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Process for producing spherical FeOOH nano-powder

A nano-powder and spherical technology, which is applied in the field of preparation of spherical FeOOH nano-powder, can solve the problems of uneven average particle size, complex synthesis steps, and low purity of spherical powder, and achieve low cost, short reaction time, and high purity. Effect

Inactive Publication Date: 2009-05-13
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The above-mentioned methods are either costly; or the purity is not high; or the synthesis steps are complicated; or the average particle size of the spherical powder is uneven; or there is waste liquid discharge

Method used

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  • Process for producing spherical FeOOH nano-powder
  • Process for producing spherical FeOOH nano-powder

Examples

Experimental program
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Effect test

Embodiment 1

[0025] A preparation method of spherical FeOOH nanopowder, comprising the steps of:

[0026] (1) Under stirring, tributyl phosphate, isooctyl alcohol, kerosene and 0.2mol·L -1 Fe 3+ Mix the aqueous solution (choose ferric chloride aqueous solution to prepare), adjust pH=2.5, continue to stir after 0.5 hour, put the mixed solution in the liquid separation device, stand still for 10 minutes, separate the organic phase and the aqueous phase of loading metal iron, washing the organic phase loaded with metallic iron for 3 times with distilled water, and then separating the liquids to collect the organic phase loaded with metallic iron;

[0027] (2) The organic phase loaded with metallic iron and the aqueous ammonia solution with pH=8 are uniformly mixed in a volume ratio of 1:1 and then introduced into a high-pressure axe, at a stirring rate of 500 rpm and a temperature of 130°C, The pressure is 0.5Mpa, and the hydrothermal stripping reaction is carried out for 30 minutes;

[00...

Embodiment 2

[0031] A preparation method of spherical FeOOH nanopowder, comprising the steps of:

[0032] (1) Under stirring, tributyl phosphate, B liquid and 0.05mol·L -1 Fe 3+ Mix the aqueous solution (choose ferric chloride aqueous solution to prepare), adjust pH=3.0, continue to stir for 0.5 hour, put into the separatory device, stand still for 60 minutes, separate the organic phase and the aqueous phase loaded with metal iron, wash with distilled water Describe the organic phase loaded with metallic iron for 2 times, then separate liquids, collect the organic phase loaded with metallic iron, and the B liquid is isooctyl alcohol and kerosene with a volume ratio of 1:3;

[0033] (2) Mix the organic phase loaded with metallic iron and ammonia water with pH=7 in a ratio of 1:1 by volume and then introduce it into a high-pressure axe. 4.0Mpa, carry out hydrothermal stripping reaction for 60 minutes;

[0034] (3) Naturally cool the reaction system to 20° C., turn on the high-pressure axe...

Embodiment 3

[0037] A preparation method of spherical FeOOH nanopowder, comprising the steps of:

[0038] (1) Under stirring, di(2-ethylhexyl)phosphoric acid, liquid B and 1.0mol·L -1 Fe 3+ Mix the aqueous solution (select ferric nitrate aqueous solution to prepare), adjust pH=0, continue to stir for 1.0 hour, put into the separatory device, stand still for 40 minutes, separate the organic phase and aqueous phase of loading metal iron, wash described loading with distilled water The organic phase of metallic iron was separated for 3 times, and the organic phase loaded with metallic iron was collected. The B liquid was isooctyl alcohol and kerosene with a volume ratio of 1:1;

[0039] (2) The organic phase loaded with metallic iron and the potassium hydroxide aqueous solution of pH=10 are uniformly mixed in a ratio of 4:1 by volume and then introduced into the high-pressure axe. °C, the pressure is 4.0Mpa, and the hydrothermal stripping reaction is carried out for 30 minutes;

[0040] (3...

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Abstract

The invention discloses a method for preparing spherical FeOOH nano-powder, which comprises the following steps: blending a liquid A, a liquid B and Fe<3+> water solution while stirring; adjusting the pH value; stirring; separating the liquids into the organic phase and the water phase loading metal Fe, wherein, the liquid A is tributyl phosphate (TBP), and the liquid B is isooctyl alcohol and kerosene; blending the organic phase and the inorganic base solution; stirring; conducting the hydrothermal back-extraction reaction at the temperature of 100 to 200 DEG C; cooling to 20 to 35 DEG C; opening the autoclave; taking out the materials; carrying out the solid-liquid separation; rinsing the solid part with absolute alcohol; and drying to obtain the spherical FeOOH nano-powder. The invention has the advantages that only the raw material of iron salt is consumed, thereby ensuring the low cost; the purity of the product is high; the average particle diameter is about 100 nm; the reaction is mild; the reaction time is short; the high-temperature calcination is not required; the process is simple; the energy consumption is low; the extracting agent can be directly recycled; the discharge of the waste liquid is avoided; and the method belongs to green synthesis technology.

Description

technical field [0001] The invention relates to the field of preparation of inorganic functional materials, in particular to a method for preparing spherical FeOOH nanopowder. Background technique [0002] Iron oxyhydroxide (FeOOH) is an important functional material, which is widely used in catalysts, adsorbents, pigments, precursors of magnetic recording media, magnetic coatings, gas sensors, etc.; it can also be used as a functional material in the process of environmental protection, such as gas Desulfurization agent, heavy metal removal agent in wastewater, etc. The method of synthesizing nano-FeOOH can be divided into solid-phase method and liquid-phase method. The particle size distribution of the product prepared by the solid-phase method is often uneven. The liquid-phase method mainly includes oxidation method, sol method, uniform precipitation method and colloid chemical method. [0003] The above-mentioned method either has high cost; or low purity; or complex sy...

Claims

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Application Information

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IPC IPC(8): C01G49/02
Inventor 王兴尧王艳明苗翠张辉平
Owner TIANJIN UNIV
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