CN103204550A - Controllable preparation method of micron-order Fe2O3 - Google Patents
Controllable preparation method of micron-order Fe2O3 Download PDFInfo
- Publication number
- CN103204550A CN103204550A CN2013101281794A CN201310128179A CN103204550A CN 103204550 A CN103204550 A CN 103204550A CN 2013101281794 A CN2013101281794 A CN 2013101281794A CN 201310128179 A CN201310128179 A CN 201310128179A CN 103204550 A CN103204550 A CN 103204550A
- Authority
- CN
- China
- Prior art keywords
- solution
- feso
- micron
- gained
- throw out
- 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.)
- Pending
Links
Abstract
The invention provides a controllable preparation method of micron-order Fe2O3. The controllable preparation method comprises the following steps of: mixing an FeSO4 with a sodium hydroxide solution according to a volume ratio of 2:5, fully dissolving, and performing low-frequency ultrasonic auxiliary processing until the mixed liquor is light green; then transferring the solution into a Teflon hydrothermal kettle, wherein the packing ratio in reaction kettle is 10-70%; and preserving heat at 130-150 DEG C for 1-15 hours, taking out precipitate, washing and then centrifugalizing, and drying at 80 DEG C under an air atmosphere. The method provided by the invention solves the problem that nucleation and growth are uncontrollable, and the prepared micron-sized grains are very narrow in size distribution and have high phase purity.
Description
[technical field]
The invention belongs to wet chemistry method and prepare the nano-powder technical field, be specifically related to a kind of controllable method for preparing of micron order ferric oxide.
[background technology]
Fe
2O
3Material becomes the focus of Recent study because of its application at aspects such as coating, sensor, catalysis and electrode materialss.At present, the preparation method of a lot of different ferric oxide is arranged both at home and abroad, the preparation method who has reported all can obtain than fine particle, still in the result that still can not obtain aspect the controllability of the size of particle and nucleating growth to be satisfied with.
Chinese patent is announced CN100436334C number and has been reported that a kind of is the feedstock production magnetic Fe with converter slag
2O
3Method.By slag is ground, pickling is leached and is made FeSO
4Solution then with obtaining precipitation after the alkaline purification, adds crystal seed at last and forms γ--Fe through high temperature crystallization
2O
3Though method can obtain high-purity powder, but still owing to obtain by intermediate processing, nucleation process is uncontrollable, and the particle diameter of acquisition is bigger.In addition, also need to add crystal seed.
Li Yuehuas etc. are with Fe
3O
4Be raw material, prepared γ-Fe by air oxidation process
2O
3, but its particle diameter is bigger, and distribution range is very wide, between 30nm-400nm.In addition, people such as Wu is with citric acid, FeSO
47H
2O and PEG are raw material, the single-phase α-Fe that adopted Prepared by Sol Gel Method
2O
3Particle.But processing parameter is strict and wayward, and the reaction times is longer, the cost height, and also can volatilize toxic organic compound in the preparation process, contaminate environment is not suitable for scale operation.
Reference:
Liu Chengjun, etc. a kind of for the preparation method who makes the high purity magnetic material nano ferric oxide, Chinese invention patent, CN100436334C, 2007.
Li Yuehua, etc. preparation and the magnetic behavior thereof of nanometer-Fe2O3 particle, functional materials, 2007,38(supplementary issue): 1981-1983.
Y.L.Wu,X.F.Wang.Preparation?and?characterization?of?single-phaseα-Fe2O3nano-powders?by?pechini?sol-gel?method[J].Materials?Letters,2011,65(13):2062-2065．
[summary of the invention]
The purpose of this invention is to provide a kind of micron order Fe
2O
3Controllable method for preparing, solved nucleation and the growth uncontrollable problem, the particle size distribution of the micron-scale of preparation is very narrow, phase purity is higher.
Concrete grammar of the present invention is as follows:
A kind of micron order Fe
2O
3Controllable method for preparing, be 2:5 mixing FeSO according to volume ratio
4Solution and sodium hydroxide solution fully after the dissolving, adopt the low-frequency ultrasonic waves auxiliary treatment, are light green until mixed solution; Then, solution is moved in the Teflon water heating kettle, wherein, the packing ratio of reactor is 10～70%, at 130～150 ℃ of insulation 1～15h, takes out throw out, flushing back centrifugal treating, then under 80 ℃ in air atmosphere dry getting final product.
As the preferred embodiments of the present invention, described FeSO
4The volumetric molar concentration of solution is 0.8～1.8mol/L.
As the preferred embodiments of the present invention, the volumetric molar concentration of described sodium hydroxide solution is 5～10mol/L.
As the preferred embodiments of the present invention, during the low-frequency ultrasonic waves auxiliary treatment, ultrasonic power is 40-70W.
As the preferred embodiments of the present invention, the throw out that takes out from described water heating kettle cleans after centrifugal to the neutrality dry again.
Compared with prior art, the present invention has the following advantages at least:
1) Fe of the present invention's preparation
2O
3, desired raw material is easy to get, and synthetic cost is lower.
2) the present invention is by Hydrothermal Preparation Fe
2O
3, its nucleation and process of growth are controlled, particle crystallization degree height.
3) the present invention is by Hydrothermal Preparation Fe
2O
3, with ultrasonic applications in chemical reaction process, the Fe of preparation
2O
3Technological operation is easy, sample phase purity height, and grain graininess is more even, and particle size distribution range concentrates between the 1um-2um.
[description of drawings]
Fig. 1 is the Fe of example 1 preparation
3O
4X ray diffracting spectrum, the result shows that the submicron powder phase purity of preparation is higher, and degree of crystallinity is better.
[concrete embodiment]
Concrete grammar of the present invention is as follows:
1) with FeSO
47H
2O and NaOH are dissolved in respectively in the distilled water, and it is the FeSO of 0.8～1.8mol/L that the dissolving back forms concentration
4Solution and concentration are the NaOH solution of 5～10mol/L;
2) FeSO that step 1 is disposed
4Solution is dissolved in the NaOH solution of step 1 configuration, control FeSO
4The volume ratio of solution and NaOH solution is 2:5, stirs it is fully dissolved;
3) with the mixing solutions of low-frequency ultrasonic waves auxiliary treatment step 2 gained, ultrasonic power is 40～70W, and ultrasonic time is 8～12min, is light green until mixed solution;
4) in the Teflon water heating kettle that the solution immigration volume that step 3 is obtained is, packing ratio is 10～70%, under 130-150 ℃ of temperature, and insulation 1～15h;
5) in step 4 gained precipitation, add the 200ml distilled water flushing, and carry out centrifugal treating, centrifuge speed is 12000r/min, centrifugation time is 5～10min, after centrifugally operated is finished most of supernatant liquid is outwelled, cleaning so repeatedly 5～10 times, is neutral (pH=7.0～7.5) until supernatant liquid, obtains throw out;
6) with step 5 gained throw out under 80 ℃ of conditions, carry out drying in the air atmosphere, obtain product;
7) product is carried out the identification of phases by X-ray diffraction (XRD) analysis, field emission scanning electron microscope (FE-SEM) carries out morphology observation, obtains micron-sized Fe at last
2O
3
Below in conjunction with accompanying drawing the present invention is described in further detail:
Embodiment 1
1) with FeSO
47H
2O and NaOH are dissolved in respectively in the distilled water, and it is the FeSO of 0.8mol/L that the dissolving back forms concentration
4Solution and concentration are the NaOH solution of 6.50mol/L;
2) FeSO that step 1 is disposed
4Solution is dissolved in the NaOH solution of step 1 configuration, control FeSO
4The volume ratio of solution and NaOH solution is 2:5, stirs it is fully dissolved;
3) with the mixing solutions of low-frequency ultrasonic waves auxiliary treatment step 2 gained, ultrasonic power is 60W, and ultrasonic time is 10min, is light green until mixed solution;
4) in the Teflon water heating kettle that the solution immigration volume that step 3 is obtained is, packing ratio is 40%, under 140 ℃ of temperature, and insulation 1h;
5) in step 4 gained precipitation, add the 200ml distilled water flushing, and carry out centrifugal treating, centrifuge speed is 12000r/min, centrifugation time is 10min, after centrifugally operated is finished most of supernatant liquid is outwelled, cleaning so repeatedly 7 times, is neutral (pH=7.0～7.5) until supernatant liquid, obtains throw out;
6) with step 5 gained throw out under 80 ℃ of conditions, carry out drying in the air atmosphere, obtain product;
7) product is carried out the identification of phases by X-ray diffraction (XRD) analysis, field emission scanning electron microscope (FE-SEM) carries out morphology observation, obtains micron-sized Fe at last
2O
3Particle, median size 1 μ m.
Embodiment 2
1) with FeSO
47H
2O and NaOH are dissolved in respectively in the distilled water, and it is the FeSO of 1.40mol/L that the dissolving back forms concentration
4Solution and concentration are the NaOH solution of 5.0mol/L;
2) FeSO that step 1 is disposed
4Solution is dissolved in the NaOH solution of step 1 configuration, control FeSO
4The volume ratio of solution and NaOH solution is 2:5, stirs it is fully dissolved;
3) with the mixing solutions of low-frequency ultrasonic waves auxiliary treatment step 2 gained, ultrasonic power is 70W, and ultrasonic time is 10min, is light green until mixed solution;
4) in the Teflon water heating kettle that the solution immigration volume that step 3 is obtained is, packing ratio is 60%, under 130 ℃ of temperature, and insulation 10h;
5) in step 4 gained precipitation, add the 200ml distilled water flushing, and carry out centrifugal treating, centrifuge speed is 12000r/min, centrifugation time is 5min, after centrifugally operated is finished most of supernatant liquid is outwelled, cleaning so repeatedly 9 times, is neutral (pH=7.0～7.5) until supernatant liquid, obtains throw out;
6) with step 5 gained throw out under 80 ℃ of conditions, carry out drying in the air atmosphere, obtain product;
7) product is carried out the identification of phases by X-ray diffraction (XRD) analysis, field emission scanning electron microscope (FE-SEM) carries out morphology observation, obtains micron-sized Fe at last
2O
3Particle, median size are 2 μ m.
Embodiment 3
1) with FeSO
47H
2O and NaOH are dissolved in respectively in the distilled water, and it is the FeSO of 1.80mol/L that the dissolving back forms concentration
4Solution and concentration are the NaOH solution of 10.00mol/L;
2) FeSO that step 1 is disposed
4Solution is dissolved in the NaOH solution of step 1 configuration, control FeSO
4The volume ratio of solution and NaOH solution is 2:5, stirs it is fully dissolved;
3) with the mixing solutions of low-frequency ultrasonic waves auxiliary treatment step 2 gained, ultrasonic power is 70W, and ultrasonic time is 8min, is light green until mixed solution;
4) in the Teflon water heating kettle that the solution immigration volume that step 3 is obtained is, packing ratio is 10%, under 150 ℃ of temperature, and insulation 15h;
5) in step 4 gained precipitation, add the 200ml distilled water flushing, and carry out centrifugal treating, centrifuge speed is 12000r/min, centrifugation time is 8min, after centrifugally operated is finished most of supernatant liquid is outwelled, cleaning so repeatedly 7 times, is neutral (pH=7.0～7.5) until supernatant liquid, obtains throw out;
6) with step 5 gained throw out under 80 ℃ of conditions, carry out drying in the air atmosphere, obtain product;
7) product is carried out the identification of phases by X-ray diffraction (XRD) analysis, field emission scanning electron microscope (FE-SEM) carries out morphology observation, obtains micron-sized Fe at last
2O
3Particle, median size are 1 μ m.
Embodiment 4
1) with FeSO
47H
2O and NaOH are dissolved in respectively in the distilled water, and it is the FeSO of 1.22mol/L that the dissolving back forms concentration
4Solution and concentration are the NaOH solution of 6.00mol/L;
2) FeSO that step 1 is disposed
4Solution is dissolved in the NaOH solution of step 1 configuration, control FeSO
4The volume ratio of solution and NaOH solution is 2:5, stirs it is fully dissolved;
3) with the mixing solutions of low-frequency ultrasonic waves auxiliary treatment step 2 gained, ultrasonic power is 40W, and ultrasonic time is 12min, is light green until mixed solution;
4) in the Teflon water heating kettle that the solution immigration volume that step 3 is obtained is, packing ratio is 70%, under 140 ℃ of temperature, and insulation 6h;
5) in step 4 gained precipitation, add the 200ml distilled water flushing, and carry out centrifugal treating, centrifuge speed is 12000r/min, centrifugation time is 10min, after centrifugally operated is finished most of supernatant liquid is outwelled, cleaning so repeatedly 8 times, is neutral (pH=7.0～7.5) until supernatant liquid, obtains throw out;
6) with step 5 gained throw out under 80 ℃ of conditions, carry out drying in the air atmosphere, obtain product;
7) product is carried out the identification of phases by X-ray diffraction (XRD) analysis, field emission scanning electron microscope (FE-SEM) carries out morphology observation, obtains micron-sized Fe at last
2O
3Particle, median size are 2 μ m.
Claims (6)
1. micron order Fe
2O
3Controllable method for preparing, it is characterized in that: be 2:5 mixing FeSO according to volume ratio
4Solution and sodium hydroxide solution fully after the dissolving, adopt the low-frequency ultrasonic waves auxiliary treatment, are light green until mixed solution; Then, solution is moved in the Teflon water heating kettle, wherein, the packing ratio of reactor is 10～70%, at 130～150 ℃ of insulation 1～15h, takes out throw out, flushing back centrifugal treating, then under 80 ℃ in air atmosphere dry getting final product.
2. the method for claim 1 is characterized in that: described FeSO
4The volumetric molar concentration of solution is 0.8～1.8mol/L.
3. the method for claim 1, it is characterized in that: the volumetric molar concentration of described sodium hydroxide solution is 5～10mol/L.
4. the method for claim 1, it is characterized in that: during the low-frequency ultrasonic waves auxiliary treatment, ultrasonic power is 40-70W.
5. the method for claim 1 is characterized in that: the throw out that takes out from described water heating kettle cleans after centrifugal to the neutrality dry again.
6. micron order Fe
2O
3Controllable method for preparing, it is characterized in that: may further comprise the steps:
1) with volumetric molar concentration is the FeSO of 0.8～1.8mol/L
4Solution is dissolved in the NaOH solution that volumetric molar concentration is 5～10mol/L, control FeSO
4The volume ratio of solution and NaOH solution is 2:5, stirs it is fully dissolved;
2) with the mixing solutions of low-frequency ultrasonic waves auxiliary treatment step 1 gained, ultrasonic power is 40～70W, and ultrasonic time is 8～12min, is light green until mixed solution;
3) solution that step 2 is obtained moves in the Teflon water heating kettle, and packing ratio is 10～70%, under 130-150 ℃ of temperature, and insulation 1～15h;
4) add the 200ml distilled water flushing in step 3 gained precipitation, and carry out centrifugal treating, centrifuge speed is 12000r/min, after centrifugally operated is finished most of supernatant liquid is outwelled, cleaning so repeatedly 5～10 times, is neutral until supernatant liquid, obtains throw out;
5) with step 4 gained throw out under 80 ℃ of conditions, carry out drying in the air atmosphere, obtain product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101281794A CN103204550A (en) | 2013-04-12 | 2013-04-12 | Controllable preparation method of micron-order Fe2O3 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101281794A CN103204550A (en) | 2013-04-12 | 2013-04-12 | Controllable preparation method of micron-order Fe2O3 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103204550A true CN103204550A (en) | 2013-07-17 |
Family
ID=48751993
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2013101281794A Pending CN103204550A (en) | 2013-04-12 | 2013-04-12 | Controllable preparation method of micron-order Fe2O3 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103204550A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108264092A (en) * | 2018-02-09 | 2018-07-10 | 河南理工大学 | A kind of high circulation performance lithium ion battery negative material Fe2O3The preparation method of nanometer needle |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4224175A (en) * | 1978-04-17 | 1980-09-23 | Montedison S.P.A. | Process for the preparation of magnetic powders based on γ-Fe2 O3 |
| CN101817562A (en) * | 2009-09-05 | 2010-09-01 | 大连理工大学 | Method for preparing hollow spherical Alpha-Fe2O3 by carbon-sugar microsphere template method |
| CN101913658A (en) * | 2010-09-16 | 2010-12-15 | 厦门大学 | Alpha type ferric oxide and preparation method thereof |
| CN102180522A (en) * | 2011-03-28 | 2011-09-14 | 陕西宏炬电子科技有限公司 | Controllable preparation method of nano magnetic iron oxide with narrow particle size distribution |
-
2013
- 2013-04-12 CN CN2013101281794A patent/CN103204550A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4224175A (en) * | 1978-04-17 | 1980-09-23 | Montedison S.P.A. | Process for the preparation of magnetic powders based on γ-Fe2 O3 |
| CN101817562A (en) * | 2009-09-05 | 2010-09-01 | 大连理工大学 | Method for preparing hollow spherical Alpha-Fe2O3 by carbon-sugar microsphere template method |
| CN101913658A (en) * | 2010-09-16 | 2010-12-15 | 厦门大学 | Alpha type ferric oxide and preparation method thereof |
| CN102180522A (en) * | 2011-03-28 | 2011-09-14 | 陕西宏炬电子科技有限公司 | Controllable preparation method of nano magnetic iron oxide with narrow particle size distribution |
Non-Patent Citations (1)
| Title |
|---|
| 董强等: "水热条件下氧化铁纳微粒子的可控合成", 《中国稀土学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108264092A (en) * | 2018-02-09 | 2018-07-10 | 河南理工大学 | A kind of high circulation performance lithium ion battery negative material Fe2O3The preparation method of nanometer needle |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109205567B (en) | Method for preparing metal oxide multilevel structure by utilizing MOF derived bimetallic oxide template | |
| CN105384192B (en) | Method for preparing one-dimensional nanorod self-assembled flower type three-dimensional Nb2O5 | |
| Komarneni et al. | Solvothermal/hydrothermal synthesis of metal oxides and metal powders with and without microwaves | |
| CN102107910A (en) | Preparation method of nano magnesium ferrite | |
| CN104439276B (en) | A kind of quick method and product preparing hollow porous silica/argentum nano composite material | |
| CN105381813A (en) | Preparation method of carbon and nitrogen doped niobium (V) pentoxide nano sheet and application of nano sheet as photocatalyst | |
| CN109399711A (en) | A kind of preparation method of rutile phase hypovanadic oxide nano-powder | |
| CN103204551B (en) | Controllable preparation method of micron-order Fe3O4 | |
| CN101279210B (en) | ZSM-5 molecular sieve film and use thereof in aspect of processing arsenic | |
| CN103204548B (en) | Method of controllably preparing narrow particle size distribution submicron order alpha-FeOOH | |
| Soleimani et al. | Hydrothermal synthesis, structural and catalytic studies of CuBi2O4 nanoparticles | |
| Chen et al. | Microwave hydrothermal synthesis of nanocrystalline rutile | |
| Liu et al. | Large-scale fabrication of H2 (H2O) Nb2O6 and Nb2O5 hollow microspheres | |
| CN100391845C (en) | Method for preparing nano-magnesia by utilizing self-spreading sol-gel method | |
| CN106882842A (en) | A kind of mesoporous petal-shaped ZnCo2O4The preparation method of meter Sized Materials | |
| CN101525155B (en) | Method for preparing manganese sesquioxide one dimension nano material | |
| CN101024510A (en) | Novel method for quickly synthesizing porous nano ZnO powder material by direct deposition process | |
| CN103204550A (en) | Controllable preparation method of micron-order Fe2O3 | |
| CN104227017A (en) | Preparation method of silver nanoparticle with controllable particle size | |
| CN107261860A (en) | A kind of method that sol-gal process prepares metal oxide membrane for water treatment | |
| CN104402050B (en) | D phase hypovanadic oxide nanometer star powder and preparation method thereof | |
| CN106698514A (en) | Preparation method of P-phase VO2 nano-powder | |
| CN108502931A (en) | A kind of preparation method of sea urchin shape FeOOH micro materials | |
| CN103482709A (en) | High-power ultrasound assisted controllable preparation method of nanoscale Fe3O4 powder | |
| CN104045345A (en) | Titanium dioxide and M-phase vanadium dioxide composite nanoparticle and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130717 |