CN107043133A - Flower-shaped γ Fe2O3The preparation method of microballoon - Google Patents
Flower-shaped γ Fe2O3The preparation method of microballoon Download PDFInfo
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- CN107043133A CN107043133A CN201710186596.2A CN201710186596A CN107043133A CN 107043133 A CN107043133 A CN 107043133A CN 201710186596 A CN201710186596 A CN 201710186596A CN 107043133 A CN107043133 A CN 107043133A
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- flower
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- microballoon
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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
- C01G49/06—Ferric oxide (Fe2O3)
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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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
The invention discloses a kind of flower-shaped γ Fe2O3The preparation method of microballoon, belongs to field of nano material preparation, and it is that filling carries out product separating, washing, drying after solvent thermal reaction, reaction in a kettle., obtains flower-shaped γ Fe after mixing iron pentacarbonyl and glycerine solvent2O3Microballoon.The flower-shaped γ Fe of gained2O3Microballoon property is stable, with good light resistance and the shielding to ultraviolet, is widely used in fields such as magnetic, air-sensitive and catalysis.The preparation technology of the present invention is simple, easy to operate, and product purity is high, and uniform particle diameter, good dispersion is particularly suitable for large-scale industrial production.
Description
Technical field
The present invention relates to a kind of flower-shaped γ-Fe2O3The preparation method of microballoon, belongs to technical field of nano material.
Background technology
In numerous metal oxides, γ-Fe2O3Microballoon is because it is in the potential of the fields such as magnetic, air-sensitive, sensing and catalysis
Application prospect has attracted the great interest of researcher.Wherein, γ-Fe2O3The pattern and size dispersity of microballoon are influences
γ-Fe2O3Two the most key factors of performance, directly decide γ-Fe2O3Physico-chemical property and practical application effect.
Currently, researcher has been developed that a variety of synthetic methods prepare γ-Fe2O3It is microballoon, such as chemical coprecipitation, molten
The hot method of agent, microemulsion method, sol-gal process, electrochemical process, vapour deposition process, flame thermal decomposition method, laser heating etc..Using
Efficient synthetic method, prepares high-quality γ-Fe2O3Microballoon is still important research class of the pendulum in face of scientific worker
Topic.
The content of the invention
It is an object of the invention to：A kind of flower-shaped γ-Fe are provided2O3The preparation method of microballoon, simplifies process conditions, realizes
Flower-shaped γ-Fe2O3The scale industrial production of microballoon.
The present invention technical solution be：Flower-shaped γ-Fe2O3The preparation method of microballoon be by source of iron of iron pentacarbonyl, third
Triol is solvent, and flower-shaped γ-Fe are prepared under the conditions of solvent heat2O3Microballoon；Comprise the following steps that：Iron pentacarbonyl is added to third
In three alcoholic solvents, under normal temperature and pressure, stirring obtains light yellow settled solution；Again by the filling of light yellow settled solution in a kettle.
Carry out solution solvent thermal response；Product after solvent thermal reaction is centrifuged, and product is carried out with ethanol and deionized water
Exchange washing；Product freeze-day with constant temperature, produces flower-shaped γ-Fe after cleaning2O3Microspheres product.
Wherein, the volume ratio of iron pentacarbonyl and glycerine solvent is 1:35.
Wherein, reaction solution accounts for the 60%-80% of reactor volume, and 180-220 DEG C is warming up to 5 DEG C/minute of the rate of heat addition,
And react 12-16 hours at such a temperature.
Wherein, product 100-140 DEG C of constant temperature drying 10 hours after cleaning.
Advantages of the present invention and effect are：
1st, traditional source of iron such as ferric nitrate, iron chloride, ferric sulfate is substituted using iron pentacarbonyl, and is solvent from glycerine, used
The simple step of solvent thermal reaction technique one obtains flower-shaped γ-Fe2O3Microspheres product, the technique of this method and required production equipment
Simply, it is easy to operate, it is adapted to large-scale industrial production.
2nd, synthesized γ-Fe2O3Microballoon is flower-shaped, uniform particle diameter, and dispersive property is good, and particle diameter is about 2 microns, and product is pure
Degree is high.
Brief description of the drawings
Flower-shaped γ-the Fe of Fig. 12O3The stereoscan photograph of microspheres product.
Embodiment
Technical scheme is further illustrated with reference to embodiment, but these embodiments are not to be construed as to skill
The limitation of art scheme.
Embodiment 1：By iron pentacarbonyl with volume ratio 1:35 are added in glycerine solvent, and under normal temperature and pressure, stirring is obtained
Light yellow settled solution；The filling of light yellow settled solution is subjected to solution solvent thermal response in a kettle. again, reaction solution is accounted for
The 60% of reactor volume, is warming up to 180 DEG C, and react 12 hours at such a temperature with 5 DEG C/minute of the rate of heat addition；Solvent heat is anti-
Product after answering is centrifuged, and washing is swapped to product with ethanol and deionized water；100 DEG C of product constant temperature after cleaning
Dry 10 hours, obtain flower-shaped γ-Fe2O3Microspheres product.
Embodiment 2：By iron pentacarbonyl with volume ratio 1:35 are added in glycerine solvent, and under normal temperature and pressure, stirring is obtained
Light yellow settled solution；The filling of light yellow settled solution is subjected to solution solvent thermal response in a kettle. again, reaction solution is accounted for
The 70% of reactor volume, is warming up to 200 DEG C, and react 14 hours at such a temperature with 5 DEG C/minute of the rate of heat addition；Solvent heat is anti-
Product after answering is centrifuged, and washing is swapped to product with ethanol and deionized water；120 DEG C of product constant temperature after cleaning
Dry 10 hours, obtain flower-shaped γ-Fe2O3Microspheres product.
Embodiment 3：By iron pentacarbonyl with volume ratio 1:35 are added in glycerine solvent, and under normal temperature and pressure, stirring is obtained
Light yellow settled solution；The filling of light yellow settled solution is subjected to solution solvent thermal response in a kettle. again, reaction solution is accounted for
The 80% of reactor volume, is warming up to 220 DEG C, and react 16 hours at such a temperature with 5 DEG C/minute of the rate of heat addition；Solvent heat is anti-
Product after answering is centrifuged, and washing is swapped to product with ethanol and deionized water；140 DEG C of product constant temperature after cleaning
Dry 10 hours, obtain flower-shaped γ-Fe2O3Microspheres product.
Flower-shaped γ-Fe obtained by embodiment 1-32O3The stereoscan photograph of microspheres product is as shown in Figure 1.
Claims (4)
1. flower-shaped γ-Fe2O3The preparation method of microballoon, it is characterised in that：By source of iron of iron pentacarbonyl, glycerine be solvent, molten
Flower-shaped γ-Fe are prepared under agent heat condition2O3Microballoon；Comprise the following steps that：Iron pentacarbonyl is added in glycerine solvent, normal temperature
Under normal pressure, stirring obtains light yellow settled solution；The filling of light yellow settled solution is subjected to solution solvent heat in a kettle. again
Reaction；Product after solvent thermal reaction is centrifuged, and washing is swapped to product with ethanol and deionized water；After cleaning
Product freeze-day with constant temperature, produces flower-shaped γ-Fe2O3Microspheres product.
2. flower-shaped γ-Fe according to claim 12O3The preparation method of microballoon, it is characterised in that：Iron pentacarbonyl and the third three
The volume ratio of alcoholic solvent is 1:35.
3. flower-shaped γ-Fe according to claim 12O3The preparation method of microballoon, it is characterised in that：Reaction solution accounts for reaction
The 60%-80% of kettle volume, is warming up to 180-220 DEG C, and react 12-16 hours at such a temperature with 5 DEG C/minute of the rate of heat addition.
4. flower-shaped γ-Fe according to claim 12O3The preparation method of microballoon, it is characterised in that：Product constant temperature after cleaning
100-140 DEG C of drying 10 hours.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710186596.2A CN107043133B (en) | 2017-03-27 | 2017-03-27 | Flower-shaped γ Fe2O3The preparation method of microballoon |
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| CN201710186596.2A CN107043133B (en) | 2017-03-27 | 2017-03-27 | Flower-shaped γ Fe2O3The preparation method of microballoon |
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| CN107043133A true CN107043133A (en) | 2017-08-15 |
| CN107043133B CN107043133B (en) | 2018-04-10 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107649132A (en) * | 2017-09-22 | 2018-02-02 | 陕西科技大学 | The preparation method of nanometer γ di-iron trioxide photochemical catalysts |
| CN108393088A (en) * | 2018-01-23 | 2018-08-14 | 西北大学 | A kind of preparation method of γ-di-iron trioxide/rGO composite materials of flower-like microsphere structure |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101293674A (en) * | 2008-06-12 | 2008-10-29 | 浙江大学 | Method for preparing spindle shaped alpha-Fe2O3 powder |
| 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 |
| CN103949212A (en) * | 2014-04-11 | 2014-07-30 | 上海交通大学 | Preparation method of biomass-based magnetic biochar |
| CN105036115A (en) * | 2015-07-29 | 2015-11-11 | 桂林电子科技大学 | Carbon nanotube uniformly and stably loaded with iron-containing nano particles and preparation method of carbon nanotube |
-
2017
- 2017-03-27 CN CN201710186596.2A patent/CN107043133B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101293674A (en) * | 2008-06-12 | 2008-10-29 | 浙江大学 | Method for preparing spindle shaped alpha-Fe2O3 powder |
| 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 |
| CN103949212A (en) * | 2014-04-11 | 2014-07-30 | 上海交通大学 | Preparation method of biomass-based magnetic biochar |
| CN105036115A (en) * | 2015-07-29 | 2015-11-11 | 桂林电子科技大学 | Carbon nanotube uniformly and stably loaded with iron-containing nano particles and preparation method of carbon nanotube |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107649132A (en) * | 2017-09-22 | 2018-02-02 | 陕西科技大学 | The preparation method of nanometer γ di-iron trioxide photochemical catalysts |
| CN107649132B (en) * | 2017-09-22 | 2019-11-15 | 陕西科技大学 | Nanometer γ-di-iron trioxide photochemical catalyst preparation method |
| CN108393088A (en) * | 2018-01-23 | 2018-08-14 | 西北大学 | A kind of preparation method of γ-di-iron trioxide/rGO composite materials of flower-like microsphere structure |
| CN108393088B (en) * | 2018-01-23 | 2020-11-27 | 西北大学 | Preparation method of gamma-ferric oxide/rGO composite material with flower-like microsphere structure |
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| CN107043133B (en) | 2018-04-10 |
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