Method for preparing superfine even Fe2O3

A uniform and nanotechnology, applied in the direction of nanotechnology, nanotechnology, nanostructure manufacturing, etc., can solve the problems of complex preparation process, expensive raw materials, and magnetic performance decline, and achieve no environmental pollutant emissions, simple process, and good dispersion and the effect of uniformity

Inactive Publication Date: 2007-10-10
HEBEI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example: D.K.Kim. used the co-precipitation method to obtain nano-Fe with a particle size of 13-60nm and different magnetic properties after surface treatment with sodium oleate. 3 o 4 (J.Magnetism MagneticMater.2001, 225, 30-36); An Lijuan et al. used co-precipitation method, and used oleic acid and sodium dodecylbenzene sulfonate as double-layer surfactants for surface modification, and obtained particle size 10nm stable water-dispersible nano-Fe 3 o 4 (Acta Chemical Journal of Chinese Universities, 2005, 26 (2), 366-369); Wang Hanbin etc. also adopt co-precipitation method, add citrate to control nano-Fe 3 o 4 The growth of Fe, with a particle size of less than 5nm 3 o 4 - particles, but the crystallization of the sample is not ideal (Journal of Inorganic Chemistry, 2004, 20(11), 1279-1283); in addition, Shufeng Si et al. 3 .6H 2 O and Fe powder are used as precursors. In the presence of oleic acid and dodecylamide, monodisperse Fe wi

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0012] Example 1

[0013] Add FeSO with a concentration of 1.0mol / L to the reactor 4 The solution is 50ml, while stirring, adjust the pH=9 with 6.0mol / L sodium hydroxide solution, and at the same time make the volume of the resulting suspension 100ml, add 30% H at room temperature 2 O 2 2.4ml, oxidized for 30min, can prepare amorphous δ-FeOOH suspension, add FeSO according to the ratio of δ-FeOOH precursor to Fe(II) as 1.85:1 4 The solution, then adjust the pH value of the system to 10 with sodium hydroxide solution, boil and reflux for 2h at 100°C, filter the product, wash it with water several times and then wash it with dilute ammonia water. After drying, about 18g of product can be obtained with a particle size of 51nm.

Example Embodiment

[0014] Example 2

[0015] Add FeSO with a concentration of 1.0mol / L to the reactor 4 Solution 10ml, add 40ml water, while stirring, adjust pH=8.7 with 6mol / l sodium hydroxide solution, and at the same time make the volume of the resulting suspension 100ml, add 30% H at room temperature 2 O 2 0.48ml, oxidized for 30min, can prepare amorphous δ-FeOOH suspension; add FeSO according to the ratio of δ-FeOOH precursor to Fe(II) to 1.47:1 4 The solution, then adjust the pH value of the system to 8 with sodium hydroxide solution, boil and reflux at 100°C for 2h, filter the product, wash it with water several times and then wash it with dilute ammonia water, and dry it to obtain 3.3g product with a particle size of 68nm.

Example Embodiment

[0016] Example 3

[0017] Add FeCl with a concentration of 1.0mol / L to the reactor 2 Solution 10ml, add 40ml water, while stirring, adjust pH=8.7 with 6mol / l sodium hydroxide solution, and at the same time make the volume of the resulting suspension 100ml, add 30% H at room temperature 2 O 2 0.48ml, oxidized for 30min, can prepare amorphous δ-FeOOH suspension; add FeCl according to the ratio of δ-FeOOH precursor to Fe(II) as 1.47:1 2 The solution, then adjust the pH value of the system to 13 with sodium hydroxide solution, boil and reflux at 100°C for 2h, filter the product, wash it with water several times and then wash it with dilute ammonia water. After drying, 3.4g of the product can be obtained with a particle size of 29nm.

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Abstract

This invention discloses a method for preparing uniform nanoscale Fe3O4. The method comprises: adjusting the pH value of ferrous salt solution or waste acid solution containing ferrous ions to 8.7-10 with NaOH, adding H2O2 at room temperature to prepare amorphous delta-FeOOH precursor, adding ferrous salt solution at a delta-FeOOH/ferrous salt mol. ratio of (1.32-1.92):1, adjusting the pH value to 8-13 with NaOH, refluxing under boiling for 1.5-2.5 h, filtering the product, washing with water, washing with diluted ammonia solution, and drying to obtain spherical Fe3O4 nanopowder. The particle sizes of the Fe3O4 nanopowder are 30-70 nm, and can be artificially controlled. The Fe3O4 nanopowder has high crystallinity. The method has such advantages as simple process, short reaction time, mild reaction conditions, abundant raw material, and no pollution.

Description

technical field [0001] The invention relates to a method for preparing nano-Fe 3 o 4 method, especially a liquid-phase rapid preparation of ultra-fine uniform nano-Fe 3 o 4 Methods. Background technique [0002] Fe 3 o 4 It is an ancient and traditional magnetic material, and it is also the earliest non-metallic magnetic material. Due to its many advantages and special properties, it has always been valued in the field of magnetic material research and application. With the informatization of society and the application of nanotechnology, people's synthesis of it gradually transitions from micron, submicron to nanometer size. This miniaturized nanotechnology has created conditions for the development of many fields. Due to the size effect of nanoparticles, different sizes of Fe 3 o 4 Magnetic nanoparticles often exhibit different magnetic properties. Therefore, for Fe with controllable particle size 3 o 4 The synthesis of magnetic materials has become a research h...

Claims

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Application Information

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IPC IPC(8): C01G49/08B82B3/00
Inventor 刘辉魏雨
Owner HEBEI NORMAL UNIV
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