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Preparation method of ferroferric oxide nanoparticles

A technology of ferroferric oxide and nanoparticles, which is applied in the direction of iron oxide/iron hydroxide, nanotechnology, ferrous oxide, etc., and can solve the problem of wide particle size distribution range and fine particle size of nanometer ferric oxide particles. It is difficult to meet the requirements of nanoscale and uneven particle size distribution, and achieve the effect of low price, convenient large-scale production, and easy control of operating conditions

Inactive Publication Date: 2012-11-28
LUOYANG NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation of nano-ferric oxide by ball milling has good reproducibility and simple operation, but the production cycle is long, the particle size refinement is difficult to meet the nano-scale requirements, and the particle size distribution is uneven, and it is easy to be oxidized during the preparation process; the microemulsion method prepared Nanoparticles have small particle size and good monodispersity, but the surfactants, co-surfactants and oils introduced in the synthesis process have to be washed repeatedly with organic solvents, and it is not easy to remove; although the hydrothermal method can control the crystal structure of nanoparticles and purity, but because the reaction is carried out in a high-pressure reactor, the equipment requirements are relatively high, resulting in high costs; the sol-gel method prepares nano-ferric oxide with various crystal forms; the vapor deposition method is costly and difficult to operate The common co-precipitation process is simple and can synthesize iron ferric oxide nanoparticles in a large amount, but it is difficult to control the particle size and particle size distribution of the product. The prepared nano ferric oxide particle size distribution range is wide and does not have good dispersion. properties, and during the preparation process, the proportion of the reaction changes due to the fact that ferrous ions are easily oxidized to ferric ions in the air

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preparation example Construction

[0024] A preparation method of iron ferric oxide nanoparticles, the particle size of iron ferric oxide nanoparticles is 14.0-19.0 nm, the steps of the preparation method are:

[0025] Step 1. Take 0.01 mol-0.03 mol ferric ammonium sulfate and ferrous ammonium sulfate respectively according to the molar ratio, and add ferric ammonium sulfate and ferrous ammonium sulfate to 40-120 ml with a molar concentration of 0.1-1.5 mol L -1 in the sodium sulfate solution, put it into a mixer, and stir for 10-20 minutes at a speed of 200-300 rpm to obtain a dispersion mixture of iron source and ferrous source, and set aside;

[0026] Step 2: Take 0.02-0.03 mol of sodium hydroxide in molar ratio, and add sodium hydroxide to 30-45 ml with a molar concentration of 0.1-1.5 mol L -1 In the sodium sulfate solution, put it in the mixer, stir for 10-20 minutes with the rotating speed of 200-300 rev / min, make the alkali source dispersion solution, set aside;

[0027] Step 3: Heat the alkali source ...

Embodiment 1

[0035]A preparation method of iron ferric oxide nanoparticles, comprising the steps of:

[0036] Step 1. Take 0.01 mol ferric ammonium sulfate and 0.01 mol ferrous ammonium sulfate in molar ratio, and add ferric ammonium sulfate and ferrous ammonium sulfate to 40 ml with a molar concentration of 0.1 mol L -1 in the sodium sulfate solution, put it into a mixer, and stir it for 10 minutes at a speed of 200 rpm to obtain a dispersed mixed solution of iron source and ferrous source, and set aside;

[0037] Step 2: Take 0.02 mol of sodium hydroxide in molar ratio, and add sodium hydroxide to 30 ml with a molar concentration of 0.1 mol L -1 in the sodium sulfate solution, put it into the mixer, and stir for 10 minutes with the rotating speed of 200 rev / min to prepare the alkali source dispersion solution, and set aside;

[0038] Step 3: Heat the alkali source dispersion solution to 80°C, add the iron source and ferrous source dispersion mixed solution while stirring, stir until bla...

Embodiment 2

[0044] A preparation method of iron ferric oxide nanoparticles, comprising the steps of:

[0045] Step 1. Take 0.01 mol ferric ammonium sulfate and 0.02 mol ferrous ammonium sulfate in molar ratio, and add ferric ammonium sulfate and ferrous ammonium sulfate to 80 ml with a molar concentration of 0.5 mol L -1 In the sodium sulfate solution, put in the mixer, stir with the rotating speed of 200 revs / min for 13 minutes, obtain the dispersion mixed solution of iron source and ferrous source, for subsequent use;

[0046] Step 2: Take 0.02 mol of sodium hydroxide in molar ratio, and add sodium hydroxide to 30 ml with a molar concentration of 0.5 mol L -1 In the sodium sulfate solution, put into the mixer, stir for 13 minutes with the rotating speed of 200 revs / min, make alkali source dispersion solution, for subsequent use;

[0047] Step 3. Heat the alkali source dispersion solution to 83°C, add the iron source and ferrous source dispersion mixed solution while stirring, stir unti...

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Abstract

The invention relates to a preparation method of ferroferric oxide nanoparticles, relating to the field of preparation of inorganic non-metallic nano materials. The preparation method comprises the steps of: firstly, preparing a mixed dispersion solution of a ferric source and a ferrous source and a dispersion solution of an alkali source, adding the prepared mixed dispersion solution of the ferric source and the ferrous source into the dispersion solution of the alkali source, stirring for reaction for 50-70min to generate black precipitates in a reaction process, delivering reactants to a centrifuger, washing the separated precipitates sequentially with distilled water, a water-alcohol solution and absolute ethyl alcohol, centrifuging, separating and drying to obtain ferroferric oxide nanoparticles. In the invention, a used reaction solvent has the advantages of low cost and no toxicity and harmfulness, can be recycled and has no environment pollution problem; and used equipment is simple, operation conditions are easy to master, and thus, large-scale production is convenient.

Description

technical field [0001] The invention relates to a preparation method of nanomaterials, in particular to a preparation method of iron ferric oxide nanoparticles, belonging to the field of preparation of inorganic nanomaterials. Background technique [0002] In recent years, nanotechnology has developed rapidly, and nanomaterials have attracted more and more attention because of their unique properties different from ordinary materials. [0003] Ferroferric oxide nanoparticles have a unique structure, good magnetic properties and biocompatibility, and are widely used in the fields of magnetic media storage, magnetic fluid, catalysis, magnetic pigments and biomedicine. Especially in the field of biomedicine, ferric iron tetroxide nanoparticles have great potential in magnetic immune cell separation, cell therapy, tissue repair, targeted drug delivery, tumor hyperthermia therapy and magnetic embolization therapy, magnetic response imaging, enzyme immobilization and immunodetect...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G49/08B82Y40/00
Inventor 胡少强王桂霞杨卓张永花郭文博
Owner LUOYANG NORMAL UNIV
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