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Method for preparing paramagnetic Fe3O4 nanoparticles by using iron tailings

A superparamagnetic and nanoparticle technology, which is applied in nanotechnology, ferrous oxides, solid waste removal, etc., can solve the problems of particle instability and easy agglomeration, and achieve simple equipment, no agglomeration, and reproducible good sex effect

Inactive Publication Date: 2012-07-18
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation process does not use protective gas, and uses surfactant to coat the formed particles, which better solves the problem of Fe 2+ Oxidation and particle instability and easy to agglomerate, the preparation of Fe with good particle dispersibility and uniform particle size 3 o 4 nanoparticles

Method used

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  • Method for preparing paramagnetic Fe3O4 nanoparticles by using iron tailings
  • Method for preparing paramagnetic Fe3O4 nanoparticles by using iron tailings
  • Method for preparing paramagnetic Fe3O4 nanoparticles by using iron tailings

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Step 1: Mix 100 g of iron tailings with 37.5 wt% concentrated hydrochloric acid, stir mechanically for 2-4 hours at a stirring rate of 150-250 r / min, and filter out the pickling solution. Add appropriate amount of hydrogen peroxide in the filtrate, so that all the iron elements are replaced by Fe 3+ The form exists, heat the filtrate to 60 ℃, then add an appropriate amount of concentrated ammonia water, adjust the pH value to 3.2, and only make the iron element in the filtrate as Fe 3 Precipitation in the form of iron, so as to realize the separation of iron from tailings.

[0025] Take a certain amount of Fe 3 The precipitate was washed with deionized water several times and then calcined to obtain Fe 2 o 3 , weighed, and elemental analysis was performed to obtain the percentage content of iron element, which provided a basis for subsequent preparation work. Table 1 is the elemental analysis table of the calcined product. Pure Fe 2 o 3 The percentage composi...

Embodiment 2

[0033] Step 1: Same as Step 1 in Example 1, realize the separation of iron in iron tailings.

[0034] Step 2: Fe obtained by separating iron 3 The precipitate was washed with deionized water several times and then dissolved in hydrochloric acid to obtain FeCl 3 of aqueous solution. Add metered FeSO 4 ·7H 2 0, so that Fe in solution 3+ and Fe 2+ The molar ratio is 1.5:1, and a certain amount of 1 mol / L NaOH aqueous solution is prepared simultaneously as a precipitating agent. in Fe 3+ and Fe 2+ Add surfactant sodium lauryl sulfate (C 12 h 25 OSO 3 Na), Fe 3+ The molar ratio to sodium lauryl sulfate is 10:1. Under the action of ultrasonic waves with a power of 200 W and a frequency of 100 kHz, Fe 3+ and Fe 2+ The mixed solution is slowly dropped into NaOH lye, OH - The molar mass of Fe 3+ and Fe 2+ Fe in the mixed solution 3+ The molar ratio is 4.5:1.

[0035] Step 3: with step 3 in embodiment 1, make Fe 3 0 4 magnetic powder. Field emission scanning elec...

Embodiment 3

[0037] Step 1: Same as Step 1 in Example 1, realize the separation of iron in iron tailings.

[0038] Step 2: with the step 2 in the embodiment 1, the Fe in the solution 3+ and Fe 2+ The mol ratio is 1.75:1, and surfactant is the mixture of sodium lauryl sulfate and polyethylene glycol, and Fe in the solution 3+的 The molar ratio is 0.125:1, and the alkaline precipitant is ammonia water, OH - The molar mass of Fe 3+ and Fe 2+ Fe in the mixed solution 3+ The molar ratio is 4.25:1 under the action of ultrasonic waves with a power of 125 W and a frequency of 70 kHz.

[0039] Step 3: Wait for a large amount of black Fe 3 0 4 After the particles were formed, they were heated in a water bath to 75 °C, crystallized for 90 min, and then centrifuged. The precipitate was washed with deionized water for several times, and then placed in a drying oven at 70 °C for 2 h at constant temperature to obtain Fe 3 0 4 magnetic powder.

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Abstract

The invention belongs to a method for preparing paramagnetic Fe3O4 nanoparticles by using iron tailings. The method comprises the following steps of: dissolving the iron tailings in a hydrochloric acid solution, filtering, and washing to realize solid-liquid separation; adding hydrogen peroxide into filtrate to oxidize Fe<2+> into Fe<3+>, adding ammonia water to regulate the pH to be 3.2, and ensuring that only Fe<3+> ions in various metal ions in the filtrate are precipitated in a form of Fe3 to separate iron; dissolving the Fe3 precipitate obtained through separation by using hydrochloric acid, adding a Fe<2+> solution, ensuring that a molar ratio of Fe<3+> to Fe<2+> in the solution is 1.5:1-1.75:1, performing coprecipitation reaction under the action of an alkali solution precipitator to obtain Fe3O4 nanoparticles, and performing ultrasonic dispersion and surfactant modification to make the prepared Fe3O4 nanoparticles have high purity, the particle size of less than 20nm, uniform particle distribution, high particle dispersibility, superparamagnetism and the saturation magnetization of 74.86emu / g. The invention provides a way for recycling waste iron tailings; and the method is easy to implement and low in cost, the environmental burden is effectively reduced, and the added value of waste resources can be improved.

Description

technical field [0001] The invention provides a method for preparing superparamagnetic ferric iron tetroxide nanoparticles by utilizing iron tailings, and belongs to the fields of secondary utilization of resources and preparation of inorganic nanometer materials. Background technique [0002] With the depletion of raw ore resources, the secondary utilization of tailings has received widespread attention. Iron tailings are one of the most important industrial solid wastes. Since the residual strong magnetic substances in iron tailings are very small, most of them are weak magnetic substances, and the composition is complex and the particle size is fine. Or the flotation treatment effect is not good, so that its utilization rate in our country is very low, only 7%. In my country's mining and metallurgical industries, the iron tailings that are difficult to dispose of are mainly discharged to tailings ponds as waste, and a small amount is treated by concentrated filtration an...

Claims

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Application Information

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IPC IPC(8): C01G49/08B82Y40/00B09B3/00
Inventor 孙爱芝吴深徐文欢张倩邹超杨俊董娟
Owner UNIV OF SCI & TECH BEIJING
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