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A method for preparing oil-soluble iron ferric oxide nanoparticles by oil-water interface method

A technology of ferric oxide, oil-water interface method, applied in the direction of iron oxide/iron hydroxide, ferrous oxide, etc., can solve the problems of product purity not easy to be controlled, troublesome synthesis steps, poor particle dispersibility, etc. Achieve the effect of good particle uniformity and dispersion, easy operation and small particle size

Inactive Publication Date: 2011-12-07
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the raw materials required for synthesis are relatively expensive, the synthesis steps are cumbersome, and the purity of the product is not easy to control
In addition, the article titled "Facile Hydrothermal Synthesis of Iron Oxide Nanoparticles with Tunable Magnetic Properties" published in "Advanced Materials" ("Advanced Materials") 2009 Volume 113 13593 mainly has the following disadvantages. The method FeCl 2 Synthesized Fe 3 o 4 , but the synthesis uses a high-temperature and high-pressure reactor, the conditions are harsh, and the dispersibility of the produced particles is relatively poor, and the uniformity is not good

Method used

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  • A method for preparing oil-soluble iron ferric oxide nanoparticles by oil-water interface method
  • A method for preparing oil-soluble iron ferric oxide nanoparticles by oil-water interface method
  • A method for preparing oil-soluble iron ferric oxide nanoparticles by oil-water interface method

Examples

Experimental program
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Effect test

Embodiment 1

[0028] 1) Weigh 0.7g of ferric sulfate and dissolve it in 30ml of deionized water; Weigh 906.9g of sodium stearate and dissolve it into 60ml of aqueous solution under magnetic stirring and heating. The ferric sulfate solution was added dropwise to sodium stearate and reacted at 60°C for 30 minutes. After the reaction is over, the reactant is taken, filtered with a Buchner funnel, and washed 3 times with hot water. Put it in a blast drying box and dry for 24 hours.

[0029] (2) Weigh 2.715g of the above iron stearate solution, 0.003mol, and dissolve it in 40ml of cyclohexane. After heating to dissolve, a 0.075mol / L iron stearate solution is prepared. Then use a syringe to inject 5ml of oleic acid into a three-necked flask. Vacuum is maintained at -0.9Pa for 2 minutes. High-purity nitrogen gas was blown into it and maintained for 20 minutes under high-speed magnetic stirring (v=400rpm). Connect the reflux tube, keep the reactor in an oxygen-free state and pure nitrogen state, a...

Embodiment 2

[0034] (1) Weigh 0.35 g of ferric sulfate and dissolve in 30 ml of deionized water; weigh and dissolve 453.5 g of sodium stearate into 60 ml of aqueous solution under magnetic stirring and heating. The ferric sulfate solution was added dropwise to sodium stearate and reacted at 80°C for 40 minutes. After the reaction is over, the reactant is taken, filtered with a Buchner funnel, and washed 3 times with hot water. Put it in a blast drying box and dry for 24 hours.

[0035] (2) Weigh 1.375g of the above-mentioned iron stearate solution and dissolve it in 40ml of cyclohexane. After heating and dissolving, a 0.00375mol / L iron stearate solution is prepared. Then use a syringe to inject 2.5ml of oleic acid into a three-necked flask. Vacuum is maintained at -0.9Pa for 2 minutes. High-purity nitrogen gas was blown into it and maintained for 20 minutes under high-speed magnetic stirring (v=400rpm). Connect the reflux tube, keep the reactor in an oxygen-free state and pure nitrogen st...

Embodiment 3

[0040] (1) Weigh 0.7 g of ferric nitrate and dissolve in 30 ml of deionized water; weigh 1813.8 g of sodium stearate and dissolve it into 60 ml of aqueous solution under magnetic stirring and heating. The ferric sulfate solution was added dropwise to sodium stearate and reacted at 80°C for 40 minutes. After the reaction is over, the reactant is taken, filtered with a Buchner funnel, and washed 3 times with hot water. Put it in a blast drying box and dry for 24 hours.

[0041] (2) Weigh 2.715g of the above-mentioned iron stearate, 0.0015mol, and dissolve it into 40ml of cyclohexane. After heating and dissolving, a 0.00375mol / L iron stearate solution is prepared. Vacuum is maintained at -0.9Pa for 2 minutes. High-purity nitrogen gas was blown into it and maintained for 20 minutes under high-speed magnetic stirring (v=400rpm). Connect the reflux tube, keep the reactor in an oxygen-free state and pure nitrogen state, and stop stirring for 20 minutes to repel the gas in the reflux ...

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Abstract

The invention relates to a method for preparing oil-soluble ferroferric oxide nanoparticles by virtue of an oil-water interface, and the method comprises the following steps: synthesizing oil-soluble iron stearate from a water-soluble iron salt and a fatty acid salt and dispersing the oil-soluble iron stearate in a non-polar solvent to prepare an oil-phase reaction solution; mixing an aqueous phase, namely a water-soluble ferrous salt solution) with the oil phase, adding an oil-soluble surfactant, adding a water-soluble base solution into the oil-water system, stirring at a high speed, and reacting while condensing and refluxing; and after the reaction is finished, standing for layering, and collecting the upper-layer oil phase to finally prepare the ultra-fine oil-soluble ferroferric oxide nanoparticles. The method provided by the invention has the advantages of simplicity and convenience in operation, low production cost, short production period and good repeatability; and the prepared ferroferric oxide nanoparticles are monodisperse and have the advantages of excellent particle uniformity and dispersion property, very small particle size, high purity, no settlement when being dispersed in the oil phase for a long time, easiness in storage and the like.

Description

Technical field [0001] The invention belongs to the field of preparation of ferroferric oxide nanoparticles, and particularly relates to a method for preparing oil-soluble ferroferric oxide nanoparticles by an oil-water interface method. Background technique [0002] Fe 3 O 4 It is rich in natural magnetite and is widely distributed. Because of its abundant resources, low price, and good magnetism at room temperature, it has a wide range of uses in the fields of magnetic materials, pigments, etc. With the informatization of society and the application of nanotechnology, people are 3 O 4 His research has also completed a transition from macro to micro, particle size transition from micron, sub-micron to nano-size. This miniaturized nanotechnology has created conditions for the development of many fields. With ordinary Fe 3 O 4 Compared to nano Fe 3 O 4 Powder (particle size in the range of 5--100nm), should belong to the quasi-zero-dimensional category (size between atoms, molecu...

Claims

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Application Information

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IPC IPC(8): C01G49/08
Inventor 周兴平王会
Owner DONGHUA UNIV
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