decomposition method is to decompose iron precursors, such as iron acetylacetonate, iron pentacarbonyl and iron oleate, at high temperature (generally greater than 250°C) in the presence of surfactant oleylamine, etc. etc. The prepared nanoparticles h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/08B82Y40/00A61K49/06A61N2/00
Inventor 葛广路李学毅
Owner THE NAT CENT FOR NANOSCI & TECH NCNST OF CHINA
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