CN108910961A - A kind of preparation method of ferroso-ferric oxide - Google Patents

A kind of preparation method of ferroso-ferric oxide Download PDF

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Publication number
CN108910961A
CN108910961A CN201811021160.9A CN201811021160A CN108910961A CN 108910961 A CN108910961 A CN 108910961A CN 201811021160 A CN201811021160 A CN 201811021160A CN 108910961 A CN108910961 A CN 108910961A
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iron salt
ferroso
ferric
ferric oxide
preparation
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不公告发明人
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • C01G49/02Oxides; Hydroxides
    • C01G49/08Ferroso-ferric oxide [Fe3O4]
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/62Submicrometer sized, i.e. from 0.1-1 micrometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/64Nanometer sized, i.e. from 1-100 nanometer
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/54Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Hard Magnetic Materials (AREA)

Abstract

The invention discloses a kind of preparation methods of ferroso-ferric oxide, this method is using ionic liquid as reaction dissolvent, pass through coprecipitation, nano-scale magnetic ferroso-ferric oxide is prepared, soluble divalent iron salt and soluble trivalent iron salt are added in ionic liquid and obtain solution, then it is slow added into sodium hydroxide and insulation reaction, reaction mixture is centrifugated, washs, is dried to obtain nano-scale magnetic ferroso-ferric oxide.The present invention utilizes the special nature of ionic liquid, replace the aqueous solvent in traditional co-precipitation method, conveniently prepare nanoscale magnetic ferroferric oxide particle, particle diameter distribution is uniform, and spherical shape is good, and magnetic property is excellent, and preparation method is simple, equipment requirement is low, is suitable for producing in enormous quantities, is a kind of preparation method with bright prospects.

Description

A kind of preparation method of ferroso-ferric oxide
Technical field
The present invention relates to the preparation methods of magnetic material, more particularly, to a kind of preparation method of ferroso-ferric oxide.
Background technique
Nano magnetic material is as a kind of emerging functional material, due to its unique physicochemical properties, make its physics, Chemistry etc. shows the specific use different from conventional magnetic material.Nano ferriferrous oxide is exactly one of multi-functional Magnetic material, magnetic recording material, magnetic fluid, catalysis, medicine, in terms of have a wide range of applications.
Ferroso-ferric oxide(ferroferric oxide), chemical formula Fe3O4, it is commonly called as iron oxide black, magnet, magnet, black Iron oxide, belongs to cubic system, and inverse spinel structure has excellent Magnetics characteristL, therefore also referred to as magnetic iron oxide.
The principal element for influencing nanoscale ferroso-ferric oxide performance includes superparamagnetism, coercivity, magnetic saturation amount, crystallinity And partial size and pattern etc..The preparation method of ferroferric oxide nano granules has huge shadow to its performance and suitable application area It rings.Method currently used for preparing nano ferriferrous oxide particle mainly has physical method and chemical method.Wherein, physical method The nano ferriferrous oxide purity of preparation is low, particle diameter distribution is uneven, so its application range of products is relatively narrow.Chemical method obtains Product run-of-the-mill it is preferable, operating method is also relatively easy to, thus obtain extensively research and concern;But its also have it is unfavorable On one side, it as reaction principle is typically more complicated, is not easy accurately to control its pattern and performance.
At present be used to prepare nano ferriferrous oxide chemical method mainly have coprecipitation, hydro-thermal method or solvent-thermal method, Microemulsion method, sol-gel method etc..Different methods, reaction principle, consersion unit and reaction condition have very big difference, The pattern and property of product are also not quite similar.
Ionic liquid, that is, the liquid being composed entirely of ions, since it is low with fusing point, electric conductivity is strong, dissolubility is high etc. Characteristic not available for many usual vehicles, thus be a hot fields of Recent study, it is sent out in compound synthesis field Wave important function.
Ionic liquid is generally made of organic cation and big inorganic anion, common cation have quaternary ammonium salt from Son, quaternary phosphine salt ion, imidazolium ion and pyrroles's salt ion etc., anion has halide ion, tetrafluoroborate ion, hexafluoro phosphorus Acid ion etc..
Summary of the invention
It is reaction dissolvent, the excellent nano-magnetic of processability that the purpose of the present invention is to provide a kind of using ionic liquid The method of ferroso-ferric oxide.
Technical scheme is as follows:
Using ionic liquid as reaction dissolvent, by coprecipitation, nanoscale is prepared in a kind of preparation method of ferroso-ferric oxide Magnetic ferroferric oxide;Described method includes following steps:
(1)Analytically pure soluble divalent iron salt and soluble trivalent iron salt are taken, according to molar ratio Fe2+:Fe3+=1:2~2:3 claim Measure divalent iron salt and trivalent iron salt;
(2)Divalent iron salt and trivalent iron salt are added separately in ionic liquid to and are stirred 10 ~ 20min, it is molten to obtain divalent iron salt The concentration of liquid and ferric salt solution, the divalent iron salt solution and ferric salt solution is 0.3 ~ 0.6mol/L;
(3)Divalent iron salt solution and ferric salt solution are uniformly mixed under agitation, while with heating water bath and being kept the temperature At 30 ~ 40 DEG C, then proceed to be slowly added to powdered analysis pure cerium hydroxide sodium under agitation, after adding keep the temperature 30min ~ 2h;
(4)It is centrifugated reaction mixture, by isolated product with heptane wash 2 ~ 3 times, then is washed with deionized 2 ~ 3 It is secondary, it is dried at 40 ~ 60 DEG C to get nano-scale magnetic ferroso-ferric oxide is arrived.
Wherein, the divalent iron salt is one of frerrous chloride, ferrous nitrate, ferrous sulfate or a variety of, the trivalent Molysite is one of iron chloride, ferric nitrate, ferric sulfate or a variety of.
Further, the ionic liquid is [Bmim] BF4
Further, step(3)In, the additional amount of the sodium hydroxide is 0.5-1 relative to the mole of divalent iron salt Times, it is described to be slowly added to be to be added to complete in 10-30min.
Ionic liquid is a kind of solvent of green high-efficient, plays important role in synthesis chemistry, synthesis is each extensively Kind organic substance, but the research for synthesizing inorganic compound with it so far is still less.The present invention is special using ionic liquid Property replaces the aqueous solvent in traditional co-precipitation method, conveniently prepares nanoscale magnetic ferroferric oxide particle, grain Diameter is evenly distributed, and spherical shape is good, by Magnetic Test, has preferable coercivity and magnetic saturation amount, and preparation method is simple, Equipment requirement is low, is suitable for producing in enormous quantities, is a kind of preparation method with bright prospects.
Specific embodiment
The following are a specific embodiment of the invention, the present invention to be explained and illustrated.
Embodiment 1
A kind of preparation method of ferroso-ferric oxide, preparation method include the following steps:
(1)Analytically pure frerrous chloride and iron chloride are taken, frerrous chloride 0.5mol, iron chloride 1mol are weighed;
(2)Frerrous chloride and iron chloride are added separately to [Bmim] BF4In and stir 10min, obtain solution of ferrous chloride and Ferric chloride solution, concentration are 0.6mol/L;
(3)Solution of ferrous chloride and ferric chloride solution are uniformly mixed under agitation, while with heating water bath and being kept the temperature It 30 DEG C, then proceedes to be slowly added to powdered analysis pure cerium hydroxide sodium 0.5mol in 20min under agitation, be kept the temperature after adding 2h;
(4)It is centrifugated reaction mixture, by isolated product with heptane wash 3 times, then is washed with deionized 3 times, It is dried at 40 DEG C to get nano-scale magnetic ferroso-ferric oxide is arrived.
It is detected through SEM, obtained ferroso-ferric oxide partial size is between 60-150nm.
Embodiment 2
A kind of preparation method of ferroso-ferric oxide, described method includes following steps:
(1)Analytically pure frerrous chloride, ferrous sulfate and ferric nitrate are taken, according to molar ratio Fe2+:Fe3+=2:3 weigh protochloride Iron, ferrous sulfate and ferric nitrate;
(2)Frerrous chloride, ferrous sulfate and ferric nitrate are added separately to ionic liquid [Bmim] BF4In and stir 10 ~ 20min, obtains divalent iron salt solution and ferric salt solution, and the concentration of the divalent iron salt solution and ferric salt solution is 0.3mol/L;
(3)Divalent iron salt solution and ferric salt solution are uniformly mixed under agitation, while with heating water bath and being kept the temperature At 40 DEG C, then proceed to be slowly added in 30min under agitation powdered analysis pure cerium hydroxide sodium to pH be about 8.5(Hydrogen The additional amount of sodium oxide molybdena is frerrous chloride, 0.7 times of ferrous sulfate integral molar quantity), and keep the temperature 1h;
(4)It is centrifugated reaction mixture, by isolated product with heptane wash 2 times, then is washed with deionized 2 times, It is dried at 60 DEG C to get nano-scale magnetic ferroso-ferric oxide is arrived.

Claims (4)

1. a kind of preparation method of ferroso-ferric oxide, which is characterized in that using ionic liquid as reaction dissolvent, by coprecipitation, Nano-scale magnetic ferroso-ferric oxide is prepared;Described method includes following steps:
(1)Analytically pure soluble divalent iron salt and soluble trivalent iron salt are taken, according to molar ratio Fe2+:Fe3+=1:2~2:3 weigh Divalent iron salt and trivalent iron salt;
(2)Divalent iron salt and trivalent iron salt are added separately in ionic liquid to and are stirred 10 ~ 20min, it is molten to obtain divalent iron salt The concentration of liquid and ferric salt solution, the divalent iron salt solution and ferric salt solution is 0.3 ~ 0.6mol/L;
(3)Divalent iron salt solution and ferric salt solution are uniformly mixed under agitation, while with heating water bath and being kept the temperature At 30 ~ 40 DEG C, then proceed to be slowly added to powdered analysis pure cerium hydroxide sodium under agitation, after adding keep the temperature 30min ~ 2h;
(4)It is centrifugated reaction mixture, by isolated product with heptane wash 2 ~ 3 times, then is washed with deionized 2 ~ 3 It is secondary, it is dried at 40 ~ 60 DEG C to get nano-scale magnetic ferroso-ferric oxide is arrived.
2. a kind of preparation method of ferroso-ferric oxide according to claim 1, which is characterized in that the divalent iron salt is chlorine Change one of ferrous iron, ferrous nitrate, ferrous sulfate or a variety of, the trivalent iron salt is iron chloride, in ferric nitrate, ferric sulfate It is one or more.
3. a kind of preparation method of ferroso-ferric oxide according to claim 1, which is characterized in that the ionic liquid is [Bmim]BF4
4. a kind of preparation method of ferroso-ferric oxide according to claim 1, which is characterized in that step(3)In, the hydrogen The additional amount of sodium oxide molybdena is 0.5-1 times relative to the mole of divalent iron salt, described be slowly added to be added in 10-30min It completes.
CN201811021160.9A 2018-09-03 2018-09-03 A kind of preparation method of ferroso-ferric oxide Pending CN108910961A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109806844A (en) * 2019-03-21 2019-05-28 西南大学 A kind of magnetic metal organic framework materials of dephosphorization and preparation method thereof
CN110508284A (en) * 2019-08-30 2019-11-29 中南大学 A kind of preparation method of two dimension ferroso-ferric oxide class fenton catalyst and its application in wastewater degradation containing aminobenzenesulfonic acid
CN113041996A (en) * 2021-03-05 2021-06-29 福州海关技术中心 Preparation method and application of magnetic graphitized carbon black
CN115818724A (en) * 2022-12-16 2023-03-21 上海允复纳米科技有限公司 Nanoscale gamma-phase magnetic ferric oxide and preparation process and application thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101162634A (en) * 2007-09-20 2008-04-16 华东师范大学 Ion liquid based magnetofluid preparation method
CN103449534A (en) * 2013-08-06 2013-12-18 陕西科技大学 Method for preparing magnetic nanoparticle by using ionic liquid as template agent
CN104030363A (en) * 2014-02-17 2014-09-10 瑞安市浙工大技术转移中心 Preparing method of ferroferric oxide nanometer particles
CN104386760A (en) * 2014-10-31 2015-03-04 山东师范大学 Method for rapidly preparing magnetic carrier material in large quantity

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101162634A (en) * 2007-09-20 2008-04-16 华东师范大学 Ion liquid based magnetofluid preparation method
CN103449534A (en) * 2013-08-06 2013-12-18 陕西科技大学 Method for preparing magnetic nanoparticle by using ionic liquid as template agent
CN104030363A (en) * 2014-02-17 2014-09-10 瑞安市浙工大技术转移中心 Preparing method of ferroferric oxide nanometer particles
CN104386760A (en) * 2014-10-31 2015-03-04 山东师范大学 Method for rapidly preparing magnetic carrier material in large quantity

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109806844A (en) * 2019-03-21 2019-05-28 西南大学 A kind of magnetic metal organic framework materials of dephosphorization and preparation method thereof
CN110508284A (en) * 2019-08-30 2019-11-29 中南大学 A kind of preparation method of two dimension ferroso-ferric oxide class fenton catalyst and its application in wastewater degradation containing aminobenzenesulfonic acid
CN113041996A (en) * 2021-03-05 2021-06-29 福州海关技术中心 Preparation method and application of magnetic graphitized carbon black
CN115818724A (en) * 2022-12-16 2023-03-21 上海允复纳米科技有限公司 Nanoscale gamma-phase magnetic ferric oxide and preparation process and application thereof

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