CN101049977A - Method for preparing Nano Fe2O3 - Google Patents
Method for preparing Nano Fe2O3 Download PDFInfo
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- CN101049977A CN101049977A CN 200710061882 CN200710061882A CN101049977A CN 101049977 A CN101049977 A CN 101049977A CN 200710061882 CN200710061882 CN 200710061882 CN 200710061882 A CN200710061882 A CN 200710061882A CN 101049977 A CN101049977 A CN 101049977A
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- iron salt
- concentration
- divalent iron
- nanometer
- fe3o4
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Abstract
This invention discloses a method for preparing uniform nanoscale Fe3O4. The method comprises: adjusting the pH value of ferrous salt solution to 9-11 with NaOH, adding trace amount of complexone, and oxidizing in air under the induction of visible light to obtain spherical Fe3O4 nanopowder. The particle sizes of the Fe3O4 nanopowder are 10-50 nm, and can be artificially controlled. The Fe3O4 nanopowder has such advantages as uniform particle size distribution, good dispersibility, high purity and high yield. The method is simple and economic.
Description
Technical field
The present invention relates to a kind of nanometer Fe
3O
4Preparation method, particularly a kind of preparing uniform nanoscale Fe
3O
4Method.
Background technology
Nanometer Fe
3O
4Have excellent properties at aspects such as magnetic, catalysis, biologies, not only show the using value make new advances but also become again the important component part of magnetic liquid, magnetic micro-beads, the new material such as magnetic and medicated in traditional field.Since the dimensional effect of nano particle, the Fe of different size
3O
4Magnetic nanoparticle usually shows different magnetic characteristics.But Fe
3O
4Very easily reuniting in generative process has affected its application, thereby prepares the controlled nanometer Fe of single fineness of dispersion
3O
4Powder becomes the research emphasis of various countries.S.H.Sun etc. are by thermal decomposition [Fe (acac)
3] in the presence of acetylacetone,2,4-pentanedione, oleyl amine etc., obtain preferably nanometer Fe of high-quality decentralized
3O
4(J.Am.Chem.Soc.2004,126,273-279); Zhen Li etc. are with FeCl
3.6H
2O places pyrrolidones boiling reflux different time to obtain particle diameter at single Fe of dispersion of 4-60nm
3O
4(Angew.Chem.Int.Ed.2005,44,123-126); Sun Kang etc. are with FeCl
3.6H
2O and FeCl
2.4H
2O is dissolved in the non-polar organic solvent, makes 10nm left and right sides superparamagnetic Fe
3O
4Powder (ZL200510111014.1); Simultaneously, Shufeng Si etc. is with FeCl
3.6H
2O and Fe powder are predecessor, in the presence of oleic acid and laurylamide, through 180 ℃ of Hydrothermal Synthesis different times, obtain particle diameter at the single Fe of dispersion of 5.2-12.7nm with hydro-thermal method
3O
4Powder; The bear letter is brave to be waited by control galvanic cell electromotive force control trivalent iron salt and divalent iron salt concentration ratio, makes the Fe that particle diameter is 2-20nm
3O
4Powder (ZL200310103713.2); The usefulness ferrous salt such as Ren Jicun and molysite are raw material, adopt microwave reaction, obtain 3-40nm Fe
3O
4, its saturation magnetization is 70～120emu/g (ZL200610025662.X).In addition, in aqueous slkali with a certain proportion of FeCl
3.6H
2O and FeCl
2.H
2O is raw material, at logical N
2Atmosphere under to nanometer Fe
3O
4Preparation also carried out a large amount of research.Such as: the D.K.Kim. coprecipitation, obtaining granularity through the enuatrol surface treatment is 13-60nm, and the nanometer Fe of different magnetic characteristics is arranged
3O
4(J.Magnetism Magnetic Mater.2001,225,30-36); The coprecipitation such as An Lijuan, and be that double-layer surface-active agent carries out finishing with oleic acid and neopelex, having made particle diameter is the stable water dispersible nanometer Fe of 10nm
3O
4(SCI, 2005,26 (2), 366-369); Wang Hanbin etc. also adopt coprecipitation, add citrate and control nanometer Fe
3O
4Growth, prepare particle diameter less than the Fe of 5nm
3O
4Particle, but the crystallization of sample not ideal (Chinese Journal of Inorganic Chemistry, 2004,20 (11), 1279-1283); But with Fe
2+Be raw material, add alkali control pH value, the Fe that obtains with air oxidation
3O
4Particle diameter is generally bigger, does not still have particle diameter less than the report of 20nm at present, and uniformity is not good enough.In recent years, although at Fe
3O
4Fabrication and modification aspect make significant progress, but still have two typical problems: the raw material of (1) preparation is more expensive, and cost is higher, and relative preparation technology is complicated; (2) to nanometer Fe
3O
4The surface modify the grain size that can reduce sample, and improve the dispersiveness of sample, but can cause thus nanometer Fe
3O
4The decline of magnetic property.Therefore, seek new reaction process, low cost is synthesized the nanometer Fe that even particle size distribution is controlled, have good dispersion
3O
4Powder has important practical significance.
Summary of the invention
The purpose of this invention is to provide a kind of efficient, economic, simple and convenient, low-cost prepared sizes and be evenly distributed controlledly, have good dispersion and inhomogeneity nanometer Fe
3O
4Method.
The present invention gives the preparation nanometer Fe
3O
4Different-grain diameter and improve its dispersed condition, and the concentration of reactant and additive is provided.
The object of the present invention is achieved like this.A kind ofly prepare that to have even particle size distribution controlled, the nanometer Fe that monodispersity is good
3O
4Method, divalent iron salt solution added alkali after, add again complexones, under radiation of visible light, air oxidation, 20～50 ℃ of control reaction temperatures, light intensity 0～80000lux, 1～5 hour reaction time, reaction makes product separate with mother liquor after finishing after filtration, washs with distilled water again, oven dry obtains Fe
3O
4Powder;
Among the present invention, the concentration of divalent iron salt solution is in 0.1～1.0mol/L scope, and divalent iron salt solution is 1 with the mol ratio of mixing of complexone: (0.003～0.03).
The present invention by control reaction time and temperature can Quality control granule size.Reaction is carried out in reactor, does not have adding and the taking-up of species between the stage of reaction.
Among the present invention, described complexone is wherein a kind of of ethylenediamine-N,N'-diacetic acid(EDDA) (EDTA), ethylene glycol diethyl ether ethylenediamine tetraacetic acid (EDTA) (EGTA), nitrilotriacetic acid(NTA) (NTA), quadrol (EDA).
In the present invention, adding NaOH solution control reacting solution pH value is 9～11; Can be by in reaction solution, adding the dispersiveness of tensio-active agent control sample.
The Fe of the present invention's preparation
3O
4Powder is ball-type, and particle diameter can be regulated and control at 10～50nm, and monodispersity is good; Fe
3O
4Saturation magnetization at 50～90emu/g; Fe
3O
4Yield and purity are more than 98%.
The good effect that the present invention obtains is: the present invention is take the ferrous salt that is easy to get as raw material, and complexones is made derivant, and it is controlled to prepare granularity, has good dispersed and inhomogeneity nanometer Fe
3O
4Powder, technology is simple, and is economical and practical, is the Fe of industrial production high-purity, high yield
3O
4Production method and operating condition are provided.
Embodiment
Following examples are used to illustrate the present invention.
Embodiment 1
Adding 30ml concentration in the reactor is the FeSO of 1mol/L
4, adding concentration is that the NaOH solution of 6mol/L makes pH=11, adding 2ml concentration is the EDTA of 0.05mol/L, with ordinary lamps irradiation (illumination 12000Lux), passes into air (air mass flow 0.132m
3/ h) oxidation, the control reaction temperature is 30 ℃, and sustained response 1.5h filters earlier after reaction finishes, and with the distilled water washing for several times, obtains product 2.31g again, and product cut size is about 20nm.
Embodiment 2
Adding 30ml concentration in the reactor is the FeSO of 1mol/L
4, adding concentration is that the NaOH solution of 6mol/L makes pH value=10, adding 2ml concentration is the EDTA of 0.05mol/L, with ordinary lamps irradiation (illumination 12000Lux), passes into air (air mass flow 0.132m
3/ h) oxidation, the control reaction temperature is 50 ℃, sustained response 1.2h filters earlier after reaction finishes, and with the distilled water washing for several times, obtains product F e again
3O
4Particle diameter is about 40nm, and its saturation magnetization is 70emu/g.
Embodiment 3
Adding 30ml concentration in the reactor is the FeSO of 1mol/L, adding concentration is that the NaOH solution of 6mol/L makes pH value=11, adding 2ml concentration is the EDTA of 0.05mol/L, adding 10ml concentration is the dodecyl sodium sulfate surfactant of 0.01mol/L, with ordinary lamps irradiation (illumination 12000Lux), drum air (air mass flow 0.132m
3/ h), the control reaction temperature is 30 ℃, and sustained response 1.5h filters earlier after reaction finishes, and with the distilled water washing for several times, obtains product 2.31g again, and the uniformity of product is better, and particle diameter is about 16nm.
Embodiment 4
Adding 30ml concentration in the reactor is the FeSO of 1mol/L
4Adding concentration is that the NaOH solution of 6mol/L makes pH=11, and adding 2ml concentration is the EDTA of 0.05mol/L, and adding 10ml concentration is the dodecyl sodium sulfate surfactant of 0.01mol/L, with ordinary lamps irradiation (illumination 80000Lux), drum air (air mass flow 0.132m
3/ h), the control reaction temperature is 30 ℃, sustained response 1.5h filters earlier after reaction finishes, and again with the distilled water washing for several times, obtains single Fe of dispersion
3O
4The particle diameter of product is about 13nm, and its saturation magnetization is 52emu/g.
Embodiment 5
Adding 30ml concentration in the reactor is the FeCl of 1mol/L
2Adding concentration is that the NaOH of 6mol/L makes pH value=11, and adding 2ml concentration is the EDTA of 0.05mol/L, and adding 10ml concentration is the dodecyl sodium sulfate surfactant of 0.01mol/L, with ordinary lamps irradiation (illumination 12000Lux), drum air (air mass flow 0.132m
3/ h), the control reaction temperature is 20 ℃, sustained response 1.5h filters earlier after reaction finishes, and again with the distilled water washing for several times, obtains single Fe of dispersion
3O
4The particle diameter of product is about 13nm.
Claims (3)
1, a kind of nanometer Fe
3O
4The preparation method, it is characterized in that: after divalent iron salt solution is added alkali, add again complexones, under radiation of visible light, air oxidation, 20～50 ℃ of control reaction temperatures, light intensity 0～80000lux, 1～5 hour reaction time, reaction makes product separate with mother liquor after finishing after filtration, washs with distilled water, oven dry obtains Fe
3O
4Powder;
Wherein, the concentration of divalent iron salt solution is in 0.1～1.0mol/L scope, and divalent iron salt solution is 1 with the mol ratio of mixing of complexone: (0.003～0.03).
2, by the described preparation method of claim 1, it is characterized in that: said divalent iron salt is ferrous sulfate or iron protochloride, and complexone is EDTA, wherein a kind of of EGTA, NTA, quadrol.
3, by the described preparation method of claim 1, it is characterized in that: it is NaOH solution that institute adds alkali, and the control reacting solution pH value is 9～11.
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|---|---|---|---|
| CN 200710061882 CN101049977A (en) | 2007-05-15 | 2007-05-15 | Method for preparing Nano Fe2O3 |
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|---|---|---|---|
| CN 200710061882 CN101049977A (en) | 2007-05-15 | 2007-05-15 | Method for preparing Nano Fe2O3 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104511270A (en) * | 2013-10-07 | 2015-04-15 | 财团法人工业技术研究院 | Ferrite adsorption material for adsorbing rare earth elements and adsorption method thereof |
| CN107804877A (en) * | 2017-11-17 | 2018-03-16 | 山西农业大学 | A kind of preparation method of magnetic Nano material |
| CN108238645A (en) * | 2016-12-26 | 2018-07-03 | 惠州市华阳光学技术有限公司 | A kind of preparation method of paramagnetic nanoparticles particle |
| CN110026195A (en) * | 2019-05-05 | 2019-07-19 | 河北师范大学 | A kind of high activity α-Fe2O3Nanometer sheet and its preparation method and application |
| CN110064395A (en) * | 2019-01-29 | 2019-07-30 | 吉林师范大学 | A kind of preparation method for the visible light catalyst having Magnetic Isolation function |
| CN110451579A (en) * | 2019-08-20 | 2019-11-15 | 临沂大学 | A kind of dispersion Fe2O3Preparation method |
| 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 |
-
2007
- 2007-05-15 CN CN 200710061882 patent/CN101049977A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104511270A (en) * | 2013-10-07 | 2015-04-15 | 财团法人工业技术研究院 | Ferrite adsorption material for adsorbing rare earth elements and adsorption method thereof |
| CN108238645A (en) * | 2016-12-26 | 2018-07-03 | 惠州市华阳光学技术有限公司 | A kind of preparation method of paramagnetic nanoparticles particle |
| CN107804877A (en) * | 2017-11-17 | 2018-03-16 | 山西农业大学 | A kind of preparation method of magnetic Nano material |
| CN110064395A (en) * | 2019-01-29 | 2019-07-30 | 吉林师范大学 | A kind of preparation method for the visible light catalyst having Magnetic Isolation function |
| CN110026195A (en) * | 2019-05-05 | 2019-07-19 | 河北师范大学 | A kind of high activity α-Fe2O3Nanometer sheet and its preparation method and application |
| CN110026195B (en) * | 2019-05-05 | 2021-09-03 | 河北师范大学 | High-activity alpha-Fe2O3Nanosheet and preparation method and application thereof |
| CN110451579A (en) * | 2019-08-20 | 2019-11-15 | 临沂大学 | A kind of dispersion Fe2O3Preparation method |
| 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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Open date: 20071010 |