Method for preparing nanometer iron oxide red

A red iron oxide, nanotechnology, applied in the direction of iron oxide, iron oxide/iron hydroxide, etc., can solve the problems of poor dispersibility and long working cycle, and achieve the effect of ensuring dispersibility, short drying time and reducing production cost.

Inactive Publication Date: 2011-07-06
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a nano-iron oxide red with small particle size, easy to obtain raw materials, low pollution, short cycle and good dispersibility in view of the shortcomings of the existing preparation methods such as long working cycle and poor dispersibility. Particle Preparation Method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In 250mL0.3mol / L FeSO 4 Add 10mLH to the solution 2 SO 4 , adjust the pH to 4, then add saturated H 2 C 2 o 4 The solution was 200mL, stirred and heated to boiling to form a yellow precipitate. After standing still, the supernatant was poured off, and the precipitate was washed with 40°C deionized water. Repeat 3 times to remove soluble impurities. Slowly add 200 mL of 3% H 2 o 2 solution and at 0.12m 3 The flow of / h is passed into O 2 , maintain the temperature at 40°C, pH 4, and keep stirring until the reaction is completely oxidized to Fe 3+ , react for 20min. Boil to remove residual H 2 o 2 , filtered while hot. After filtering, the precipitate was washed with deionized water, dried at 30° C. for 1.5 h, mixed with ammonium bicarbonate containing 5% of the total mass of the precipitate, and the mixture was calcined at 700° C. for 1.5 h, and the nanomaterial iron oxide red was obtained after grinding.

Embodiment 2

[0025] In 250mL0.4mol / L FeSO 4 Add 10mLH to the solution 2 SO 4 , then add saturated H 2 C 2 o 4 The solution was 250mL, stirred and heated to boiling to form a yellow precipitate. After standing still, the supernatant was poured off, and the precipitate was washed with 40°C deionized water. Repeat 2 times to remove soluble impurities. Slowly add 250 mL of 3% H 2 o 2 solution and at 0.15m 3 The flow of / h is passed into O 2 , maintain the temperature at 40°C, pH 5.0, and keep stirring until the reaction is completely oxidized to Fe 3+ , react for 20min. Boil to remove residual H 2 o 2 , filtered while hot. After filtering, the precipitate was washed with deionized water, dried at 30° C. for 1.5 h, mixed with ammonium bicarbonate containing 6% of the total mass of the precipitate, and the mixture was calcined at 750° C. for 1.5 h, and the nanomaterial iron oxide red was obtained after grinding.

Embodiment 3

[0027] In 250mL0.5mol / L FeSO 4 Add 10mLH to the solution 2 SO 4 , then add saturated H 2 C 2 o 4 The solution was 250mL, stirred and heated to boiling to form a yellow precipitate. After standing still, the supernatant was poured off, and the precipitate was washed with 40°C deionized water. Repeat 3 times to remove soluble impurities. Slowly add 200 mL of 3% H 2 o 2 solution and at 0.16m 3 The flow of / h is passed into O 2 , maintain the temperature at 50°C, pH 5.0, and keep stirring until the reaction is completely oxidized to Fe 3+ , react for 30min. Boil to remove residual H 2 o 2 , filtered while hot. After filtration, the precipitate was washed with deionized water, dried at 40° C. for 1.5 h, mixed with 8% ammonium bicarbonate of the mass of the precipitate, calcined at 750° C. for 1 h, and ground to obtain iron oxide red nanomaterial.

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Abstract

The invention provides a method for preparing nanometer iron oxide red. The method comprises the following steps of: adding proper amount of H2C2O4 to solution of ferrous salt, boiling and stirring the mixed solution to form yellow precipitate, standing the mixed solution, removing supernatant, adding 3 percent H2O2 solution, filling O2 to the mixed solution under a continuously stirring condition, keeping a proper temperature and pH value until the oxidizing reaction is completed, removing excessive H2O2 and then filtering the mixed solution while the mixed solution is still hot; and after filtering, washing and drying the precipitate, mixing the precipitate with proper amount of ammonium bicarbonate, burning the mixture, and grinding the mixture to obtain the nanometer-grade powdery iron oxide red. The method has the advantages of simple operation, low material cost, and small grain size and good product dispersibility.

Description

technical field [0001] The invention relates to the technical field of preparation of nanometer materials, in particular to a preparation technology of nanometer iron oxide red. Background technique [0002] The chemical formula of iron oxide red is α-Fe 2 o 3 . Nano-iron oxide has surface effect, volume effect, and quantum size effects, and exhibits unique optical, magnetic, thermal, and catalytic properties. It is widely used in the preparation of magnetic materials, pigments, fine ceramics, and plastic products, as well as in the catalyst industry. It also has extensive application value and prospects in acoustics, electronics, optics, thermals, especially medicine and bioengineering, so it has important research value. [0003] In the reports of scientific papers, the common preparation methods of monodisperse nanoparticles include sol-gel method, hydrothermal method, radiation synthesis method, hydrolysis method, adhesion method, flame combustion decomposition method...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G49/06
Inventor 方卫民陆晓星郭伟强何雨舟鲁旻阳
Owner ZHEJIANG UNIV
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