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Method for manufacturing nano-ferrous acid in supercritical water

A nano-cobalt ferrite and supercritical water technology, applied in nanostructure manufacturing, nanotechnology, nanotechnology and other directions, can solve the problems of high calcination temperature and complex process, and achieve the effects of good dispersion, simple process and simple composition

Active Publication Date: 2009-10-28
INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] There are relatively few patents on the preparation method of nano-cobalt ferrite. Chinese patent (application number: 200410065678.4) reports the preparation method of combining microwave drying and calcination with high-energy ball mill ball milling to prepare nano-cobalt compounds. This method requires microwave drying and high calcination temperature. Obtaining solid powder requires ball milling, and the process is relatively complicated

Method used

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  • Method for manufacturing nano-ferrous acid in supercritical water
  • Method for manufacturing nano-ferrous acid in supercritical water
  • Method for manufacturing nano-ferrous acid in supercritical water

Examples

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Effect test

Embodiment 1

[0032] 2g Co(NO 3 ) 2 ·6H 2 O was dissolved in 150ml deionized water, and Fe(NO 3 ) 3 9H 2 O, make the molar ratio of cobalt ions to iron ions r=0.5, stir the glass rod evenly; add 0.01~0.1mol / L NaOH dropwise to the mixed solution to adjust the pH=11; then pour the mixed solution into the supercritical water reaction equipment, turn on the heating Furnace and magnetic stirrer, heated to 400°C, the corresponding pressure is 3920psi, and reacted for 1h; after the reaction, passed cooling water, poured out the mixture, filtered on a vacuum filter, rinsed with deionized water until neutral, and baked at 25°C Dry cobalt ferrite particles with good dispersibility can be obtained, the particle size is 3-10nm, see figure 1 a and figure 2 Figure a in.

Embodiment 2

[0034] The difference from Example 1 is that the pH is adjusted to 13; cobalt ferrite particles with good dispersibility and a particle size of 3-10 nm are obtained.

Embodiment 3

[0036] The difference from Example 1 is: 1g Co(NO 3 ) 2 ·6H 2 O was dissolved in 150ml deionized water, and Fe(NO3 ) 3 9H 2 O, make the molar ratio of cobalt ions to iron ions r=0.5, stir evenly with a glass rod; obtain cobalt ferrite particles with good dispersion and particle size of 3-10 nm.

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Abstract

The invention relates to a preparation method of nanometer material and super-critical water technical application, in particular to the method of synthesizing nanometer cobalt ferrite by utilizing super-critical water. The preparation process comprises the following steps: dissolving the ferric nitrate and cobalt nitrate with a certain proportion in the deionized water and stirring; regulating the Ph of the mixed liquid from 9 to 13; pouring the mixed solution into the kettle-type super-critical water reaction equipment, heating to 375 to 450 DEG C by continuous stirring and react for 0.5 to 6 hours; after the reaction, rapidly cooling, filtering, washing by deionized water and drying to get the cobalt ferrite grain with sound dispersion and average grain size of 5nm. The preparation method has the advantages of small environmental pollution and simple technology. The nanometer cobalt ferrite grain produced has magnetic, and thus having potential application prospects in anisotropy permanent magnet, magnetic recorder, magnetic fluid and other fields.

Description

technical field [0001] The invention relates to the preparation of nanometer materials and the application of supercritical water technology, in particular to a method for synthesizing nanometer cobalt ferrite by supercritical water. Background technique [0002] The critical temperature of pure water is 647K, and the critical pressure is 22.1MPa. Above this temperature and pressure, it is called supercritical water. Compared with water at normal temperature, the physical properties of water in the supercritical state have changed greatly, mainly in: the dielectric constant becomes smaller, the hydrogen bond becomes weaker, the flow viscosity decreases, the diffusion coefficient becomes larger, and the organic matter and most Gases can be freely miscible, etc.; moreover, the solubility of inorganic salts in supercritical water is very small, showing the characteristics of organic solvents. Supercritical water has been widely used in organic wastewater treatment and metal ox...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G51/00C01G49/16B82B3/00B01J3/00
CPCY02P20/54
Inventor 赵丹吴欣强关辉韩恩厚
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI
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