Method of controllably preparing narrow particle size distribution submicron order alpha-FeOOH

A submicron, narrow particle technology, applied in the direction of iron oxide/iron hydroxide, etc., can solve the problems of uncontrollable nucleation and growth, narrow distribution of submicron particle size, etc., achieving low synthesis cost, uniform particle size, The effect of high sample phase purity

Inactive Publication Date: 2013-07-17
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The purpose of the present invention is to provide a controllable preparation method of submicron α-FeOOH with narrow particle size distribution, which solves the problem of uncontrollable nucleation and growth, and the prepared submicron particle size distribution range is very narrow

Method used

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  • Method of controllably preparing narrow particle size distribution submicron order alpha-FeOOH
  • Method of controllably preparing narrow particle size distribution submicron order alpha-FeOOH
  • Method of controllably preparing narrow particle size distribution submicron order alpha-FeOOH

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 1) FeSO 4 ·7H 2 O and NaOH are dissolved in distilled water respectively, and form FeSO with a concentration of 0.17mol / L after dissolution. 4 Solution and concentration are the NaOH solution of 5.80mol / L;

[0032] 2) FeSO configured in step 1 4 The solution is dissolved in the NaOH solution configured in step 1, and the FeSO 4 The volume ratio of the solution to the NaOH solution is 2:5, stir to fully dissolve it;

[0033] 3) The mixed solution obtained in step 2 was assisted with low-frequency ultrasonic treatment, the ultrasonic frequency was 50W, and the ultrasonic time was 10min, until the mixed solution was light green;

[0034] 4) Transfer the solution obtained in step 3 into a Teflon hydrothermal kettle with a filling ratio of 40%, and keep it warm for 1 hour at a temperature of 110°C;

[0035] 5) Add 200ml of distilled water to the precipitate obtained in step 4 to rinse, and perform centrifugation. The centrifuge speed is 12000r / min, and the centrifugatio...

Embodiment 2

[0039] 1) FeSO 4 ·7H 2 O and NaOH are dissolved in distilled water respectively, and form FeSO with a concentration of 0.50mol / L after dissolution. 4 solution and a NaOH solution with a concentration of 1mol / L;

[0040] 2) FeSO configured in step 1 4 The solution is dissolved in the NaOH solution configured in step 1, and the FeSO 4 The volume ratio of the solution to the NaOH solution is 2:5, stir to fully dissolve it;

[0041] 3) The mixed solution obtained in step 2 is assisted by low-frequency ultrasonic wave, the ultrasonic power is 40W and the ultrasonic time is 8min, until the mixed solution is light green;

[0042] 4) Transfer the solution obtained in step 3 into a Teflon hydrothermal kettle with a filling ratio of 70%, and keep it warm for 6 hours at a temperature of 125°C;

[0043] 5) Add 200ml of distilled water to the precipitate obtained in step 4 to rinse, and perform centrifugation. The centrifuge speed is 12000r / min, and the centrifugation time is 5min. U...

Embodiment 3

[0047] 1) FeSO 4 ·7H 2 O and NaOH are dissolved in distilled water respectively, and form FeSO with a concentration of 0.60mol / L after dissolution. 4 solution and a NaOH solution with a concentration of 10.00mol / L;

[0048] 2) FeSO configured in step 1 4 The solution is dissolved in the NaOH solution configured in step 1, and the FeSO 4 The volume ratio of the solution to the NaOH solution is 2:5, stir to fully dissolve it;

[0049] 3) The mixed solution obtained in step 2 is assisted by low-frequency ultrasonic wave, the ultrasonic power is 70W and the ultrasonic time is 10min, until the mixed solution is light green;

[0050] 4) Transfer the solution obtained in step 3 into a Teflon hydrothermal kettle with a filling ratio of 60%, and keep it warm for 2 hours at a temperature of 80°C;

[0051] 5) Add 200ml of distilled water to the precipitate obtained in step 4 to rinse, and perform centrifugation. The centrifuge speed is 12000r / min, and the centrifugation time is 5min. ...

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Abstract

The invention provides a method of controllably preparing narrow particle size distribution submicron order alpha-FeOOH. The method comprises steps of: mixing a FeSO4 solution with a sodium hydroxide solution at a volume ratio of 2:5, and after fully dissolving, carrying out low frequency ultrasonic wave auxiliary treatment until a mixed solution is light green; and then, pouring the solution into a Teflon hydrothermal reactor with a packing ratio of 30-70%, insulating at 80-125 DEG C for 1-10h, extracting precipitate, carrying out centrifugal treatment after washing the precipitate, and then drying the precipitate at 80 DEG C in the air atmosphere. The method can be used for solving uncontrollable nucleation and growth problems, and the size distribution scope of the prepared submicron particles is very narrow.

Description

【Technical field】 [0001] The invention belongs to the technical field of preparing nanometer powder by wet chemical method, and in particular relates to a controllable preparation method of submicron α-FeOOH. 【Background technique】 [0002] Iron oxides mainly include iron hydroxides and oxides, which are widely used in the field of catalysis, magnetic materials, sensors, pigments, and environmental pollution control. Among them, α-FeOOH is one of the most representative iron oxide compounds, which widely exists in the natural environment and is the most suitable method for the synthesis of α-FeOOH. 2 o 3 and γ-Fe 2 o 3 one of its precursors. [0003] The preparation methods of α-FeOOH that have been reported so far can produce finer particles, but still cannot obtain satisfactory results in terms of particle size and controllability of nucleation and growth. For example, Chinese Patent Announcement No. CN101428863 reports a method for synthesizing FeOOH nanopowder by hy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/02
Inventor 于成龙高丹鹏郝欣乔畅君刘谦柴思敏姚田力唐宁波
Owner SHAANXI UNIV OF SCI & TECH
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