CN101003386A - Method for preparing Nano microparticles of monodisperse, oil soluble, surface modified iron oxide - Google Patents
Method for preparing Nano microparticles of monodisperse, oil soluble, surface modified iron oxide Download PDFInfo
- Publication number
- CN101003386A CN101003386A CN 200610107323 CN200610107323A CN101003386A CN 101003386 A CN101003386 A CN 101003386A CN 200610107323 CN200610107323 CN 200610107323 CN 200610107323 A CN200610107323 A CN 200610107323A CN 101003386 A CN101003386 A CN 101003386A
- Authority
- CN
- China
- Prior art keywords
- ferric
- soluble
- fatty acid
- salt
- concentration
- 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.)
- Granted
Links
Images
Landscapes
- Compounds Of Iron (AREA)
Abstract
This invention discloses a method for preparing monodisperse oil-soluble surface-modified ferric oxide nanoparticles. The method comprises: mixing ethanol solution of soluble ferric salt with ethanol solution of fatty acid, adding alkali, stirring to obtain precursor of ferric oxyhydrogen fatty acid salt precipitate, and cracking at 210-280 deg.C without solvent to obtain the target product. The soluble ferric salt is ferric nitrate, ferric chloride or ferric sulfate. The fatty acid is one or more of C6-22 saturated or unsaturated fatty acids. The alkali is NaOH, KOH or concentrated ammonia solution. The mol ratio of fatty acid to soluble ferric salt is (1-3):1. The concentration of ethanol solution of fatty acid is 0.01-1 mol/L. The concentration of ethanol solution of soluble ferric salt is 0.2 mol/L (saturation concentration). The method has such advantages as simple process, simple equipment, low raw material cost and high yield. The obtained ferric oxide nanoparticles can be stably dispersed in organic solvents.
Description
Technical field
The invention belongs to new function nano material preparation technical field, particularly a kind of solvent-free pyrolysis prepares the method for single dispersion, oil soluble, surface modified iron oxide nanoparticle.
Background technology
Nano-sized iron oxide is owing to using and to be subjected to extensive and deep research having potential aspect magnetics, pigment and the biological medicine.γ-Fe particularly
2O
3, Fe
3O
4The research of nanoparticle is maximum, has developed the method that is prepared as follows high quality, monodispersed ferric oxide nano crystallite: 1) the direct pyrolysis presoma of solvent-thermal method (FeCup
3, Fe (acac)
3, Fe (ac)
3); 2) solvent-thermal method pyrolysis Fe (CO)
5, utilize (CH again
3)
3The NO selective oxidation can prepare the ferric oxide nano particulate of different oxidation state.These methods all are to adopt the organic solvent that contains modifier at high temperature to react, and be recycled very difficult solvent is separated in the last handling process, and environmental pollution is serious.In recent years, to prepare nano material be one of target of pursuing of investigator to development greenization, eco-friendly method.After Travis H.L. group reported that solvent-free pyrolysis thiol derivative presoma prepares the cuprous sulfide nanometer rod, this group utilized this method to prepare cuprous sulfide nanometer sheet, nanometer nickel sulfide rod, triangular nano dish, bismuth trisulfide nanometer rod band etc. in succession.Ling chen group has prepared cuprous sulfide nano wire, silver sulfide nanometer plate and silver-colored nanometer plate with metal-sulfur alkoxide polymer presoma on this basis.The presoma of the preparation metallic sulfide of being reported contains the modifier octylate.Generally speaking, no-solvent process has reduced pollution to a great extent demonstrating special advantages aspect preparation, size and the morphology control of nano metal sulfide material, is a kind of eco-friendly method for preparing nano material.
Summary of the invention
The object of the invention is to provide a kind of solvent-free pyrolysis to prepare the method for single dispersion, oil soluble, surface modified iron oxide nanoparticle.
The present invention realizes by following technical solution: a kind of method for preparing single dispersion, oil soluble, surface modified iron oxide nanoparticle, the ethanolic soln of soluble ferric iron salt is mixed with the ethanolic soln of lipid acid, add alkali and stir to such an extent that presoma ferric iron hydrogen-oxygen soap precipitates; Unit presoma ferric iron hydrogen-oxygen soap solves target product in solvent-free direct heat down.
Described soluble ferric iron salt is iron nitrate, iron(ic) chloride or ferric sulfate, and described lipid acid is that carbon chain lengths is one or more combination of 6～22 saturated fatty acid or unsaturated fatty acids, and described alkali is sodium hydroxide, potassium hydroxide or strong aqua.
The mol ratio of described lipid acid and soluble ferric iron salt is 1-3; The concentration 0.01-1mol/L of fatty acid ethanolamide solution, the concentration of soluble ferric iron salt ethanolic soln is the 0.2mol/L-saturation concentration; Pyrolysis temperature 210-280 ℃.
In the invention process process, earlier lipid acid is dissolved in ethanol, at room temperature the ethanolic soln that is dissolved with soluble ferric iron salt is added above-mentioned solution stirring 5min then, add alkaline solution more rapidly and produce a large amount of pale brown look precipitations.Through filtration under diminished pressure, washing, drying, get pale brown toner end and be precursor.Get presoma and place retort furnace in airtight tetrafluoroethylene reactor, decomposition obtains powder and is target product-iron oxide modified surface nanoparticle between 210-280 ℃.The present invention adopts the unit precursor to decompose in an organic solvent condition direct heat not, directly modifies at nano-particle surface when forming nanoparticle.
Technology of the present invention, equipment are simple, and raw material is cheap and easy to get, and cost is low, and the productive rate height is fit to large-scale industrial production.Prepared ferric oxide nano diameter of particle homogeneous can change the particle diameter and the pattern of nanoparticle by the carbon chain lengths that changes lipid acid, regulates the crystal formation that decomposition temperature changes gained ferric oxide nano particulate.And prepared ferric oxide can be stablized in the organic solvents such as being dispersed in chloroform, toluene and whiteruss surely.
Description of drawings
Fig. 1 (a), Fig. 1 (b) are respectively the transmission electron microscope figure and the x-ray diffraction pattern of the Indian red nanoparticle that stearic acid is modified among the embodiment 1.As seen from the figure: the Indian red particle diameter that the gained stearic acid is modified is even, and median size is about 5nm; XRD figure is consistent with the figure of oblique six side's ferric oxide that standard card 84-0308 is given;
Fig. 2 (a), Fig. 2 (b) are respectively the transmission electron microscope figure and the x-ray diffraction pattern of the Indian red nanoparticle that stearic acid is modified among the embodiment 2.As seen from the figure: the Indian red particle diameter that the gained stearic acid is modified is not too even, and median size is about 7nm; XRD figure is consistent with the figure of oblique six side's ferric oxide that standard card 84-0308 is given.
Fig. 3 (a), Fig. 3 (b) are respectively the transmission electron microscope figure (a) and the x-ray diffraction pattern (b) of the 14 Indian red nanoparticles of modifying among the embodiment 3.As seen from the figure: the Indian red particle diameter that the gained TETRADECONIC ACID is modified is even, and median size is about 5nm; XRD figure is consistent with the figure of oblique six side's ferric oxide that standard card 84-0308 is given.
Fig. 4 is the transmission electron microscope figure of the Indian red nanoparticle that laurostearic acid is modified among the embodiment 4.As seen from the figure: the Indian red particle diameter that the gained laurostearic acid is modified is even, is sphere, and median size is about 8nm.
Fig. 5 is the transmission electron microscope figure of the Indian red nanoparticle that capric acid is modified among the embodiment 5.As seen from the figure: the Indian red particle diameter that the gained capric acid is modified is even, is sphere, and median size is about 5nm.
Fig. 6 (a), Fig. 6 (b) are respectively the transmission electron microscope figure and the x-ray diffraction pattern of the Indian red nanoparticle that capric acid is modified among the embodiment 6.As seen from the figure: the Indian red particle diameter that the gained capric acid is modified is even, is cubes, and median size is about 40nm; Belong to oblique six side's ferric oxide (PDF card number 13-0534).
Fig. 7 (a), Fig. 7 (b) are respectively the transmission electron microscope figure and the x-ray diffraction pattern of the Indian red nanoparticle of modifying into n-caproic acid among the embodiment 7.As seen from the figure: the Indian red particle diameter that the gained n-caproic acid is modified is inhomogeneous, is cubes, and median size is about 28nm; Belong to oblique six side's ferric oxide (PDF card number 13-0534).
Embodiment
Example 1, the stearic acid of getting 0.01mol are dissolved in the 10ml ethanol.Under room temperature and agitation condition, add the ethanolic soln 50ml that is dissolved with 4.4g nine nitric hydrate iron, behind the reaction 5min, add the 5ml strong aqua rapidly, produce a large amount of pale brown look precipitations in the brown-red solution at once, filtration, dry that pale brown toner end is presoma.Get the 5g presoma and put into airtight tetrafluoroethylene reactor and be placed on retort furnace, be warming up to 250 ℃ of insulation 6h after, get the ferric oxide that the 2.3g brown-black powder is stearic acid modification with minimum of chloroform and washing with acetone.
In example 2, the present embodiment, be warming up to 280 ℃ of insulations in the retort furnace, getting the 2.21g brown-black powder at last is the ferric oxide that stearic acid is modified.Other are with embodiment 1.
In example 3, the present embodiment, stearic acid changes TETRADECONIC ACID into, and getting the 2.5g brown-black powder at last is the ferric oxide that TETRADECONIC ACID is modified.Other are with embodiment 1.
In example 4, the present embodiment, stearic acid changes laurostearic acid into, and getting the 2.56g brown-black powder at last is the ferric oxide that laurostearic acid is modified.Other are with embodiment 1.
In example 5, the present embodiment, stearic acid changes capric acid into, is incubated 1h in the retort furnace, and getting the 2.63g brown-black powder at last is the ferric oxide that capric acid is modified.Other are with embodiment 1.
In example 6, the present embodiment, be incubated 6h in the retort furnace, getting the 2.4g brown-black powder at last is the ferric oxide that capric acid is modified.Other are with embodiment 5.
In example 7, the present embodiment, stearic acid changes n-caproic acid into, is incubated 1h in the retort furnace, and getting the 3.1g brown-black powder at last is the ferric oxide that n-caproic acid is modified.Other are with embodiment 1.
Interpretation with instrument and experiment condition is: JEM100CX-II type transmission electron microscope, Japanese JEOL company, acceleration voltage 100kV; X ' pert pro type x-ray diffractometer, Dutch Philips company, the X-ray diffraction device adopts monochromator CuK α target, scanning speed 0.02s
-1
Claims (3)
1, a kind of method for preparing single dispersion, oil soluble, surface modified iron oxide nanoparticle is characterized in that, the ethanolic soln of soluble ferric iron salt is mixed with the ethanolic soln of lipid acid, add alkali stir presoma ferric iron hydrogen-oxygen soap precipitation; Unit presoma ferric iron hydrogen-oxygen soap solves target product in solvent-free direct heat down.
2, the method for preparing single dispersion, oil soluble, surface modified iron oxide nanoparticle as claimed in claim 1, it is characterized in that, described soluble ferric iron salt is iron nitrate, iron(ic) chloride or ferric sulfate, described lipid acid is that carbon chain lengths is one or more combination of 6～22 saturated fatty acid or unsaturated fatty acids, and described alkali is sodium hydroxide, potassium hydroxide or strong aqua.
3, the method for preparing single dispersion, oil soluble, surface modified iron oxide nanoparticle as claimed in claim 1 or 2 is characterized in that the mol ratio of described lipid acid and soluble ferric iron salt is 1-3; The concentration 0.01-1mol/L of fatty acid ethanolamide solution, the concentration of soluble ferric iron salt ethanolic soln is the 0.2mol/L-saturation concentration; Pyrolysis temperature 210-280 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200610107323A CN101003386B (en) | 2006-10-19 | 2006-10-19 | Method for preparing Nano microparticles of monodisperse, oil soluble, surface modified iron oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200610107323A CN101003386B (en) | 2006-10-19 | 2006-10-19 | Method for preparing Nano microparticles of monodisperse, oil soluble, surface modified iron oxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101003386A true CN101003386A (en) | 2007-07-25 |
| CN101003386B CN101003386B (en) | 2010-05-12 |
Family
ID=38702823
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200610107323A Expired - Fee Related CN101003386B (en) | 2006-10-19 | 2006-10-19 | Method for preparing Nano microparticles of monodisperse, oil soluble, surface modified iron oxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101003386B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103274475A (en) * | 2013-06-04 | 2013-09-04 | 桂林理工大学 | Preparation method of castor oil coated magnetic iron oxide nanoparticles |
| CN109897700A (en) * | 2019-02-19 | 2019-06-18 | 南京科技职业学院 | A kind of iron-based nano material and its application |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1180079A (en) * | 1995-07-06 | 1998-04-29 | 中国科学院兰州化学物理研究所 | Fatty acid modifying metallic oxide or hydroxide nanometre powder and its preparing method |
| CN100335171C (en) * | 2004-10-21 | 2007-09-05 | 北京大学 | Transition metal-gamma-Fe2o3 nano material, its preparation method and application |
-
2006
- 2006-10-19 CN CN200610107323A patent/CN101003386B/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103274475A (en) * | 2013-06-04 | 2013-09-04 | 桂林理工大学 | Preparation method of castor oil coated magnetic iron oxide nanoparticles |
| CN109897700A (en) * | 2019-02-19 | 2019-06-18 | 南京科技职业学院 | A kind of iron-based nano material and its application |
| CN109897700B (en) * | 2019-02-19 | 2020-11-03 | 南京科技职业学院 | Iron-based nano material and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101003386B (en) | 2010-05-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Darezereshki et al. | A novel thermal decomposition method for the synthesis of ZnO nanoparticles from low concentration ZnSO4 solutions | |
| CN103204525A (en) | Application of lactam as solvent in nano-grade material preparation | |
| CN109437341B (en) | Preparation method of metal oxide or composite material thereof, application and battery | |
| CN102674476A (en) | Chemical preparation method of magnetic graphene | |
| Ying et al. | Preparation of ultrafine nickel powder by polyol method and its oxidation product | |
| CN105460978A (en) | Large-scale preparation method of carbon-doped ferrite porous microspheres | |
| CN102838172B (en) | Method for preparing nanometer alpha-Fe2O3 material | |
| Zanchettin et al. | High performance magnetically recoverable Fe3O4 nanocatalysts: fast microwave synthesis and photo-fenton catalysis under visible-light | |
| CN101508468B (en) | Nano-superstructure polyporous material of ferrite and method of preparing the same | |
| US20050214190A1 (en) | Method of synthesizing nanorods by reaction of metal-surfactant complexes injected using a syringe pump | |
| Matson et al. | Nanophase iron-based liquefaction catalysts: Synthesis, characterization, and model compound reactivity | |
| Thambiliyagodage et al. | Leaching of ilmenite to produce titanium based materials: a review | |
| CN101136278A (en) | Method for producing magnetic fluid | |
| CN111530459A (en) | Preparation method and application of 0D/2D composite material based on AlOOH nanosheets | |
| CN101003386B (en) | Method for preparing Nano microparticles of monodisperse, oil soluble, surface modified iron oxide | |
| Darezereshki et al. | Chemical process of synthesizing zinc oxide (ZnO) with nanorod and spherical morphologies | |
| WO2006098756A2 (en) | Synthetic control of metal oxide nanocrystal sizes and shapes | |
| CN102001712A (en) | Method for preparing superparamagnetic Fe3O4 nano particle based on thermal decomposition of template | |
| CN1230472C (en) | Method for preparing nano iron oxide red | |
| CN112125344A (en) | Preparation method of monodisperse nano iron oxide dispersoid | |
| Vakylabad et al. | A procedure for processing of pregnant leach solution (PLS) produced from a chalcopyrite-ore bio-heap: CuO Nano-powder fabrication | |
| CN103920874A (en) | Preparation method of hollow composite nano-particles | |
| CN101003388A (en) | Method for preparing Nano cube of hematite | |
| CN110339844A (en) | Fe nanometer rods and Pt@Fe Nanorods Catalyst and synthesis and application | |
| CN1103257C (en) | Process for preparing superfine powder by thermolyzing metal complex |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20100512 Termination date: 20201019 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |