CN102295454B - Microreaction system for preparing ferrite nano powder and preparation method of ferrite nano powder - Google Patents
Microreaction system for preparing ferrite nano powder and preparation method of ferrite nano powder Download PDFInfo
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Abstract
The invention discloses a microreaction system for preparing ferrite nano powder and a preparation method of ferrite nano powder. The microreaction system comprises a feeding device, a micromixing device and a crystal growth groove, wherein magnet coils are wound around the exteriors of the micromixing device and the crystal growth groove; and the feeding device is connected with one end of the micromixing device, and the crystal growth groove is connected with the other end of the micromixing device. The microreaction system is based on a coprecipitation method, a dynamic magnetic field is utilized to replace the traditional stirring so that reaction materials reach even micromixing effect, and generated nano particles are good in dispersion. According to the method provided by the invention, the nucleation and growth processes of a crystal are separated out, thereby effectively solving the problem of wide particle distribution caused by uneven mass transfer in the traditional preparation method. In the preparation method disclosed by the invention, a surface active agent dose not need to be used, thereby avoiding the influence of the surface active agent on a nano ferrite powder surface and being beneficial to application of nano ferrite. The preparation method disclosed by the invention is simple in process, is convenient for operation, and is especially suitable for large-scale continuous production.
Description
Technical field
The present invention relates to the nano-powder material field, particularly relate to a kind of little reaction system of ferrite nano powder preparation, and the preparation method of ferrite nano powder.
Background technology
Magnetic Nano material is to produce gradually, develop, grow in strength and become to be full of vitality most and the novel magnetic material of broad prospect of application after the seventies in 20th century.In general, because nano material has little size and bigger features such as specific area, compare with body phase magnetic material, magnetic Nano material has some novel features, as small-size effect, skin effect, quantum size effect, macro quanta tunnel effect etc.Utilize the magnetic characteristic of many uniquenesses that magnetic Nano material has, can make the material of variforms such as nanometer magnetic film (comprising the magnetic multilayer film), nanometer magnet-wire, nano-magnetic powder and magnetic liquid, thereby it has obtained in conventional art and high technology industry, industrial and agricultural production, biomedical sector, national defence scientific research and social life extensively and important use.Ferromagnetic oxide powder and device have played great function to development most advanced branches of science technology and the reinforcement development of the national economy.In many Ferrite Materials, spinel type ferrite is with fastest developing speed, most species, most widely used a kind of ferrite, and as magnetic recording medias such as our tape used in everyday, disks, what adopt more than 80% all is spinel type ferrite.
The preparation method of nanometer ferrite and technology of preparing have directly determined the performance of nanometer ferrite, thereby further have influence on manufacturing and the economic benefit of device.The preparation method of spinel type ferrite is a lot, mainly contains mechanical ball-milling method, coprecipitation, thermal decomposition method, hydro-thermal method, sol-gel process, microemulsion method etc.Wherein, the wet chemistry method of preparation ferromagnetic oxide powder is described as the best approach that the preparation magnetic recording is used magnetic always in solution.The wet preparation method that generally uses still is the method for preparing pigment the thirties in 20th century now, but this method preparation section is various, the condition harshness, as require deoxygenation, environment purifications etc. more and more can not adapt to magnetic recording to the needs of high-density development.Advantages such as coprecipitation is because simple, the applicability of its technology is strong, not high to equipment, specification requirement, and product purity height, particle size are little are widely used in preparation ferrite magnetic nano particle in recent years.But the magnetic-particle particle diameter wider distribution of this method preparation, it is serious to reunite, and is difficult to large-scale production.Traditional solution is to disperse with ultrasonic wave in course of reaction or add surfactant to reach the purpose of disperseing magnetic particle in solution.But dispersion effect is subjected to the restriction of ultrasonic power and coverage, and surfactant is difficult to washing, and factors such as magnetic particle surface clad surface activating agent are had a greatly reduced quality the performance of magnetic particle.
Therefore, seek, develop a kind of new equipment and technology of preparing and become the key that can the nanometer ferrite particle obtain more effective and extensive use.
Summary of the invention
The purpose of this invention is to provide a kind of little reaction system for preparing the ferrite nano powder.
Another object of the present invention provides and a kind ofly adopts described little reaction system to prepare the method for ferrite nano powder.
To achieve these goals, the present invention has adopted following technical scheme:
The invention discloses a kind of little reaction system for preparing the ferrite nano powder, described little reaction system comprises feeding device, micro mixing device and crystal growth groove; Feeding device links to each other with the arrival end of micro mixing device, and the crystal growth groove links to each other with the port of export of micro mixing device; Described micro mixing device comprises micro-mixer and winding at its outside solenoid.The effect that it is pointed out that described micro-mixer is to make that reactant liquor evenly mixes, and forms a large amount of nucleus, and, under the effect of solenoid, strengthened mass transfer and the mixing function of micro-mixer, make the nucleus that forms evenly disperse; Described crystal growth groove is nonconducting container that can be used for water-bath or evenly heat, this container can be the container that plastics, glass, pottery or other material are made, its role is to make and the reactant liquor water-bath therein that contains nucleus make nucleus further grow into needed crystal.
Further, the outside of described crystal growth groove is arranged with solenoid.The main effect that it is pointed out that the solenoid in micro mixing device and the crystal growth groove is to produce dynamic electromagnetic field, and magnetic particle is played the mixed uniformly effect of microcosmic.In micro mixing device, reactant liquor is uniformly mixed to form a large amount of nucleus; In the crystal growth groove, nucleus is further grown up, because the problem that nano particle is easily reunited in the conventional method has been avoided in the introducing of dynamic magnetic field, make that the nano particle that generates is more even, and particle size range is narrow, good dispersion.
Described feeding device comprises reservoir and constant flow pump, has at least two cover feeding devices to link to each other with micro mixing device in described little reaction system; The quantity that it is pointed out that feeding device is determined according to the quantity of reactant liquor, also can improve by actual demand.The little reaction system that also it is pointed out that above-mentioned preparation ferrite nano powder not only is applicable to the preparation of nano-powder, can be applied to the preparation of other magnetic nano powder material equally.
The invention also discloses a kind of improved coprecipitation and prepare the method for ferrite nano powder, described method is carried out at above-mentioned little reaction system; Comprise reactant liquor is mixed in micro mixing device, form a large amount of nucleus, water-bath growth in the crystal growth groove then, synthetic described ferrite nano powder.It is pointed out that in the said method, the nucleation of entire reaction is separated with two processes of growth of nano-powder, it is carried out in micro mixing device and crystal growth groove respectively; And in little reaction system, adopt dynamic magnetic field to replace traditional stirring, make reactant liquor can reach microcosmic and mix, in preparation process, do not need to add surfactant and just can prepare dispersed well particle.
Further, among the present invention, said method specifically comprises the steps:
A. with water-soluble divalent metal salt and water-soluble trivalent ferric salt mixed dissolution in water, as reactant liquor A, aqueous slkali is as reactant liquor B, place the feeding device of little reaction system respectively, it is pointed out that water-soluble divalent metal salt and water-soluble trivalent ferric salt among the reactant liquor A are configured by stoichiometric proportion, preferred, both ratio is 1: 2, and preferred water-soluble iron salinity is 0.01-1.0mol/L;
B. the solenoid of micro mixing device outside feeds alternating current, reactant liquor in the feeding device is sent into micro mixing device simultaneously according to stoichiometric proportion, preferably, the flow of controlling two reactant liquors is 0.1-0.4L/min, it is to be noted, preferred among the present invention, with reactant liquor A and reactant liquor B simultaneously, when sending into micro mixing device equal-volume, the ratio of its amount of substance just in time meets the stoichiometric proportion of reaction, reactant liquor A and reactant liquor B evenly mix in micro mixing device, and initial reaction forms a large amount of nucleus;
C. the nucleus in micro mixing device enters into before the crystal growth groove, solenoid to crystal growth groove outside feeds alternating current, the mixed liquor that flows out from micro mixing device enters the crystal growth groove, and with it water bath processing, it is to be noted, in fact water bath processing is exactly to make the nucleus that forms in micro mixing device further react growth, forms ferrite nanometer particle;
D. after handling through step c, with precipitated product water and the ethanol washing respectively that obtains in the crystal growth groove, oven dry namely obtains described ferrite nano powder.
Among the present invention, preferred water-soluble divalent metal comprises Fe
2+, Co
2+, Ni
2+, Zn
2+, Mn
2+In one or more, it is pointed out that at divalent metal be Fe
2+The time, can add an amount of hydrazine hydrate among the described reactant liquor B, in order to protect Fe
2+Not oxidized.
Preferred slaine comprises at least a in chlorate, nitrate, the sulfate.
Preferably, aqueous slkali comprises NaOH, KOH, NH
4At least a among the OH.
Among the present invention, the frequency of described alternating current is preferably 50-2000Hz, and the magnetic field intensity of electromagnetic field is preferably 0-1.5T.The temperature of water bath processing is preferably 40-95 ℃.
Because adopt above technical scheme, beneficial effect of the present invention is:
Adopt little reaction system provided by the invention, utilize dynamic magnetic field to replace traditional stirring, efficiently solve in the ferrite production process a series of problems such as easily reunite, inhomogeneous.This little reaction system make reactive material reach on the micro-scale evenly, make the nanoparticulate dispersed that obtains good, and can realize that low energy efficiently can produce continuously.Simultaneously, the present invention improves the method that coprecipitation prepares ferrite powder, in conjunction with little reaction system of the present invention, crystal nucleation is separated with growth course, efficiently solves the inhomogeneous wide problem of particle diameter distribution that causes of traditional preparation process method mass transfer.In the method for the present invention because the use of dynamic magnetic field, make reactive material reach on the micro-scale evenly, the nano-particles size narrowly distributing that makes; Dynamic magnetic field has been upset the microcosmic magnetic moment of ferrite particle, and dipolar magnetic interaction is reduced, and has solved the problem that magnetic particle is easily reunited, the particle good dispersion; In preparation process, do not add surfactant and just can prepare dispersed well particle, avoided the influence of surfactant to the nanometer ferrite particle surface, be conducive to the application of nanometer ferrite; In addition, by the isoparametric adjustment of concentration, reaction time, reaction temperature to mixing velocity, reactant liquor, particle diameter can be controlled in the 10-100nm scope.Preparation method's technology of ferrite nano powder provided by the invention is simple, is convenient to operation, is particularly suitable for large-scale continuous production.
Description of drawings
Fig. 1 is the experimental provision schematic diagram of little reaction system in the embodiment of the invention, and 1 is reservoir among the figure, and 2 is constant flow pump, and 3 is micro-mixer, and 4 are the crystal growth groove, and 5 is solenoid;
Fig. 2 is the CoFe of the embodiment of the invention 2 preparations
2O
4X-ray diffraction (XRD) spectrogram;
Fig. 3 is the CoFe of the embodiment of the invention 2 preparations
2O
4Transmission electron microscope (TEM) photo;
Fig. 4 is the Fe of the embodiment of the invention 3 preparations
3O
4X-ray diffraction (XRD) spectrogram;
Fig. 5 is the Fe of the embodiment of the invention 3 preparations
3O
4Transmission electron microscope (TEM) photo.
Also by reference to the accompanying drawings the present invention is described in further detail below by specific embodiment.Following examples only are further detailed the present invention, should not be construed as limitation of the present invention.
Embodiment 1
The invention discloses a kind of new little reaction system for preparing the ferrite nano powder, its innovation part mainly is presented as: set up solenoid at the micro mixing device of described little reaction system and the outside of crystal growth groove, further strengthen its mass transfer function, make reactive material reach mixing on the microcosmic.Concrete, little reaction system of the present invention comprises: feeding device, micro mixing device and crystal growth groove; Feeding device links to each other with micro mixing device one end, and the crystal growth groove links to each other with the other end of micro mixing device.Described feeding device comprises reservoir and constant flow pump, has at least two cover feeding devices to link to each other with micro mixing device in described little reaction system, and the number of feeding device is determined according to the quantity of reactant liquor.Described micro mixing device is made up of at the solenoid of micro-mixer or microreactor outside micro-mixer or microreactor and winding.Described crystal growth groove is made up of at the solenoid of stock chest outside stock chest and winding.It is pointed out that in the solenoid of above-mentioned micro mixing device and crystal growth groove outside to feed alternating current, produce dynamic magnetic field, the magnetic nano powder that generates is play a part to stir and evenly mix.Preferably, the frequency of described alternating current is preferably 50-2000Hz, and the magnetic field intensity of electromagnetic field is preferably 0-1.5T.Little reaction system of the present invention, the nucleation and growth process of crystal is separated, and adopt dynamic magnetic field to replace traditional stirring, efficiently solve the inhomogeneous wide problem of particle diameter distribution that causes of traditional preparation process method mass transfer, and realization low energy efficiently can be produced continuously, can be good at being applied in large-scale the production.
The method of preparing cobalt ferrite by coprecipitation, step is as follows:
Take by weighing 0.06mol Fe (NO
3)
39H
2O and 0.03mol CoCl
26H
2O dissolves in distilled water, obtains the 1L solution A; Measure 25% NH
4OH 50ml obtains solution B with distilled water diluting to 1L.Open two constant flow pumps, with solution A with B is isopyknic is pumped into simultaneously in the micro mixing device, control the flow of two solution at 0.2L/min, two kinds of solution have reached the even mixing of microscopic scale in the microenvironment of small container, form a large amount of nucleus in the reactant liquor; The reactant liquor that obtains enters in the crystal growth groove, and the ageing processing makes the crystal further growth in 90 ℃ of water-baths; The ac frequency that feeds in the solenoid of micro mixing device and crystal growth groove is 500Hz, magnetic field intensity 1T; The reactant liquor product that the water-bath ageing obtained after 10 hours in the crystal growth groove filters all over the back with distilled water and ethanol washing 3-5,60 ℃ of oven dry in convection oven, and drying time is 24 hours.The CoFe that obtains
2O
4Diameter is about 15nm, as shown in Figure 3.
Embodiment 3
Coprecipitation prepares the method for nano ferriferrous oxide granule, and step is as follows:
Take by weighing 0.2mol Fe (NO
3)
39H
2O and 0.1mol FeSO
47H
2O dissolves in distilled water, obtains the 1L solution A; Measure 25% NH
4OH 90ml and 80% N
2H
4H
2O 50ml obtains solution B with distilled water diluting to 1L.Open constant flow pump, with solution A with B is isopyknic is pumped into simultaneously in the micro mixing device, control the flow of two solution at 0.4L/min, two kinds of solution have reached the even mixing of microscopic scale in the microenvironment of small container, form a large amount of nucleus in the reactant liquor; The reactant liquor that obtains enters in the crystal growth groove, and the ageing processing makes the crystal further growth in 80 ℃ of water-baths; The AC field frequency that feeds in the solenoid of micro mixing device and crystal growth groove is 500Hz, magnetic field intensity 0.5T; The reactant liquor product that the water-bath ageing obtained after 6 hours in the crystal growth groove filters all over the back with distilled water and ethanol washing 3-5,60 ℃ of oven dry in air dry oven, and the time is 24 hours.The Fe that obtains
3O
4The particle dispersiveness is fine, and diameter is about 20nm, as shown in Figure 5.
Coprecipitation prepares nano Co
0.5Ni
0.5Fe
2O
4The method of particle, step is as follows:
Take by weighing 0.02mol Fe (NO
3)
39H
2O, 0.005mol CoCl
26H
2O and 0.005mol NiCl
26H
2O dissolves in distilled water, obtains the 1L solution A; Measure 25% NH
3H
2O 20ml obtains solution B with distilled water diluting to 1L.Open constant flow pump, with solution A with B is isopyknic is pumped into simultaneously in the micro mixing device, control the flow of two solution at 0.2L/min, two kinds of solution have reached the even mixing of microscopic scale in the microenvironment of small container, form a large amount of nucleus in the reactant liquor; The reactant liquor that obtains enters in the crystal growth groove, and the ageing processing makes the crystal further growth in 90 ℃ of water-baths.The ac frequency that feeds in the solenoid of micro mixing device and crystal growth groove is 500Hz, magnetic field intensity 1T; The reactant liquor product that the water-bath ageing obtained after 8 hours in the crystal growth groove filters all over the back with distilled water and ethanol washing 3-5,60 ℃ of oven dry in air dry oven, and the time is 24 hours.The Co that obtains
0.5Ni
0.5Fe
2O
4The particle dispersiveness is fine, and diameter is about 30nm.
Coprecipitation prepares nanometer Zn
0.25Mn
0.25Ni
0.5Fe
2O
4The method of particle, step is as follows:
Take by weighing 0.02mol Fe (NO
3)
39H
2O, 0.005mol NiCl
26H
2O, 0.0025mol ZnCl
26H
2O and 0.0025mol MnCl
26H
2O dissolves in distilled water, obtains the 1L solution A; Get NaOH or KOH dissolve the 1L that obtains in the aqueous solution solution B, molar concentration is 0.01mol/L.Open constant flow pump, solution A and B equal-volume ground are pumped in the micro mixing device simultaneously, control the flow of two solution at 0.1L/min, two kinds of solution have reached the even mixing of microscopic scale in the microenvironment of small container, form a large amount of nucleus in the reactant liquor; The reactant liquor that obtains enters in the crystal growth groove, and the ageing processing makes the crystal further growth in 90 ℃ of water-baths.The ac frequency that feeds in the solenoid of micro mixing device and crystal growth groove is 500Hz, magnetic field intensity 1.5T; The reactant liquor product that the water-bath ageing obtained after 24 hours in the crystal growth groove filters all over the back with distilled water and ethanol washing 3-5,60 ℃ of oven dry in air dry oven, and the time is 24 hours.The magnetic particle dispersiveness that obtains is fine, and diameter is about 50nm.
Above content be in conjunction with concrete embodiment to further describing that the present invention does, can not assert that concrete enforcement of the present invention is confined to these explanations.For the general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, can also make some simple deduction or replace, all should be considered as belonging to protection scope of the present invention.
Claims (7)
1. little reaction system for preparing the ferrite nano powder, it is characterized in that: described little reaction system comprises feeding device, micro mixing device and crystal growth groove (4); Feeding device links to each other with the arrival end of micro mixing device, and the crystal growth groove links to each other with the port of export of micro mixing device; Described micro mixing device comprises that micro-mixer (3) and winding are at its outside solenoid (5).
2. little reaction system according to claim 1, it is characterized in that: the outside of described crystal growth groove (4) is arranged with solenoid.
3. little reaction system according to claim 1, it is characterized in that: described feeding device comprises reservoir (1) and constant flow pump (2), has at least two cover feeding devices to link to each other with micro mixing device in described little reaction system.
4. the method for a prepared by co-precipitation ferrite nano powder, it is characterized in that: described method is carried out at each described little reaction system of claim 1-3; Comprise reactant liquor is mixed in the micro mixing device that solenoid is passed to alternating current that form nucleus, the reactant liquor that will comprise described nucleus carries out water bath processing in crystal growth groove (4), the nucleus further growth obtains described ferrite nano powder; Described method specifically comprises the steps:
A. with water-soluble divalent metal salt and water-soluble trivalent ferric salt mixed dissolution in water, as reactant liquor A, aqueous slkali places the feeding device of little reaction system respectively as reactant liquor B;
B. the solenoid of micro mixing device feeds alternating current, and the reactant liquor in the feeding device is sent into micro mixing device simultaneously according to stoichiometric proportion;
C. form nucleus at micro mixing device, the reactant liquor that comprises described nucleus enters into the crystal growth groove; Feed alternating current to the solenoid of crystal growth groove, and the reactant liquor that will comprise described nucleus carries out water bath processing;
D. after handling through step c, the precipitated product that obtains in the crystal growth groove is washed, oven dry namely obtains described ferrite nano powder;
The frequency of alternating current is 50-2000Hz among described step b and the step c, and the magnetic field intensity of electromagnetic field is 0-1.5T;
The temperature of water bath processing is 40-95 ℃ among the described step c.
5. method according to claim 4, it is characterized in that: water-soluble divalent metal comprises Fe among the described step a
2+, Co
2+, Ni
2+, Zn
2+, Mn
2+In one or more.
6. method according to claim 4 is characterized in that: slaine comprises at least a in chlorate, nitrate, the sulfate among the described step a.
7. method according to claim 4, it is characterized in that: aqueous slkali comprises NaOH, KOH, NH among the described step a
4At least a among the OH.
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| CN103978228A (en) * | 2014-05-28 | 2014-08-13 | 天津大学 | Preparation method of nano manganese ferrite electromagnetic wave absorbing material |
| CN106348332B (en) * | 2016-11-21 | 2017-11-28 | 中国科学院上海高等研究院 | A kind of method and device that vaterite is prepared using dynamic magnetic agitating paddle |
| CN108623311B (en) * | 2018-07-05 | 2020-08-25 | 何莉 | Functional ceramic apparatus for producing |
| CN110156090B (en) * | 2019-06-28 | 2021-08-10 | 中国科学院合肥物质科学研究院 | For preparing Fe3O4Fluid synthesis preparation device of magnetic nanoparticles and control method thereof |
| CN113000851B (en) * | 2021-01-28 | 2023-04-18 | 南开大学 | Method for preparing superparamagnetic nano-iron with controllable particle size by using microchannel reactor |
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| CN1458118A (en) * | 2003-04-24 | 2003-11-26 | 哈尔滨工程大学 | Process for preparing nano permanent magnetic ferrite powder |
| CN101559985A (en) * | 2009-05-22 | 2009-10-21 | 华南理工大学 | Method for preparing Fe3O4 nano-particles by low-intensity external magnetic field induction and device thereof |
| CN101723655A (en) * | 2008-10-21 | 2010-06-09 | 兰州大学 | Preparation method of Mn-Zn ferrite cobalt-doped nano material |
| CN101830692A (en) * | 2010-03-31 | 2010-09-15 | 淮阴师范学院 | Synthetic method of magnetic zinc-ferrum oxide nano particles |
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| JPH0891942A (en) * | 1994-09-27 | 1996-04-09 | Tdk Corp | Production of powder for ferrite |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1458118A (en) * | 2003-04-24 | 2003-11-26 | 哈尔滨工程大学 | Process for preparing nano permanent magnetic ferrite powder |
| CN101723655A (en) * | 2008-10-21 | 2010-06-09 | 兰州大学 | Preparation method of Mn-Zn ferrite cobalt-doped nano material |
| CN101559985A (en) * | 2009-05-22 | 2009-10-21 | 华南理工大学 | Method for preparing Fe3O4 nano-particles by low-intensity external magnetic field induction and device thereof |
| CN101830692A (en) * | 2010-03-31 | 2010-09-15 | 淮阴师范学院 | Synthetic method of magnetic zinc-ferrum oxide nano particles |
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