CN102107910B - Preparation method of nano magnesium ferrite - Google Patents
Preparation method of nano magnesium ferrite Download PDFInfo
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- CN102107910B CN102107910B CN2011100713946A CN201110071394A CN102107910B CN 102107910 B CN102107910 B CN 102107910B CN 2011100713946 A CN2011100713946 A CN 2011100713946A CN 201110071394 A CN201110071394 A CN 201110071394A CN 102107910 B CN102107910 B CN 102107910B
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Abstract
The invention relates to a preparation method of nano magnesium ferrite, which comprises the following steps: mixing FeCl3.6H2O and FeCl2.4H2O in a mol ratio of 1:1, dropwisely adding a 2 mol/L NaOH solution, and preparing magnetic Fe3O4 nanoparticles by a chemical coprecipitation process; putting the magnetic Fe3O4 nanoparticles into a muffle furnace, and roasting at 500 DEG C for 3-4 hours to obtain nano Fe2O3; putting magnesium powder in a beaker, adding deionized water, and putting the beaker in an ultrasonic cleaner to treat for 5-8 hours, thereby obtaining a white turbid liquid; putting the supernatant of the turbid liquid in a clean beaker, drying in a drying box at constant temperature, and grinding the product to obtain Mg(OH)2; roasting the nano Mg(OH)2 in a muffle furnace at 350 DEG C for 3-4 hours, and roasting the Fe3O4 nanoparticles in a muffle furnace at 500 DEG C for 3-4 hours; respectively obtaining nano MgO and nano Fe2O3; and taking the nano Fe2O3 and the nano MgO, mixing the nano Fe2O3 and the nano MgO in a mol ratio of 1:1, adding deionized water, treating in an ultrasonic cleaner for 10-12 hours to obtain a red turbid liquid, sucking the supernatant of the turbid liquid into a clean beaker, drying the beaker in a drying box at constant temperature, and grinding the product to obtain the nano magnesium ferrite. The nano magnesium ferrite prepared by the method provided by the invention has the advantages of low cost, high purity, uniform appearance, environmental protection and no pollution.
Description
Technical field
The present invention relates to a kind of nanometer magnesium ferrite (MgFe
2O
4) the preparation method, belong to the nano material preparation technical field.
Background technology
MgFe
2O
4As a kind of multicomponent composite oxide of spinel structure, its absorbing property and air-sensitive performance receive people's common concern already.Ferromagnetic oxide is the electromagnetic wave absorbent material with complex phase dielectric loss and magnetic loss, wherein has the MgFe of spinel structure
2O
4Synthetic and performance study be the hot research problem always.MgFe
2O
4In Mg do not have magnetic moment, each diversity of magnetic is lower than the wustite of metallic cation that other has magnetic moment, particularly MgFe
2O
4Particle diameter also show superparamagnetism when being reduced to nano level, hertzian wave is shown better shielding absorptive capacity.In recent years, MgFe
2O
4Coming to light, to have good gas sensing property be a kind of n N-type semiconductorN gas sensitive.
At present, preparation nanometer magnesium ferrite (MgFe
2O
4) method have a lot, commonly used have ceramic process method, a high-temperature solid phase reaction method, high-temperature heat treatment hydrotalcite method, microwave burning method, sol-gel method, hydrothermal stripping are followed the example of, the microemulsion precipitator method; Oxalate coprecipitation method, residual titration chemical coprecipitation, hydrothermal synthesis method and microwave process for synthesizing etc., however these preparing methods relate to HTHP; The various product that causes of intermediate steps is impure; Particle aggregation reclaim difficulty, thereby cost is also higher.
Patent Office of the People's Republic of China has announced a kind of compound method of spinel structure magnesium frrite nano particles, and (application number: 200710057615.8), this method is come ferric ion and divalence mg ion in the aqueous phase extracted through organic extractant, makes the organic phase precursor; With obtaining purified loaded metal organic phase precursor after the second distillation water washing; Organic phase being mixed the back introduce in the autoclave, is to add zero(ppm) water in 3: 1 or 4: 1 according to the ratio of organic phase and water, and sealing is carried out the brute force stirring to solution, and the temperature of hydrothermal stripping was reacted 2.5 hours between 200-300 ℃; Naturally cool to room temperature, separatory, spinning, washing was descended dry 30-180 minute at 50 ℃, got the magnesium ferrite product.This method organic raw material can recycle; The discharging of waste water is low; Be convenient to the size of oxide precipitation particle is controlled in the ultra micro rice scope.But reaction relates to HTHP; Product is prone to residual impurity.
Patent Office of the People's Republic of China has announced a kind of preparing method's (application number: 200910311162.6) of spherical nanometre magnesium ferrite desulfurizer; This method is dissolved in iron nitrate and magnesium nitrate in the terepthaloyl moietie, under intense stirring condition, adds ammonium acetate, and this microemulsion is put into autoclave 180-200 ℃ of following crystallization 24h-48h; Through filtration, washing, drying; 500 ℃ of calcining 2h in retort furnace obtain the nanometer spherical magnesium ferrite, to SO at last
2Outstanding absorption property is arranged.But process is complicated, and energy consumption is high.
Summary of the invention
The invention discloses a kind of preparation method of nanometer magnesium ferrite, its purpose is to overcome existing high-temperature high-pressure chemical prepared in reaction technology, and apparatus expensive, cost is high and can be to drawbacks such as bad border pollute.The present invention passes through nanometer Fe
2O
3Carry out supersound process with MgO, can make the nanometer magnesium ferrite, whole process operation is convenient, and is with low cost, pollution-free.
Technical scheme of the present invention is following:
A kind of preparation method of nanometer magnesium ferrite is characterized in that: may further comprise the steps:
A, with FeCl
36H
2O and FeCl
24H
2O mixed in 1: 1 in molar ratio, dripped the NaOH solution of 2mol/L, prepared magnetic Fe through chemical coprecipitation
3O
4Nanoparticle;
B, with the magnetic Fe that is equipped with of steps A preparation
3O
4The beaker of nanoparticle is put into retort furnace at 500 ℃ of roasting 3-4h, obtains nanometer Fe
2O
3
C, the magnesium powder being placed beaker, add deionized water, is in the ultrasonic cleaner of 90Hz in frequency, handles 5-8h, obtains the turbid solution of white;
D: the upper strata turbid solution is drawn in the clean beaker, put into behind the loft drier freeze-day with constant temperature with products therefrom with agate mortar grind nanometer Mg (OH)
2
E: with nanometer Mg (OH)
2Put into retort furnace at 350 ℃ of following roasting 3-4h, obtain nano-MgO;
F: take by weighing nanometer Fe
2O
3And nano-MgO, mixed to place beaker in 1: 1 in molar ratio, add deionized water,, frequency handles 10-12h in being the ultrasonic cleaner of 90Hz;
G: red turbid solution the upper strata turbid solution is drawn in the clean beaker, put into the loft drier freeze-day with constant temperature after, with products therefrom with agate mortar grind the nanometer magnesium ferrite.
The invention has the advantages that handling the magnesium powder through ultrasonic cleaner can make nano-sized magnesium hydroxide; Product after Marinco H and the Z 250 roasting is carried out supersound process once more; Can make the nanometer magnesium ferrite under the room temperature, break through the chemical reaction of traditional HTHP.Adopt the nanometer magnesium ferrite of the inventive method preparation with low cost, purity is high, and pattern is even, and environment friendly and pollution-free, for the preparation of nanometer magnesium ferrite provides a new approach.
Description of drawings
Fig. 1 is the XRD figure of the prepared nanometer magnesium ferrite of specific embodiment;
Fig. 2 is the TEM figure of the prepared nanometer magnesium ferrite of specific embodiment.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is done and to further describe.
A kind of preparation method of nanometer magnesium ferrite, concrete preparation process is following:
A, get 2.77gFeCl
36H
2O, 1.99gFeCl
24H
2O places beaker; Add 100mlNaOH solution, prepare magnetic Fe through chemical coprecipitation
3O
4Nanoparticle;
B, with the magnetic Fe that is equipped with of steps A preparation
3O
4The beaker of nanoparticle is put into retort furnace at 500 ℃ of roasting 3-4h, obtains nanometer Fe
2O
3
C, taking by weighing 3g magnesium powder and place another beaker, add the deionized water of 60ml, is in the ultrasonic cleaner of 90Hz in frequency, handles 5-8h, obtains the turbid solution of white, and the upper strata turbid solution is drawn in the clean beaker;
D. the temperature of setting thermostatic drying chamber is 60 ℃, the beaker that turbid solution is housed is put into the loft drier freeze-day with constant temperature after, products therefrom with agate mortar grind nanometer Mg (OH)
2
E., Mg (OH) will be housed again
2The beaker of nanoparticle is put into retort furnace at 350 ℃ of roasting 3-4h, obtains nano-MgO;
F. take by weighing the 1.71g nanometer Fe
2O
3With the 1.71g nano-MgO, mix and to insert in the beaker, add the deionized water of 60ml, in frequency is the ultrasonic cleaner of 90Hz, handle 10-12h, red turbid solution;
G. the upper strata turbid solution is drawn in the clean beaker, put into the dry 12h of 60 ℃ of thermostatic drying chambers after, products therefrom ground with agate mortar obtains the nanometer magnesium ferrite.
Fig. 1 is the XRD diffractogram of the prepared nanometer magnesium ferrite that obtains of embodiment, and visible by figure, collection of illustrative plates diffraction peak shape is sharp-pointed, the equal and MgFe of all diffraction peaks
2O
4Standard diffraction peak coupling.The product crystalline condition that preparation is described is good.
Fig. 2 is the TEM figure of the prepared nanometer magnesium ferrite that obtains of embodiment, and as can be seen from the figure, the nanometer magnesium ferrite is a particulate state, is evenly distributed, and particle size is between 25-35nm, and median size is about 30nm.
Claims (1)
1. the preparation method of a nanometer magnesium ferrite is characterized in that: may further comprise the steps:
A. with FeCl
36H
2O and FeCl
24H
2O mixed in 1: 1 in molar ratio, dripped the NaOH solution of 2mol/L, prepared magnetic Fe through chemical coprecipitation
3O
4Nanoparticle;
B. with the magnetic Fe that is equipped with of steps A preparation
3O
4The beaker of nanoparticle is put into retort furnace at 500 ℃ of roasting 3-4h, obtains nanometer Fe
2O
3
C. the magnesium powder being placed beaker, add deionized water, is in the ultrasonic cleaner of 90Hz in frequency, handles 5-8h, obtains the turbid solution of white;
D: the upper strata turbid solution is drawn in the clean beaker, put into behind the loft drier freeze-day with constant temperature with products therefrom with agate mortar grind nanometer Mg (OH)
2
E: with nanometer Mg (OH)
2Put into retort furnace at 350 ℃ of following roasting 3-4h, obtain nano-MgO;
F: take by weighing nanometer Fe
2O
3And nano-MgO, mixing in 1: 1 is in molar ratio inserted in the beaker, adds deionized water, in frequency is the ultrasonic cleaner of 90Hz, handles 10-12h, red turbid solution;
G: the upper strata turbid solution that step F is obtained is drawn in the clean beaker, put into the loft drier freeze-day with constant temperature after, with products therefrom with agate mortar grind the nanometer magnesium ferrite.
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| CN102107910B true CN102107910B (en) | 2012-07-11 |
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103420428A (en) * | 2012-09-28 | 2013-12-04 | 上海理工大学 | Preparation method of magnesium ferrite nano-particles |
| CN103073063B (en) * | 2012-12-17 | 2014-11-12 | 沈阳化工大学 | Method for preparing nanometer magnesium ferrite through utilizing active magnesium oxide as raw material |
| CN104741123A (en) * | 2015-03-11 | 2015-07-01 | 大连理工大学 | Novel nano ferrite adsorption desulfurization catalyst and preparation method thereof |
| CN105753059B (en) * | 2016-03-23 | 2018-06-15 | 上海理工大学 | A kind of preparation method of carbon-based magnesium ferrite composite wave-absorbing film |
| CN106315639A (en) * | 2016-08-02 | 2017-01-11 | 上海理工大学 | Ultrasonic preparation method of high-purity ZnAl2O4 nano particles |
| CN106242548A (en) * | 2016-08-02 | 2016-12-21 | 上海理工大学 | A kind of high-purity MgAl2o4the supersonically preparation method of nano-particle |
| CN110252304B (en) * | 2018-03-12 | 2021-12-17 | 中国石油化工股份有限公司 | Iron-based catalyst, preparation method and application thereof, carbon nano tube and preparation method thereof |
| CN108554367A (en) * | 2018-05-22 | 2018-09-21 | 华东理工大学 | A method of preparing magnetic Nano iron oxide particle adsorbent |
| WO2021072635A1 (en) * | 2019-10-15 | 2021-04-22 | 诸暨易联众创企业管理服务有限公司 | Method for preparing rod-shaped ferrous chloride nano-material |
| CN111298758B (en) * | 2020-02-28 | 2023-01-17 | 内蒙古工业大学 | Lanthanum-doped magnesium ferrite composite material and preparation method and application thereof |
| CN112175020A (en) * | 2020-10-15 | 2021-01-05 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation of cyclopentadiene/magnesium ferrite/cyclopentadiene nano material, product and application |
| CN114180639B (en) * | 2021-12-08 | 2024-05-10 | 程冲 | Method for preparing yellow inorganic nano oxide pigment by steam drying and crushing |
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| JP4668574B2 (en) * | 2003-11-12 | 2011-04-13 | 関東電化工業株式会社 | Mg-based ferrite, electrophotographic developer carrier and developer using the ferrite |
| CN101070192B (en) * | 2007-06-13 | 2010-10-13 | 天津大学 | Method for synthesizing spinel structure magnesium ferrite nano particles |
| JP2009120459A (en) * | 2007-11-19 | 2009-06-04 | Admetech:Kk | METHOD OF PRODUCING MgFe2O4 USED AS LIVING BODY HEATING MATERIAL, AND MgFe2O4 OBTAINED BY THE SAME METHOD |
| CN101708423B (en) * | 2009-12-10 | 2011-09-14 | 大连理工大学 | Preparation method for spherical nanometre magnesium ferrite desulfurizer |
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