CN107055629B - Monodisperse acanthosphere shape nanometer Fe3O4Preparation method - Google Patents
Monodisperse acanthosphere shape nanometer Fe3O4Preparation method Download PDFInfo
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- CN107055629B CN107055629B CN201710186618.5A CN201710186618A CN107055629B CN 107055629 B CN107055629 B CN 107055629B CN 201710186618 A CN201710186618 A CN 201710186618A CN 107055629 B CN107055629 B CN 107055629B
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- monodisperse
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide (Fe3O4)
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
- C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
The invention discloses a kind of monodisperse acanthosphere shape nanometer Fes3O4Preparation method, belong to field of nano material preparation, be will iron pentacarbonyl and methanol solvate mix after fill and carry out solvent thermal reaction in a kettle, then the black product obtained will be reacted and centrifuged, obtain monodisperse acanthosphere shape nanometer Fe3O4.The preparation process of the present invention is simple, easy to operate, and product purity is high, and uniform particle diameter, good dispersion is very suitable for large-scale production.
Description
Technical field
The present invention relates to field of nano material preparation, especially a kind of to utilize solvent structure monodisperse acanthosphere shape nanometer
Fe3O4Method.
Background technology
Nano ferriferrous oxide（Fe3O4）Magnetic particle is using most because it is with unique magnetic effect, skin effect etc.
For one of extensive soft magnetic material, and because it is with superparamagnetism, the separation of solid, liquid phase is very simple under external magnetic field
It is single, can save the complex operations such as centrifugation, filtering, therefore in magnetic fluid, cell separation, protein purify, targeting drug delivery system and
Clinics and Practices of tumour etc. become the hot spot of nano magnetic material field and field of functional materials research.
In the past more than ten years, various preparation nanometer Fes3O4Method receive much attention, up to the present, have been developed
A variety of synthetic methods, such as hydro-thermal method（Solvent heat）, settlement-oxidation method, microemulsion method, sol-gal process, high-temperature decomposition, etc. from
Sub- synthetic method, ray Radiation Synthesis Method etc..
Granule-morphology and size dispersity are to influence nanometer Fe3O4Magnetic particle applies two the most key factors, directly
Decide nanometer Fe3O4Physico-chemical property, including magnetic, light, electricity, heat and catalytic activity etc..Prepare the nanometer Fe of high quality3O4
Magnetic particle is still important subject of the pendulum in face of scientific worker.
Invention content
It is an object of the invention to：A kind of monodisperse acanthosphere shape nanometer Fe is provided3O4Preparation method, simplify working condition,
Realize monodisperse acanthosphere shape nanometer Fe3O4Scale industrial production.
The present invention technical solution be：The monodisperse acanthosphere shape nanometer Fe3O4Preparation method be using iron pentacarbonyl as
Source of iron, methanol be both solvent or be reducing agent, under the conditions of solvent heat, one-step synthesis monodisperse acanthosphere shape nanometer Fe3O4；Specifically
Step is as follows：Iron pentacarbonyl is added in methanol solvate, under normal temperature and pressure, stirs to get yellow clear solution；Yellow is clear
Clear solution filling carries out solvent thermal reaction in a kettle；Product after solvent thermal reaction is centrifuged, with ethyl alcohol and
Deionized water repeatedly washs product, dry, obtains black product, as monodisperse acanthosphere shape nanometer Fe3O4Product.
Wherein, the volume ratio of iron pentacarbonyl and methanol solvate is 1:25.
Wherein, reaction solution accounts for the 40%-80% of reactor volume, and reaction temperature is warming up to 5 DEG C/minute of the rate of heat addition
170-200 DEG C, and react 6-12 hours at such a temperature.
Wherein, the product after solvent thermal reaction is centrifuged, is washed, and 70 DEG C of dryings 3 hours.
The present invention preparation principle be：Under the conditions of solvent heat, methanol solvate has weaker reducing property, by pentacarbonyl
Iron is reduced into ferriferrous oxide nano crystalline substance, the ferriferrous oxide nano crystalline substance of formation because grain size is small, large specific surface area, surface can be high,
Final self-assemble forms acanthosphere shape nanometer Fe3O4。
The beneficial effects of the invention are as follows：
1st, nanometer Fe will be synthesized in traditional handicraft3O4Source of iron（Such as：Ferric nitrate, iron chloride, ferric sulfate etc.）Replace with five
Carbonyl iron just obtains high quality monodisperse acanthosphere shape nanometer Fe using simple one step of solvent thermal process3O4Product, this method work
Skill and required production equipment are simple, easy to operate, are suitble to scale industrial production.
2nd, synthesized nanometer Fe3O4For acanthosphere shape, about uniform particle diameter, 500 nm, product purity is high, good dispersion.
3rd, in this reaction system, iron pentacarbonyl is unique source of iron, and methanol solvate had both been solvent or had been reducing agent, in reaction
Without additional surfactants.
Description of the drawings
Fig. 1 is monodisperse acanthosphere shape nanometer Fe3O4Stereoscan photograph.
Fig. 2 is monodisperse acanthosphere shape nanometer Fe3O4X-ray diffractogram.
Specific embodiment
The technical solution further illustrated the present invention with reference to embodiment, but embodiment is not to be construed as to skill
The limitation of art scheme.
Embodiment 1：By iron pentacarbonyl with volume ratio 1:25 are added in methanol solvate, under normal temperature and pressure, stir to get Huang
Color clear solution；Yellow clear solution filling is subjected to solvent thermal reaction in a kettle, reaction solution accounts for reactor volume
40%, 170 DEG C of reaction temperature is warming up to 5 DEG C/minute of the rate of heat addition, and in the thermotonus 6 hours；After solvent thermal reaction
Product be centrifuged, product is repeatedly washed with ethyl alcohol and deionized water, 70 DEG C of dryings 3 hours obtain black
Product, as monodisperse acanthosphere shape nanometer Fe3O4Product.
Embodiment 2：By iron pentacarbonyl with volume ratio 1:25 are added in methanol solvate, under normal temperature and pressure, stir to get Huang
Color clear solution；Yellow clear solution filling is subjected to solvent thermal reaction in a kettle, reaction solution accounts for reactor volume
60%, 180 DEG C of reaction temperature is warming up to 5 DEG C/minute of the rate of heat addition, and in the thermotonus 8 hours；After solvent thermal reaction
Product be centrifuged, product is repeatedly washed with ethyl alcohol and deionized water, 70 DEG C of dryings 3 hours obtain black
Product, as monodisperse acanthosphere shape nanometer Fe3O4Product.
Embodiment 3：By iron pentacarbonyl with volume ratio 1:25 are added in methanol solvate, under normal temperature and pressure, stir to get Huang
Color clear solution；Yellow clear solution filling is subjected to solvent thermal reaction in a kettle, reaction solution accounts for reactor volume
80%, 200 DEG C of reaction temperature is warming up to 5 DEG C/minute of the rate of heat addition, and in the thermotonus 12 hours；After solvent thermal reaction
Product be centrifuged, product is repeatedly washed with ethyl alcohol and deionized water, 70 DEG C of dryings 3 hours obtain black
Product, as monodisperse acanthosphere shape nanometer Fe3O4Product.
Embodiment 4：By iron pentacarbonyl with volume ratio 1:25 are added in methanol solvate, under normal temperature and pressure, stir to get Huang
Color clear solution；Yellow clear solution filling is subjected to solvent thermal reaction in a kettle, reaction solution accounts for reactor volume
70%, 190 DEG C of reaction temperature is warming up to 5 DEG C/minute of the rate of heat addition, and in the thermotonus 10 hours；After solvent thermal reaction
Product be centrifuged, product is repeatedly washed with ethyl alcohol and deionized water, 70 DEG C of dryings 3 hours obtain black
Product, as monodisperse acanthosphere shape nanometer Fe3O4Product.
Monodisperse acanthosphere shape nanometer Fe obtained by embodiment 1-43O4The stereoscan photograph of product is as shown in Figure 1, its X is penetrated
Ray diffraction diagram is as shown in Figure 2.
Claims (1)
1. monodisperse acanthosphere shape nanometer Fe3O4Preparation method, it be using iron pentacarbonyl as source of iron, methanol be both solvent and also for also
Former agent, under the conditions of solvent heat, one-step synthesis monodisperse acanthosphere shape nanometer Fe3O4；It is characterized in that it is as follows：
Iron pentacarbonyl is added in methanol solvate, under normal temperature and pressure, stirs to get yellow clear solution；Yellow clear solution is filled
Solvent thermal reaction is carried out in a kettle；Product after solvent thermal reaction is centrifuged, with ethyl alcohol and deionized water pair
Product is repeatedly washed, dry, obtains black product, as monodisperse acanthosphere shape nanometer Fe3O4Product；Wherein, iron pentacarbonyl
Volume ratio with methanol solvate is 1:25；Reaction solution accounts for the 40%-80% of reactor volume, is heated up with 5 DEG C/minute of the rate of heat addition
To 170-200 DEG C of reaction temperature, and react 6-12 hours at such a temperature；Product after solvent thermal reaction is centrifuged, is washed,
And 70 DEG C of dryings 3 hours.
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| CN110745869A (en) * | 2019-11-11 | 2020-02-04 | 青岛科技大学 | FeS nano-particles synthesized based on solvothermal method, preparation method and application |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103007887A (en) * | 2013-01-08 | 2013-04-03 | 长沙矿冶研究院有限责任公司 | Carbon-nanotube-loaded multi-stage nanometer ferroferric oxide adsorbent and preparation method and application thereof |
| CN103316614A (en) * | 2013-06-05 | 2013-09-25 | 浙江大学 | Gamma-Fe2O3/SiO2 nano-grade composite material preparation method, and nano-grade composite material particles |
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- 2017-03-27 CN CN201710186618.5A patent/CN107055629B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103007887A (en) * | 2013-01-08 | 2013-04-03 | 长沙矿冶研究院有限责任公司 | Carbon-nanotube-loaded multi-stage nanometer ferroferric oxide adsorbent and preparation method and application thereof |
| CN103316614A (en) * | 2013-06-05 | 2013-09-25 | 浙江大学 | Gamma-Fe2O3/SiO2 nano-grade composite material preparation method, and nano-grade composite material particles |
Non-Patent Citations (1)
| Title |
|---|
| "纳米结构Fe3O4的制备与物性研究";刘亚南;《中国优秀硕士学位论文全文数据库（电子期刊）工程科技I辑》;20120315(第3期);B020-146正文第27-28、30页 * |
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