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Method for preparing Nano Fe2O3

A nano, divalent iron salt technology, applied in the field of preparation of nano Fe3O4, can solve the problems of poor uniformity, high cost, complex preparation process, etc., and achieve good dispersion and uniformity, controllable particle size, and simple process. Effect

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 Magnetic Mater.2001, 225, 30-36); An Lijuan et al. used co-precipitation method, and used oleic acid and sodium dodecylbenzenesulfonate as double-layer surfactants to modify the surface, and prepared granules Stable water-dispersible nano-Fe with a diameter of 10 nm 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); but with Fe 2+ As a raw material, add alkali to control the pH value, and use air to oxidize the obtained Fe 3 o 4 The particle size is generally large, and there is no report of a particle size smaller than 20nm, and the uniformity is not good
In recent years, although in Fe 3 o 4 Significant progress has been made in nano-preparation and modification, but there are still two typical problems: (1) the raw materials for preparation are more expensive, the cost is higher, and the relative preparation process is more complicated; (2) for nano-Fe 3 o 4 Modification of the surface of the sample can reduce the grain size of the sample and improve the dispersion of the sample, but it will lead to nano-Fe 3 o 4 decline in magnetic properties

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Add 30ml of FeSO with a concentration of 1mol / L to the reaction kettle 4 , adding a NaOH solution with a concentration of 6mol / L to make the solution pH=11, adding 2ml of EDTA with a concentration of 0.05mol / L, irradiating with ordinary light (illuminance 12000Lux), feeding air (air flow rate 0.132m 3 / h) Oxidation, the reaction temperature is controlled at 30°C, and the reaction is continued for 1.5h. After the reaction is completed, it is filtered first, and then washed several times with distilled water to obtain 2.31g of the product, and the particle size of the product is about 20nm.

Embodiment 2

[0016] Add 30ml of FeSO with a concentration of 1mol / L to the reaction kettle 4 , adding a NaOH solution with a concentration of 6mol / L to make the pH value = 10, adding 2ml of EDTA with a concentration of 0.05mol / L, irradiating with ordinary light (illuminance 12000Lux), feeding air (air flow rate 0.132m 3 / h) Oxidation, the reaction temperature is controlled at 50°C, and the reaction is continued for 1.2h. After the reaction is completed, it is filtered first, and then washed several times with distilled water to obtain the product Fe 3 o 4 The particle size is about 40nm, and its saturation magnetization is 70emu / g.

Embodiment 3

[0018] Add 30ml of FeSO with a concentration of 1mol / L in the reaction kettle, add a NaOH solution with a concentration of 6mol / L to make the pH=11, add 2ml of EDTA with a concentration of 0.05mol / L, and add 10ml of 0.01mol / L NaOH solution. Sodium alkyl sulfonate surfactant, irradiated with ordinary light (illuminance 12000Lux), blowing air (air flow rate 0.132m 3 / h), the reaction temperature is controlled to be 30°C, and the reaction is continued for 1.5h. After the reaction is completed, it is filtered first, and then washed several times with distilled water to obtain 2.31g of the product. The product has good uniformity and a particle size of about 16nm.

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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 to 9-11 with NaOH, adding trace amount of complexone, and oxidizing in air under the induction of visible light to obtain spherical Fe3O4 nanopowder. The particle sizes of the Fe3O4 nanopowder are 10-50 nm, and can be artificially controlled. The Fe3O4 nanopowder has such advantages as uniform particle size distribution, good dispersibility, high purity and high yield. The method is simple and economic.

Description

technical field [0001] The present invention relates to a kind of nano Fe 3 o 4 preparation method, especially a liquid phase preparation of ultra-fine uniform nano-Fe 3 o 4 Methods. Background technique [0002] Nano Fe 3 o 4 It has excellent performance in magnetism, catalysis, biology, etc. It not only shows new application value in traditional fields, but also becomes an important part of new materials such as magnetic liquid, magnetic microbeads, and magnetic drugs. Due to the size effect of nanoparticles, different sizes of Fe 3 o 4 Magnetic nanoparticles often exhibit different magnetic properties. But Fe 3 o 4 It is very easy to agglomerate during the generation process, which affects its application, so the preparation of nano-Fe with controllable monodisperse particle size 3 o 4 Powder has become the research focus of various countries. S.H.Sun et al. through thermal decomposition [Fe(acac) 3 ] In the presence of acetylacetone, oleylamine, etc., high-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/08B82B3/00
Inventor 候登录魏雨陈汝芬
Owner HEBEI NORMAL UNIV
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