CN101830516B - Method for preparing nano ferroferric oxide particles - Google Patents
Method for preparing nano ferroferric oxide particles Download PDFInfo
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- CN101830516B CN101830516B CN201010176187A CN201010176187A CN101830516B CN 101830516 B CN101830516 B CN 101830516B CN 201010176187 A CN201010176187 A CN 201010176187A CN 201010176187 A CN201010176187 A CN 201010176187A CN 101830516 B CN101830516 B CN 101830516B
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Abstract
The invention discloses a method for preparing nano ferroferric oxide particles, which comprises the following steps of: thoroughly mixing soluble Fe<2+> compound and Fe<3+> compound, and dissolving in distilled water; dissolving strong base in the distilled water, and adding a surface active agent; mixing the two solutions under the ultrasonic condition, and maintaining the reaction for 0.2-2 hours to obtain a suspending liquid; centrifugally separating the suspending liquid or filtering the suspensoid with filter paper, repeatedly washing with distilled water and absolute ethyl alcohol, and then drying to obtain the Fe3O4 nano particles. The invention has the characteristics of low reaction temperature, simple preparation process, extremely short production cycle, low cost, high product purity and small particle size. The obtained nano particles are Fe3O4 single-phase particles and are granular in shape and the diameter is smaller than 10nm on average.
Description
Technical field
The present invention relates to prepare the method for nano ferriferrous oxide granule.
Background technology
Along with continuous progress in science and technology, nanotechnology has obtained continuous development.Nano material more and more receives people's attention because it is different from the special performance of common bulk.The ferromagnetic substance of nanostructure such as as ferrofluid, advanced magneticsubstance, catalyzer raw material, high-density magnetic storage apparatus and aspects such as biomedicine and biopharmacy, has attracted the interest of Many researchers because it is used widely.
Fe
3O
4Have certain magnetic, can directed move under the outside magnetic field, particle diameter is little to have superparamagnetism within certain limit, can produce heat adding the alternating electromagnetic field effect under, and its chemical property is stablized, and its purposes is quite extensive.Nanometer Fe
3O
4As a kind of important ferromagnetic substance, obtained using widely, and be considered to the desirable equivalent material that the biology aspect is used at aspects such as electron device, message memory, MRI and medicine stripping technique.
Fe
3O
4The preparation method of nano particle mainly is divided into physics method and chemical method.The physics method generally adopts vacuum condensation method, physical pulverization method, mechanical ball milling method etc.But the general purity of product is low, size distribution is inhomogeneous, and is easy oxidized, is difficult to prepare the nano particle below the 10nm.Chemical method mainly comprises coprecipitation method, sol-gel method, microemulsion method, hydrothermal method etc.Fe with the chemical method acquisition
3O
4Though the nano particle quality is better, particle diameter is less, and operating procedure is also simple, and production cost is low, and the production cycle is longer.
Summary of the invention
It is simple to the purpose of this invention is to provide a kind of technology, and production cost is low, the method for preparing ferroferric oxide nano granules with short production cycle.
The method for preparing ferroferric oxide nano granules of the present invention may further comprise the steps:
1) stirs down, the Fe of solubility
2+Compound and Fe
3+The compound thorough mixing is dissolved in the zero(ppm) water, control mol ratio Fe
2+/ Fe
3+=0.5～2, total Fe ionic concn is 0.01～0.5mol/L in the mixing solutions;
2) stir down, highly basic is dissolved in the zero(ppm) water OH
-Concentration should make pH value of solution remain in 11～13 the scope, adds tensio-active agent then, and the molar weight of tensio-active agent is 5～10 times of step 1) Fe ion integral molar quantity, OH
-Molar weight be 1～3 times of step 1) Fe ion integral molar quantity;
3) ultrasonic probe is inserted step 2) solution in, in solution, dropwise drip the mixing solutions of step 1) simultaneously, at 20～80 ℃ of reaction 0.2～2h down, suspension liquid, the control ultrasonic power is at 80～240W, frequency is in 20～40KHz scope;
4) with the suspension liquid spinning or the filter paper filtering of step 3), behind zero(ppm) water and absolute ethyl alcohol repetitive scrubbing, drying gets Fe
3O
4Nano particle.
Among the present invention to the Fe of solubility
2+The Fe of compound and solubility
3+Compound does not have particular requirement, can obtain Fe as long as be dissolved in the water fully
2+And Fe
3+Compound all meet the requirements.The Fe of solubility
2+Compound can be FeSO
4Or FeCl
2, the Fe of solubility
3+Compound can be Fe
2(SO
4)
3, FeCl
3Or Fe (NO
3)
3
Above-mentioned highly basic can be selected a kind of or its mixture among NaOH, KOH and the LiOH.Tensio-active agent can select for use sodium-acetate, Vilaterm pyrrole to iron in alkane ketone, sodium oleate, polyoxyethylene glycol, ZX-I and the oleic acid any one or a few.
The present invention has the following advantages:
(1) making nano particle is Fe
3O
4Single-phase, purity is high.
(2) technology is simple, and production cost is low, and is with short production cycle.
(3) finished product pattern rule, particle size is below 10nm.
Description of drawings
The Fe of Fig. 1 embodiment 1
3O
4The TEM photo;
The Fe of Fig. 2 embodiment 2
3O
4The TEM photo
The Fe of Fig. 3 embodiment 3
3O
4The TEM photo.
Embodiment
Embodiment 1
1) stirs down, 0.7785g FeSO
47H
2O and 1.5138g FeCl
36H
2The O thorough mixing is dissolved in the 120mL zero(ppm) water, Fe
2+/ Fe
3+Mol ratio=1: 2;
2) stir down, 0.896g NaOH is dissolved in the 112mL zero(ppm) water OH
-Concentration makes pH value of solution remain on 13, adds 1.1461g Vilaterm pyrrole then and irons alkane ketone, and the molar weight that the Vilaterm pyrrole irons alkane ketone is 10 times of step 1) Fe ion integral molar quantity;
3) ultrasonic probe is inserted step 2) solution in, in solution, dropwise drip the mixing solutions of step 1), successive reaction 1.5h simultaneously; The model of ultrasonic generator is JY92-IIDN; Power is controlled at 80W, and frequency from motion tracking, gets suspension liquid in 20～25KHz scope;
4) suspension liquid of step 3) is used filter paper filtering, use zero(ppm) water and absolute ethyl alcohol repetitive scrubbing twice respectively, seasoning under the room temperature gets Fe
3O
4Nano particle.The particulate pattern is as shown in Figure 1, finished product pattern rule, and average diameter of particles is at 6.8nm.
Embodiment 2
1) stirs down, 1.1676gFeSO
47H
2O and 1.1353g Fe
2(SO
4)
39H
2The O thorough mixing is dissolved in the 120mL zero(ppm) water, Fe
2+/ Fe
3+Mol ratio=1: 1;
2) stir down, 0.84g NaOH is dissolved in the 105mL zero(ppm) water OH
-Concentration makes pH value of solution remain on 13, adds the 6.89g sodium-acetate then;
3) ultrasonic probe is inserted step 2) solution in, in solution, dropwise drip the mixing solutions of step 1), successive reaction 1h simultaneously; The model of ultrasonic generator is JY92-IIDN; Power is controlled at 80W, and frequency from motion tracking, gets suspension liquid in 20～25KHz scope;
4) suspension liquid of step 3) is used filter paper filtering, use zero(ppm) water and absolute ethyl alcohol repetitive scrubbing twice respectively, seasoning under the room temperature gets Fe
3O
4Nano particle.The particulate pattern is as shown in Figure 2, finished product pattern rule, and average diameter of particles is 9.2nm.
Embodiment 3
1) stirs down, 0.5567gFeCl
24H
2O and 1.5736g Fe
2(SO
4)
39H
2The O thorough mixing is dissolved in the 120mL zero(ppm) water, Fe
2+/ Fe
3+Mol ratio=1: 2;
2) stir down, 1.178g KOH is dissolved in the 105mL zero(ppm) water OH
-Concentration makes pH value of solution remain on 13, adds the 6.03g ZX-I then;
3) ultrasonic probe is inserted step 2) solution in, in solution, dropwise drip the mixing solutions of step 1), successive reaction 1h simultaneously; The model of ultrasonic generator is JY92-IIDN; Power is controlled at 100W, and frequency from motion tracking, gets suspension liquid in 20～25KHz scope;
4) suspension liquid of step 3) is used filter paper filtering, use zero(ppm) water and absolute ethyl alcohol repetitive scrubbing twice respectively, seasoning under the room temperature gets Fe
3O
4Nano particle.The particulate pattern is as shown in Figure 3, finished product pattern rule, average diameter of particles 7.7nm.
Claims (5)
1. method for preparing nano ferriferrous oxide granule may further comprise the steps:
1) stirs down, the Fe of solubility
2+Compound and Fe
3+The compound thorough mixing is dissolved in the zero(ppm) water, control mol ratio Fe
2+/ Fe
3+=0.5～2, total Fe ionic concn is 0.01～0.5mol/L in the mixing solutions;
2) stir down, highly basic is dissolved in the zero(ppm) water OH
-Concentration should make pH value of solution remain in 11～13 the scope, adds tensio-active agent then, and the molar weight of tensio-active agent is 5～10 times of step 1) Fe ion integral molar quantity, OH
-Molar weight be 1～3 times of step 1) Fe ion integral molar quantity;
3) ultrasonic probe is inserted step 2) solution in, in solution, dropwise drip the mixing solutions of step 1) simultaneously, at 20～80 ℃ of reaction 0.2～2h down, suspension liquid, the control ultrasonic power is at 80～240W, frequency is in 20～40KHz scope;
4) with the suspension liquid spinning or the filter paper filtering of step 3), behind zero(ppm) water and absolute ethyl alcohol repetitive scrubbing, drying gets Fe
3O
4Nano particle.
2. the method for preparing nano ferriferrous oxide granule according to claim 1 is characterized in that the Fe of solubility
2+Compound is FeSO
4Or FeCl
2
3. the method for preparing nano ferriferrous oxide granule according to claim 1 is characterized in that the Fe of solubility
3+Compound is Fe
2(SO
4)
3, FeCl
3Or Fe (NO
3)
3
4. the method for preparing nano ferriferrous oxide granule according to claim 1 is characterized in that a kind of or its mixture among highly basic selection NaOH, KOH and the LiOH.
5. the method for preparing nano ferriferrous oxide granule according to claim 1 is characterized in that tensio-active agent selects for use sodium-acetate, Vilaterm pyrrole to iron in alkane ketone, sodium oleate, polyoxyethylene glycol, ZX-I and the oleic acid any one or a few.
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|---|---|---|---|
| CN201010176187A CN101830516B (en) | 2010-05-18 | 2010-05-18 | Method for preparing nano ferroferric oxide particles |
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| CN201010176187A CN101830516B (en) | 2010-05-18 | 2010-05-18 | Method for preparing nano ferroferric oxide particles |
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| CN101830516B true CN101830516B (en) | 2012-10-03 |
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| CN102674477A (en) * | 2012-05-24 | 2012-09-19 | 西安建筑科技大学 | Method for co-production of superfine ferroferric oxide and aluminum oxide by red mud of Bayer process |
| CN102936050B (en) * | 2012-11-26 | 2014-08-27 | 江苏永凯化学有限公司 | Preparation method of ferroferric oxide nano sheet |
| NL2010439C2 (en) * | 2013-03-12 | 2014-09-24 | Ioniqa Technologies B V | Magnetic fluid. |
| CN103387267A (en) * | 2013-07-29 | 2013-11-13 | 宿迁学院 | Method for preparing nano ferroferric oxide |
| CN103638880B (en) * | 2013-12-20 | 2015-09-02 | 齐鲁工业大学 | A kind of preparation method of porous magnetic microballoon |
| CN103862037B (en) * | 2014-02-27 | 2015-10-28 | 浙江大学 | The preparation of biomaterial embedding Zero-valent Iron-tri-iron tetroxide double nano system and pre-treatment way |
| CN103866605A (en) * | 2014-02-28 | 2014-06-18 | 苏州恒康新材料有限公司 | Magnetic composition and preparation method thereof |
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| CN108893816A (en) * | 2018-07-17 | 2018-11-27 | 佛山市南海区佳妍内衣有限公司 | A kind of scribbled with anti-static function |
| CN109675065A (en) * | 2018-12-20 | 2019-04-26 | 上海交通大学 | Nanometer magnetic bead and preparation method thereof for T1 and T2 magnetic resonance bimodal radiography |
| CN110255627A (en) * | 2019-07-12 | 2019-09-20 | 中国恩菲工程技术有限公司 | Nano ferriferrous oxide and preparation method thereof and system |
| CN111268742A (en) * | 2020-02-12 | 2020-06-12 | 西安工程大学 | Preparation method of ferroferric oxide quantum dots |
| CN113247959A (en) * | 2021-06-09 | 2021-08-13 | 东北大学 | Method for preparing functional iron oxide nanoparticles by using machine head ash as raw material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101445277A (en) * | 2008-11-14 | 2009-06-03 | 东北大学 | Nano-crystalline Fe*O* particles with high absorption capacity and preparation method thereof |
-
2010
- 2010-05-18 CN CN201010176187A patent/CN101830516B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101445277A (en) * | 2008-11-14 | 2009-06-03 | 东北大学 | Nano-crystalline Fe*O* particles with high absorption capacity and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| Young Soo Kang et al..Synthesis and Characterization of Nanometer-Size Fe3O4 and γ-Fe2O3 Particles.《Chem. Mater.》.1996,第8卷(第9期),2209-2211. * |
| 姚素薇 等.超声共沉淀法制备强磁性纳米Fe3O4颗粒.《2005年上海市电镀与表面精饰学术年会论文集》.2005,258-261. * |
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