CN103420428A - Preparation method of magnesium ferrite nano-particles - Google Patents
Preparation method of magnesium ferrite nano-particles Download PDFInfo
- Publication number
- CN103420428A CN103420428A CN2012103769897A CN201210376989A CN103420428A CN 103420428 A CN103420428 A CN 103420428A CN 2012103769897 A CN2012103769897 A CN 2012103769897A CN 201210376989 A CN201210376989 A CN 201210376989A CN 103420428 A CN103420428 A CN 103420428A
- Authority
- CN
- China
- Prior art keywords
- mixture
- ultrasonic
- preparation
- nano particle
- carrying
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Abstract
The invention discloses a preparation method of magnesium ferrite nano-particles. The preparation method comprises the following steps of mixing magnesium powder and deionized water into a first mixture according to a ratio of 1g: 25mL to 1g: 20mL, carrying out ultrasonic hydrolysis of the first mixture at a normal temperature under normal pressure to obtain white liliquoid, carrying out constant-temperature drying of the white liliquoid, grinding the dried white liliquoid to obtain Mg(OH)2 nano-particles, weighing the Mg(OH)2 nano-particles and FeCl3.6H2O according to an element content ratio of Mg to Fe of 1: 2, adding the weighed Mg(OH)2 nano-particles into a first beaker with deionized water, carrying out ultrasonic pre-treatment for 1h, putting the weighed FeCl3.6H2O into a second beaker, carrying out precipitation by a chemical coprecipitation method to obtain Fe(OH)3 precipitates, diluting the Fe(OH)3 precipitates by deionized water so that the Fe(OH)3 precipitates have a pH value of 7, mixing the pretreated Mg(OH)2 and the dilute Fe(OH)3 precipitates having a pH value of 7 by stirring for a certain time to obtain a second mixture, carrying out ultrasonic activation of the second mixture under normal pressure, in ultrasonic activation, taking out the mixture, carrying out stirring multiple times to obtain a third mixture, carrying out constant-temperature drying of the third mixture to obtain a forth mixture, grinding the forth mixture into powder, putting the powder into a muffle furnace, carrying out calcination at a temperature of 700 DEG C for 5h, and carrying out cooling in the muffle furnace.
Description
Technical field
A kind of preparation method of magnesium ferrite nano particle, particularly a kind of preparation method of ultrasonic auxiliary synthetic magnesium ferrite nano particle.
Technical background
Magnesium ferrite is as a kind of multicomponent composite oxide of spinel structure, and its absorbing property is subject to people's common concern already.Ferromagnetic oxide is the electromagnetic wave absorbent material with complex phase dielectric loss and magnetic loss, and the synthetic and performance study that wherein has spinel structure ferrous acid magnesium is the hot research problem always.Mg in magnesium ferrite does not have magnetic moment, and the wustite with the metallic cation of magnetic moment is low than other for each diversity of magnetic, also shows superparamagnetism when particularly the particle diameter of magnesium ferrite is reduced to nano level, and hertzian wave is shown to better shielding absorptive capacity.In recent years, to be found to have good catalytic performance be catalyzer in the organic synthesis process to magnesium ferrite.
At present, the method for preparing the magnesium ferrite nano particle has a lot, commonly used have ceramic process method, a high-temperature solid phase reaction method, and 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, inverse titrating chemical co-precipitation method, hydrothermal synthesis method and microwave process for synthesizing etc., yet these preparation methods relate to High Temperature High Pressure, the various product caused 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 synthetic method of spinel structure magnesium frrite nano particles, and (application number: 200710057615.8), this method is carried out ferric ion and the divalence magnesium ion in aqueous phase extracted by organic extractant, makes the organic phase precursor; With obtaining pure loaded metal organic phase precursor after the second distillation water washing; Organic phase is mixed in rear introducing autoclave, is within 3: 1 or 4: 1, to add distilled water according to the ratio of organic phase and water, and sealing is carried out strong stirring to solution, and the temperature of hydrothermal stripping is reacted 2.5 hours between 200～300 ℃; Naturally cool to room temperature, separatory, centrifugation, washing, under 50 ℃, drying is 30～180 minutes, obtains the magnesium ferrite product.This method organic raw material can recycle; The discharge of waste water is low; Be convenient to the size of oxide precipitation particle is controlled in ultra micro rice scope.But reaction relates to High Temperature High Pressure; The easy residual impurity of product.
Patent Office of the People's Republic of China has announced a kind of preparation method of nano magnesium ferrite, and (application number: 201110071394.6), this method is by FeCl
36H
2O and FeCl
24H
2O mixes in 1: 1 in molar ratio, drips the NaOH solution of 2mol/L, by chemical coprecipitation, prepares magnetic Fe
3O
4Nanoparticle; Put it into again 500 ℃ of roasting 3～4h of retort furnace, obtain nanometer Fe
2O
3The magnesium powder is placed in to beaker, adds deionized water, be placed in ultrasonic cleaner and process 5～8h, obtain white opacity liquid; Get the upper strata turbid solution and put in clean beaker, enter the loft drier freeze-day with constant temperature, products therefrom is ground to obtain to nanometer Mg (OH)
2By nanometer Mg (OH)
2Put into 350 ℃ of lower roasting 3～4h of retort furnace, by Fe
3O
4Nanoparticle is put into 500 ℃ of lower roasting 3～4h of retort furnace; Obtain respectively nano-MgO and nanometer Fe
2O
3Get nanometer Fe
2O
3And nano-MgO, mixing in 1: 1 in molar ratio adds deionized water, processes 10～12h and obtain red turbid solution in ultrasonic cleaner, and the upper strata turbid solution is drawn in clean beaker, after putting into the loft drier freeze-day with constant temperature, products therefrom is ground to obtain to nano magnesium ferrite.Nano magnesium ferrite prepared by this method is with low cost, and purity is high, and pattern is even, environment friendly and pollution-free.But the process complexity, energy consumption is high.
Summary of the invention
A kind of preparation method of magnesium ferrite nano particle is characterized in that:
A: the first mixture that magnesium powder and deionized water are mixed to gained with the ratio of 1g:25mL～1g:30mL ultrasonic hydrolysis at normal temperatures and pressures makes white liliquoid;
B: by after white liliquoid constant temperature drying, grind with agate mortar, to obtain Mg (OH)
2Nano particle;
C: by constituent content, than Mg/Fe=1:2, take Mg (OH)
2Nano particle and FeCl
36H
2O;
D: by the described Mg (OH) taken
2Nano particle adds ultrasonic pretreatment 1h in the first beaker with deionized water; By the FeCl taken
36H
2O inserts in the second beaker, by chemical coprecipitation, prepares Fe (OH)
3The precipitation, with deionized water by described Fe (OH)
3The precipitation dilution is for neutral;
E: by pretreated Mg (OH) in step D
2With described dilution be neutral Fe (OH)
3The second mixture that precipitation mix and blend certain hour forms carries out ultrasonic activation under normal pressure, takes out to stir repeatedly to obtain the 3rd mixture midway;
F: the 3rd mixture constant temperature drying is obtained to 4 mixture, with agate mortar by this 4 mixture grind into powder;
G: powder is put into to retort furnace at 700 ℃ of lower roasting 5h, obtain nano magnesium ferrite after furnace cooling.
The preparation method of ultrasonic auxiliary synthetic magnesium ferrite nano particle provided by the invention, be further characterized in that: wherein, the first mixture is formulated with the ratio of 1g:25mL by magnesium powder and deionized water.
The preparation method of ultrasonic auxiliary synthetic magnesium ferrite nano particle provided by the invention, be further characterized in that: wherein, the first mixture is formulated with the ratio of 1g:30mL by magnesium powder and deionized water.
The preparation method of ultrasonic auxiliary synthetic magnesium ferrite nano particle provided by the invention, be further characterized in that: wherein, white liliquoid is 40kHz by the first mixture being inserted to frequency, and power is that in the 120W ultrasonic cleaner, ultrasonic hydrolysis 4h～8h makes;
The 3rd mixture is 40kHz by the second mixture being put into to frequency, and power is that in the 300W temperature ultrasonic cleaner that is 60 ℃, ultrasonic activation 4h makes.
The preparation method of ultrasonic auxiliary synthetic magnesium ferrite nano particle provided by the invention, be further characterized in that: wherein, certain hour is 20～30 minutes.
Invention effect and effect
In sum, the preparation method of magnesium ferrite nano particle provided by the invention mixes the magnesium powder also ultrasonic hydrolysis at normal temperatures and pressures and makes white liliquoid with deionized water, its preparation process energy consumption is low, wherein, white liliquoid and mixing solutions make in using common ultrasonic cleaner, its equipment cost is cheap, and preparation technology is simple, for the preparation of nano magnesium ferrite provides a new approach.
The accompanying drawing explanation
The XRD diffraction that Fig. 1 is preparation-obtained nano magnesium ferrite in embodiment.
The TEM figure that Fig. 2 is preparation-obtained nano magnesium ferrite in embodiment.
The electron-diffraction diagram that Fig. 3 is preparation-obtained nano magnesium ferrite in embodiment.
Embodiment
Preparation method's method referring to accompanying drawing to magnesium ferrite nano particle involved in the present invention is elaborated.
Embodiment
Adopt a kind of preparation method's method of magnesium ferrite nano particle, step is as follows:
Steps A: the magnesium powder that is 99% by 2g purity is put into beaker, and adding the first mixture obtained after the 50mL deionized water to insert frequency is 40kHz, and in the ultrasonic cleaner that power is 120W, under normal temperature and pressure, ultrasonic hydrolysis makes white liliquoid after 4 hours;
Step B: after white liliquoid is dried in the thermostatic drying chamber of 80 ℃, grind with agate mortar, to obtain Mg (OH)
2Nano particle;
Step C: by constituent content, than Mg/Fe=1:2, take Mg (OH)
2Nano particle and FeCl
36H
2O;
Step D: by the Mg (OH) taken
2It is 40kHz by frequency that nano particle adds in the first beaker with deionized water, and power is that the 120W ultrasonic cleaner is at lower ultrasonic hydrolysis 1h; By the 9.2705g FeCl taken
36H
2O inserts in the second beaker that the 300mL deionized water is housed, stir on the magnetic stirring apparatus that to be placed on temperature be 90 ℃, then slowly add NaOH solution to the pH value of high density to be greater than 12, add a large amount of deionized waters after 5min, and put into cold water and be cooled to room temperature, obtain brown Fe (OH)
3Precipitation is finally neutral with washed with de-ionized water to solution repeatedly;
Step e: by the pretreated Mg of step D (OH)
2With described dilution be neutral Fe (OH)
3Precipitation mix and blend 30 minutes forms the second mixture, then this second mixture is put into to frequency is 40kHz, power be in the 300W ultrasonic cleaner with the temperature ultrasonic activation 4h of 60 ℃, obtain the 3rd mixture; Take out and stir 3 times in ultrasonic procedure, each 10 minutes;
Step F: above-mentioned the 3rd mixture is placed in the thermostatic drying chamber of 70 ℃ and dries the 4 mixture obtained, re-use agate mortar by this 4 mixture grind into powder;
Step G: powder is put into to retort furnace at 700 ℃ of lower roasting 5h, obtain nano magnesium ferrite after furnace cooling.
The XRD diffractogram that Fig. 1 is preparation-obtained magnesium ferrite nanometer in the present embodiment, as shown in Figure 1, this collection of illustrative plates diffraction peak shape is sharp-pointed, and all diffraction peaks are all and MgFe
2O
4Standard diffraction peak coupling.Illustrate that magnesium ferrite nanometer prepared by the present invention is typical spinel structure, and crystalline condition is good.
The TEM figure that Fig. 2 is preparation-obtained magnesium ferrite nanometer in the present embodiment, as can be seen from the figure, the magnesium ferrite nanometer is particulate state, is evenly distributed, particle size is between 20～45nm.
The electron-diffraction diagram that Fig. 3 is preparation-obtained magnesium ferrite nanometer in the present embodiment, as can be seen from the figure, the prepared magnesium ferrite of the present invention is single crystal structure, and crystallinity is good.Embodiment effect and effect
The preparation method preparation technology of the magnesium ferrite nano particle that the present embodiment provides is simple, and equipment cost is cheap, environment friendly and pollution-free, for the preparation of nano magnesium ferrite provides a new approach.
Also the magnesium powder can be mixed and makes the first mixture with the ratio of 1g:25mL～1g:30mL with deionized water in the above-described embodiments in addition, thereby reach the effect identical with the present invention.
White liliquoid in the present embodiment also can make by ultrasonic hydrolysis 4h～8h in ultrasonic cleaner, thereby reaches the effect identical with the present embodiment.
Also can be by the Fe (OH) made in the present embodiment
3Precipitation and pretreated Mg (OH)
2Mix and blend forms the second mixture in 20～30 minutes, thereby reaches the effect identical with the present embodiment.
Claims (5)
1. the preparation method of a magnesium ferrite nano particle is characterized in that:
A: the first mixture that magnesium powder and deionized water are mixed to gained with the ratio of 1g:25mL～1g:30mL ultrasonic hydrolysis at normal temperatures and pressures makes white liliquoid;
B: by after described white liliquoid constant temperature drying, grind with agate mortar, to obtain Mg (OH)
2Nano particle;
C: by constituent content, than Mg/Fe=1:2, take described Mg (OH)
2Nano particle and FeCl
36H
2O;
D: by the described Mg (OH) taken
2Nano particle adds ultrasonic pretreatment 1h in the first beaker with deionized water; By the FeCl taken
36H
2O inserts in the second beaker, by chemical coprecipitation, prepares Fe (OH)
3The precipitation, with deionized water by described Fe (OH)
3The precipitation dilution is for neutral;
E: by pretreated Mg (OH) in step D
2With described dilution be neutral Fe (OH)
3The second mixture that precipitation mix and blend certain hour forms carries out ultrasonic activation under normal pressure, takes out to stir repeatedly to obtain the 3rd mixture midway;
F: described the 3rd mixture constant temperature drying is obtained to 4 mixture, with agate mortar by this 4 mixture grind into powder;
G: described powder is put into to retort furnace at 700 ℃ of lower roasting 5h, obtain nano magnesium ferrite after furnace cooling.
2. the preparation method of ultrasonic auxiliary synthetic magnesium ferrite nano particle according to claim 1 is further characterized in that:
Wherein, described the first mixture is formulated with the ratio of 1g:25mL by described magnesium powder and deionized water.
3. the preparation method of ultrasonic auxiliary synthetic magnesium ferrite nano particle according to claim 1 is further characterized in that:
Wherein, described the first mixture is formulated with the ratio of 1g:30mL by described magnesium powder and deionized water.
4. according to the preparation method of the described ultrasonic auxiliary synthetic magnesium ferrite nano particle of claim 2 or 3, be further characterized in that:
Wherein, described white liliquoid is 40kHz by described the first mixture is inserted to frequency, and power is that in the 120W ultrasonic cleaner, ultrasonic hydrolysis 4h～8h makes;
Described the 3rd mixture is 40kHz by described the second mixture is put into to frequency, and power is ultrasonic activation 4h in the 300W temperature ultrasonic cleaner that is 60 ℃, takes out to stir repeatedly to obtain midway.
5. the preparation method of ultrasonic auxiliary synthetic magnesium ferrite nano particle according to claim 4 is further characterized in that:
Wherein, described certain hour is 20～30 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103769897A CN103420428A (en) | 2012-09-28 | 2012-09-28 | Preparation method of magnesium ferrite nano-particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103769897A CN103420428A (en) | 2012-09-28 | 2012-09-28 | Preparation method of magnesium ferrite nano-particles |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103420428A true CN103420428A (en) | 2013-12-04 |
Family
ID=49645872
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012103769897A Pending CN103420428A (en) | 2012-09-28 | 2012-09-28 | Preparation method of magnesium ferrite nano-particles |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103420428A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105753059A (en) * | 2016-03-23 | 2016-07-13 | 上海理工大学 | Preparation method of carbon-based magnesium ferrite composite membrane with wave absorbing function |
| 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 |
| CN106315639A (en) * | 2016-08-02 | 2017-01-11 | 上海理工大学 | Ultrasonic preparation method of high-purity ZnAl2O4 nano particles |
| CN106848277A (en) * | 2017-01-22 | 2017-06-13 | 曲阜师范大学 | A kind of magnesium iron oxygen/carbon composite and preparation method thereof |
| CN110252304A (en) * | 2018-03-12 | 2019-09-20 | 中国石油化工股份有限公司 | Fe-series catalyst and its preparation method and application and carbon nanotube and preparation method 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 |
| CN114180639A (en) * | 2021-12-08 | 2022-03-15 | 程冲 | Method for preparing yellow inorganic nano oxide pigment by steam drying and crushing |
| CN114180639B (en) * | 2021-12-08 | 2024-05-10 | 程冲 | Method for preparing yellow inorganic nano oxide pigment by steam drying and crushing |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101070192A (en) * | 2007-06-13 | 2007-11-14 | 天津大学 | Method for synthesizing spinel structure magnesium frrite nano particles |
| CN102107910A (en) * | 2011-03-23 | 2011-06-29 | 上海理工大学 | Preparation method of nano magnesium ferrite |
| EP2377811A2 (en) * | 2008-12-24 | 2011-10-19 | Nuri Vista Co., Ltd. | Method for preparing engineered mg doped ferrite superparamagnetic nano particle exhibiting ac magnetic induction heating at high temperature and mg doped ferrite superparamagnetic nano particles engineered by the method |
-
2012
- 2012-09-28 CN CN2012103769897A patent/CN103420428A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101070192A (en) * | 2007-06-13 | 2007-11-14 | 天津大学 | Method for synthesizing spinel structure magnesium frrite nano particles |
| EP2377811A2 (en) * | 2008-12-24 | 2011-10-19 | Nuri Vista Co., Ltd. | Method for preparing engineered mg doped ferrite superparamagnetic nano particle exhibiting ac magnetic induction heating at high temperature and mg doped ferrite superparamagnetic nano particles engineered by the method |
| CN102107910A (en) * | 2011-03-23 | 2011-06-29 | 上海理工大学 | Preparation method of nano magnesium ferrite |
Non-Patent Citations (1)
| Title |
|---|
| 吕维忠等: "超声波化学法合成纳米铁酸镁粉末", 《电子元件与材料》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105753059A (en) * | 2016-03-23 | 2016-07-13 | 上海理工大学 | Preparation method of carbon-based magnesium ferrite composite membrane with wave absorbing function |
| 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 |
| CN106315639A (en) * | 2016-08-02 | 2017-01-11 | 上海理工大学 | Ultrasonic preparation method of high-purity ZnAl2O4 nano particles |
| CN106848277A (en) * | 2017-01-22 | 2017-06-13 | 曲阜师范大学 | A kind of magnesium iron oxygen/carbon composite and preparation method thereof |
| CN110252304A (en) * | 2018-03-12 | 2019-09-20 | 中国石油化工股份有限公司 | Fe-series catalyst and its preparation method and application and carbon nanotube and preparation method thereof |
| 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 |
| 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 |
| CN114180639A (en) * | 2021-12-08 | 2022-03-15 | 程冲 | Method for preparing yellow inorganic nano oxide pigment by steam drying and crushing |
| CN114180639B (en) * | 2021-12-08 | 2024-05-10 | 程冲 | Method for preparing yellow inorganic nano oxide pigment by steam drying and crushing |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102107910B (en) | Preparation method of nano magnesium ferrite | |
| Sam et al. | Preparation of MnFe2O4 nanoceramic particles by soft chemical routes | |
| CN103420428A (en) | Preparation method of magnesium ferrite nano-particles | |
| Bhavani et al. | Okra (Abelmoschus esculentus) plant extract-assisted combustion synthesis and characterization studies of spinel ZnAl2O4 nano-catalysts | |
| CN102745675A (en) | Preparation method of spinel-type magnetic MFe2O4/graphene composite material | |
| CN101481107B (en) | Preparation of nickel-zine ferrite (Ni1-xZnxFe2O4) coated carbon nano-tube magnetic nano composite material | |
| CN102660220A (en) | Preparation method of graphene supported ferriferrous oxide nanocomposite | |
| CN103964505B (en) | A kind of preparation method of columbite shaped metal niobate nanostructure | |
| CN108393073A (en) | A kind of preparation method of general magnetic adsorbent and application | |
| CN101070192B (en) | Method for synthesizing spinel structure magnesium ferrite nano particles | |
| Khan et al. | Nanocrystalline La1− xSrxCo1− yFeyO3 perovskites fabricated by the micro-emulsion route for high frequency response devices fabrications | |
| CN102643082A (en) | Preparation method of W-shaped barium ferrite | |
| CN103447024B (en) | The preparation method of a kind of bismuthino strontium magnetic photocatalyst and bismuthino strontium magnetic photocatalyst thereof | |
| CN103818971B (en) | A kind of preparation method of superparamagnetism ferrite nano particles | |
| Liu et al. | Preparation of Cu–Zn ferrite photocatalyst and it's application | |
| CN102079544A (en) | Rapid synthesis method of ferric oxide nano powder | |
| CN102850056A (en) | Preparation method of spherical ferrite | |
| Li et al. | Syntheses of perovskite-type composite oxides nanocrystals by solid-state reactions | |
| Xi et al. | Study of the preparation of NI–Mn–Zn ferrite using spent NI–MH and alkaline Zn–Mn batteries | |
| CN101525156B (en) | Preparation method for nanometer zinc ferrite | |
| CN104003706B (en) | A kind of preparation method of nanometer ferrite composite wave-absorbing body | |
| CN105253918B (en) | A kind of easily dispersion hexagonal plate W-type ferrite BaZn2Fe16O27Preparation method | |
| CN109759071A (en) | A kind of preparation method of cerium dopping magnetic composite nano material | |
| CN102180522B (en) | Controllable preparation method of nano magnetic iron oxide with narrow particle size distribution | |
| CN103774236A (en) | Cryptomelane-type K(2-x)CoyNizMn(8-y-z)O16 nanowire and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20131204 |