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Method for preparing spherical Fe3O4 nano powder

A technology of nano-powder and spherical shape, which is applied in the field of preparation of spherical Fe3O4 nano-powder, which can solve the problems of irregular spherical shape, large powder particle size, and high price, and achieve the effects of reducing energy consumption, shortening time, and easy washing

Active Publication Date: 2009-03-11
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Currently, for spherical Fe 3 o 4 There are relatively few studies on the preparation method of magnetic powder. Although there are similar reports in China, for example, Chinese patent application numbers 200610013524.x and 200610078078.0 respectively disclose the preparation of quasi-spherical or spherical Fe 3 o 4 The method of magnetic powder, but existing preparation method still exists some deficiencies, for example: 1) preparation raw material uses the ferric iron with higher price and unnecessary sodium carbonate; 2) oxidation reaction time is all longer, energy consumption Larger; 3) The spherical shape of the product is irregular or the particle size of the powder is larger; 4) None of them solves the environmental pollution in production, etc.

Method used

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  • Method for preparing spherical Fe3O4 nano powder
  • Method for preparing spherical Fe3O4 nano powder
  • Method for preparing spherical Fe3O4 nano powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A spherical Fe 3 O 4 The preparation method of nano powder consists of the following steps:

[0029] (1) The preparation concentration is 0.5mol·L -1 An aqueous solution of ferrous sulfate; heated to 80°C within 0.6h, stirred at a speed of 400 rpm, added ammonia water, and adjusted the pH to 6.5;

[0030] (2) Put the solution prepared in step (1) into a reactor equipped with a gas distributor, stir, at a speed of 400 rpm, at 80°C, and blow in air with a flow rate of 0.8m 3 / h, add NH after 10 minutes with air 4 NO 2 Is a catalyst, the addition amount of the catalyst is 0.5% of the mass of the ferrous salt, and the reaction is carried out to detect Fe in the system 3+ With Fe 2+ When the molar ratio of is 1.8, stop the air flow;

[0031] (3) Continue to stir, the speed is 400 rpm, at 80 ℃, add ammonia water to adjust the pH to 9.5, and then heat the reaction for 2.0 hours;

[0032] (4) Stop stirring and heating, and cool to 25°C naturally;

[0033] (5) Solid-liquid separatio...

Embodiment 2

[0035] A spherical Fe 3 O 4 The preparation method of nano powder consists of the following steps:

[0036] (1) The preparation concentration is 0.6mol·L -1 An aqueous solution of ferrous sulfate; heated to 85°C within 1.0h, stirred at a speed of 500 rpm, added ammonia water, and adjusted the pH to 6.0;

[0037] (2) Put the solution prepared in step (1) into a reactor equipped with a gas distributor, stir, rotate at 500 rpm, at 85°C, blow in air, and air flow rate is 0.6m 3 / h, add NH after 11 minutes of air 4 NO 2 As a catalyst, the addition amount of the catalyst is 0.8% of the mass of the ferrous salt, the reaction is carried out, and the Fe in the detection system (that is, the reaction system at this time) 3+ With Fe 2+ When the molar ratio of is 1.91, stop the air flow;

[0038](3) Continue to stir at a speed of 500 rpm, add ammonia water to adjust the pH to 9.0 at 85°C, and then heat the reaction for 3.0 hours;

[0039] (4) Stop stirring and heating, and cool to 20°C natura...

Embodiment 3

[0042] A spherical Fe 3 O 4 The preparation method of nano powder consists of the following steps:

[0043] (1) The preparation concentration is 0.1mol·L -1 An aqueous solution of ferrous chloride; heated to 70°C within 0.5h, stirred at a speed of 100 rpm, added ammonia water, and adjusted the pH to 7.0;

[0044] (2) Put the solution prepared in step (1) into a reactor equipped with a gas distributor, stir at a speed of 100 rpm, at 70°C, blow in air, and an air flow rate of 1.0 m 3 / h, add NaNO after 12 minutes with air 2 Is a catalyst, the addition amount of the catalyst is 0.6% of the mass of the ferrous salt, the reaction is carried out, and the Fe in the system is detected 3+ With Fe 2+ When the molar ratio of is 2.4, stop the air flow;

[0045] (3) Continue to stir at a speed of 100 rpm, at 70°C, add ammonia water to adjust the pH to 10.0, then add ammonium silicate, the amount of which is 3% of the mass of ferrous sulfate, and the insulation reaction for 4.0h;

[0046] (4) S...

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Abstract

The invention discloses a method for preparing spherical Fe3O4 nanometer powder body. The method comprises the following steps: (1) an aqueous solution of ferrous salt is prepared, heated and stirred to regulate the PH value of between 4.0 and 8.0: (2) the solution is put to a reactor with a gas distributor, stirred and communicated with air; 5 to 15 minutes later after the air is communicated, NH4NO2 or NaNO2 is added for reaction; when the molar ratio of Fe<3+> and Fe<2+> is between 1.6 and 2.6, the air is stopped to communicate; (3) the solution is stirred to regulate the PH value of between 8.0 and 14.0 and react for 1.0 to 5.0 hours; (4) stirring and heating are stopped to naturally cool the solution to the temperature of between 20 and 35 DEG C; and (5) the solution is subjected to solid-liquid separation; solid is washed by deionized water and is dried to prepare the spherical Fe3O4 nanometer powder body. The method can use an industrial byproduct which is cheap and easy to obtain as a raw material, shorten time for oxidation reaction and reduce energy consumption; and the product meets the requirement on the raw material of high-grade ink powder and has no environmental pollution.

Description

Technical field [0001] The invention relates to the field of magnetic material preparation, in particular to a spherical Fe 3 O 4 Preparation method of nano powder. Background technique [0002] Nano Fe3O4 (Fe 3 O 4 ) Has a wide range of applications, and has been widely used in functional materials, magnetic materials, medical, pigments and catalysts. Fe 3 O 4 Magnetic powder is the main raw material of toner used in image and text output devices such as copiers, printers, fax machines, etc. Fe 3 O 4 There are mainly cubic and spherical powders. Currently, domestically produced Fe 3 O 4 The magnetic powder is basically cubic powder and the particle size of the powder is also relatively large. Modern graphic output equipment has a high resolution, which requires high-end toner to match it, and the high-end toner requires Fe 3 O 4 The magnetic powder should have the characteristics of special morphology, ultra-fine particle size, uniform distribution, and good dispersion. Spherica...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/08
Inventor 王兴尧苗翠王艳明王静
Owner TIANJIN UNIV
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