Method for preparing superparamagnetic Fe3O4 nano particle based on thermal decomposition of template

A superparamagnetic and nanoparticle technology, applied in ferrous oxide, iron oxide/iron hydroxide, etc., can solve the problems of wide particle size distribution, agglomeration, restricting the industrialization development of magnetic Fe nanoparticles, etc. Good dispersion, regular morphology and controllable morphology

Inactive Publication Date: 2011-04-06
SUZHOU KANG NAMI BIOLOGICAL ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the preparation of magnetic nanoparticles by hydrothermal method, although the predecessors have done a lot of work, the main problem at present is that the magnetic Fe 3 o 4 During the production scale-up of nanoparticles, there are prominent problems such as agglomeration and wide particle size distribution, which restrict the magnetic Fe 3 o 4 Industrialization Development of Nanoparticles

Method used

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  • Method for preparing superparamagnetic Fe3O4 nano particle based on thermal decomposition of template
  • Method for preparing superparamagnetic Fe3O4 nano particle based on thermal decomposition of template
  • Method for preparing superparamagnetic Fe3O4 nano particle based on thermal decomposition of template

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Effect test

Embodiment 1

[0036] Configure 0.12 mol / L Na 2 SO 4 Substrate solution, at 25 ° C and 650 rpm stirring conditions, sequentially add 20 ml of 0.25 mol / liter ZnSO 4 solution, 8 ml of 0.05 mol / L cetyltrimethylammonium bromide solution and 35 ml of 0.34 mol / L sodium carbonate solution to obtain a white sol-like slurry, then add 0.15 gram of sodium ascorbate and 50 ml of 0.4 mol / L FeSO 4 solution. After the above solutions are fully mixed, the pH value is adjusted to 11.5 with 0.5 mol / L sodium hydroxide solution, and after the obtained solid is filtered and washed, add ethanol equal to the volume of the pre-filtered slurry, stir and transfer to a hydrothermal device. Heat at 200°C for 8 hours. After the hydrothermal suspension was separated by magnet, filtered, washed and dried in vacuum (40°C, 24 hours), a large amount of black superparamagnetic Fe with a particle size of about 25nm was obtained, which was monodisperse. 3 o 4 Nanoparticles.

[0037] figure 2 Show the XRD diffraction...

Embodiment 2

[0039] Configure 0.12 mol / L Na 2 SO 4 Substrate solution, under 25 ℃ and 800 rpm stirring conditions, add 15 ml of 0.23 mol / L ZnSO 4 solution, 12 milliliters of 0.06 mol / liter cetyltrimethylammonium bromide solution and 30 milliliters of 0.27 mol / liter sodium carbonate solution to obtain a white sol-like slurry, then add 0.2 gram of sodium ascorbate and 60 milliliters of 0.4 mol / L FeSO 4 solution. After the above solutions are fully mixed, the pH value is adjusted to 11.5 with 0.5 mol / L sodium hydroxide solution, and the obtained solid is filtered and washed, and 1,3 butanediol is added with the volume equal to that of the pre-filtered slurry, stirred and transferred to Put it into a hydrothermal device, and heat it at 200°C for 10 hours. After the hydrothermal suspension was separated by magnet, filtered, washed and dried in vacuum (40°C, 24 hours), a large amount of black superparamagnetic Fe with a particle size of about 15nm was obtained, which was monodisperse. 3 o ...

Embodiment 3

[0041] Configure 0.12 mol / L Na 2 SO 4 Substrate solution, under 25 ℃ and 700 rpm stirring conditions, add 15 ml of 0.23 mol / L ZnSO 4 solution, 0.01 mol sodium oleate and 30 ml 0.27 mol / l sodium carbonate solution to obtain a white slurry, then add 0.2 g sodium ascorbate and 50 ml 0.4 mol / l FeSO 4 solution. After the above solution is fully mixed, the pH value is adjusted to 11.0 with 0.5 mol / liter sodium hydroxide solution, and the obtained solid is filtered and washed, and isopropanol of the same volume as the slurry before filtration is added, stirred and transferred to hydrothermal device, heated at 200°C for 12 hours. The hydrothermal suspension was separated by magnet, filtered, washed and dried in vacuum (40°C, 24 hours), and a large amount of black magnetic Fe with a particle size of about 80nrn was obtained, which was monodisperse. 3 o 4 Nanoparticles, synthesized magnetic particles with -COO- groups on the surface.

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Abstract

The invention relates to a method for preparing a superparamagnetic Fe3O4 nano particle based on the thermal decomposition of a template, belonging to the filed of preparation of an inorganic chemical material. The method comprises the following steps: preparing a sol soft template of which the surface contains -OH radicals by a liquid deposition reaction, using low-cost iron salt as raw materials, solidifying Fe<2+> ions in the liquid phase by means of the -OH radicals on the surface of the soft template, and performing a hydrothermal reaction at 150-2500 C for 5-15 hours to obtain a magnetic Fe3O4 nano particle having a regular appearance, a controllable particle diameter and monodispersity, wherein the particle can present superparamagnetism when the particle diameter is less than 50 nm. The synthesized magnetic nano material can be widely used in fields of biological separation, diathermic therapy on tumors, release of targeted drugs, magnetic suspensions, vacuum sealing, aerospace, sensors and the like.

Description

technical field [0001] The invention relates to a method for preparing superparamagnetic Fe 3 o 4 A nanoparticle approach, especially one based on thermal decomposition of templates to prepare superparamagnetic Fe 3 o 4 The nanoparticle method belongs to the field of preparation of inorganic chemical materials. Background technique [0002] my country is rich in iron resource reserves, but the research and development of multifunctional and high value-added iron salt materials is late, and the commercially available products are mainly conventional products with single function and low price (such as ferric sulfate, ferrous sulfate, ferric chloride, nitric acid Iron, and ordinary iron oxide, etc.), how to introduce rapid corresponding manufacturing technology in traditional powder metallurgy production, to prepare multifunctional, high value-added magnetic nanomaterial products (such as superparamagnetic Fe 3 o 4 Particles), which are necessary and urgent for powder meta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/08
Inventor 高国崔大祥
Owner SUZHOU KANG NAMI BIOLOGICAL ENG
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