CN104229900B - A kind of α-Fe 2o 3the preparation method of cubic block - Google Patents
A kind of α-Fe 2o 3the preparation method of cubic block Download PDFInfo
- Publication number
- CN104229900B CN104229900B CN201410467136.3A CN201410467136A CN104229900B CN 104229900 B CN104229900 B CN 104229900B CN 201410467136 A CN201410467136 A CN 201410467136A CN 104229900 B CN104229900 B CN 104229900B
- Authority
- CN
- China
- Prior art keywords
- cubic block
- preparation
- urea
- molysite
- alcohol
- 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.)
- Expired - Fee Related
Links
Landscapes
- Compounds Of Iron (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of α-Fe
2o
3the preparation method of cubic block, comprises the following steps: take molysite as source of iron, urea is hydroxide ion initiator, join in alcoholic solvent, stirs and raw material is mixed, obtain the precursor liquid of solvent thermal reaction; Precursor liquid is heated to 180-220 DEG C, and insulation 6-36h reacts; Centrifugal after product cooling, the sediment-filled phase washing of gained, after washing, drying obtains the α-Fe that the controlled length of side of size is 0.1-1.0 μm
2o
3cubic block.Preparation method provided by the invention, low raw-material cost, preparation process is simple, by changing additional proportion and concentration, temperature of reaction and the soaking time of molysite and urea, can obtain the α-Fe of the different length of side
2o
3cubic block, in reaction process, nucleation easily controls, and the productive rate of product is high, can realize micro/nano level α-Fe
2o
3the extensive synthesis of cubic block.
Description
Technical field
The present invention relates to a kind of α-Fe of technical field of chemical engineering
2o
3the preparation method of cubic block, especially relates to the α-Fe that a kind of length of side is controlled
2o
3the preparation method of cubic block.
Background technology
Ferric oxide is the important transition metal oxide material of a class, there is the advantages such as nontoxicity, cheap, good stability, physical and chemical performance are good, range of application is very extensive, can be used as sensitive material, catalytic material, making optics and electron device, magnetic recording material etc., cause the research interest of people.And α-Fe
2o
3be the most stable phase of thermodynamics of ferric oxide, its energy gap is 2.1eV, has larger specific surface area, demonstrates excellent characteristic in catalysis, biological medicine engineering, air-sensitive etc.
In recent years, the α-Fe of various micro-nano-scale has been prepared by the liquid phase of different system or gas-phase synthesizing method
2o
3material, comprises micro-nano granules, micro-nano mitron, cubic block, bar-shaped, the special appearance such as plate-like, needle-like, dendroid.Wherein, both at home and abroad about the α-Fe of varying particle size
2o
3the report of cubic block is also few." α-the Fe of Copper-cladding Aluminum Bar of PengSun, ChenWang, XinZhou etc.
2o
3sheet cubes: synthesis and gas-sensitive property " (Cu-doped α-Fe
2o
3hierarchicalmicrocubes:synthesisandgassensingproperties. SensorsandActuatorsB:Chemical, 2014,193:616-622) with iron(ic) chloride, urotropin for raw material, as solvent after the mixing of second alcohol and water, solvent-thermal method is utilized to synthesize at 160 DEG C of insulation 12h the α-Fe that the length of side is 1.2 μm
2o
3cubic block.ChunyangYin, ManickamMinakshi, DavidE.Ralph etc. " take glycine as raw material, water heat transfer cubes α-Fe
2o
3particle: Surface Characterization, reaction mechanism and electrochemical activity " (Hydrothermalsynthesisofcubic α-Fe
2o
3microparticlesusingglycine:surfacecharacterization, reactionmechanismandelectrochemicalactivity.2011,509,9821-9825) with iron(ic) chloride, glycine for raw material, water, as solvent, utilizes hydrothermal method to synthesize 160 DEG C of insulation for some time the α-Fe that the length of side is 0.3-1.3 μm
2o
3cubic block.But in prior art, synthesis α-Fe
2o
3expensive raw material price and large mainly with water as solvent, size regulating effect is not good.
Present stage, usually adopt hydro-thermal or solvent-thermal process legal system for the α-Fe of different size
2o
3cubic block structure, due to the restriction of differential responses system, raw materials cost is higher, the productive rate of product is on the low side, size regulating effect is not good.Therefore, study the high and controlled effective preparation method of size of a kind of productive rate simple to operate, reproducible, low raw-material cost, product, seem particularly important.
Summary of the invention
The present invention is directed to the problems referred to above, provide the α-Fe that a kind of productive rate simple to operate, reproducible, low raw-material cost, product is high, can realize having different size dimension
2o
3the controlledly synthesis of cubic block.
Technical scheme of the present invention is:
A kind of α-Fe
2o
3the preparation method of cubic block, is characterized in that, comprises the following steps:
A. be source of iron with molysite, urea is hydroxide ion initiator, source of iron and urea are joined in alcohol, by stirring, raw material being mixed, obtaining the precursor liquid of solvent thermal reaction;
B. moved in reactor by above-mentioned precursor liquid, be heated to 180-220 DEG C, insulation 6-36h carries out solvent thermal reaction;
C. by centrifugal after above-mentioned reacted product cooling, the sediment-filled phase of gained is washed, and after washing, drying obtains α-Fe
2o
3cubic block.
In described step a, molysite and urea mol ratio are 1:7-16, and the concentration of molysite in alcohol is 0.06-0.15mol/L.
Molysite in described step a is iron halide or iron nitrate.
Alcohol in described step a is ethanol or propyl alcohol.
α-Fe in described step c
2o
3the length of side of cubic block is 0.1-1.0 μm.
The present invention prepares α-Fe by solvent-thermal method
2o
3cubic block tool has the following advantages:
1. the present invention is hydroxide ion initiator with urea in solvent thermal reaction process, adopt alcohol as solvent, avoid the use of toxic substance and cost is low, each raw material can be mixed uniformly without the need to carrying out other operations, simple to operate, using alcohol as solvent, the control to Product size better can be realized.
2. reproducible, low raw-material cost, product the productive rate of the present invention high, can accomplish scale production;
3. the present invention is by the concentration of the additional proportion and molysite that change molysite and urea, temperature of reaction and soaking time, can to α-Fe
2o
3cubic block size dimension controls, the α-Fe of synthesis 0.1-1.0 μm of mass-producing
2o
3cubic block.
Accompanying drawing explanation
Fig. 1 is α-Fe prepared by the embodiment of the present invention 2
2o
3scanning electron microscope (SEM) picture of cubic block.
Fig. 2 is α-Fe prepared by the embodiment of the present invention 3
2o
3scanning electron microscope (SEM) picture of cubic block.
Fig. 3 is α-Fe prepared by the embodiment of the present invention 4
2o
3x-ray diffraction (XRD) collection of illustrative plates of cubic block.
Fig. 4 is α-Fe prepared by the embodiment of the present invention 4
2o
3scanning electron microscope (SEM) picture of cubic block.
Fig. 5 is α-Fe prepared by the embodiment of the present invention 8
2o
3scanning electron microscope (SEM) picture of cubic block.
Fig. 6 is scanning electron microscope (SEM) picture of the sample of comparative example 1 of the present invention preparation.
Embodiment
Below by embodiment, the present invention will be further elaborated, and following explanation has been only explanation the present invention, do not limit its content.
embodiment 1
The Fe(NO3)39H2O of 1.010g, the urea of 1.100g join in 17mL propanol solvent by 1, stir and obtain clear solution;
Above-mentioned solution is transferred in reactor by 2, at 180 DEG C, react 10h;
3 products are after centrifugation and washing, and drying obtains the α-Fe that the length of side is 0.14-0.19 μm
2o
3cubic block.
embodiment 2
The ferric chloride hexahydrate of 0.676g, the urea of 1.200g join in 25mL alcohol solvent by 1, stir and obtain clear solution;
Above-mentioned solution is transferred in reactor by 2, at 200 DEG C, react 16h;
3 products are after centrifugation and washing, and drying obtains the α-Fe that the length of side is 0.31-0.44 μm
2o
3cubic block, as shown in Figure 1.
embodiment 3
The ferric chloride hexahydrate of 0.676g, the urea of 1.800g join in 25mL alcohol solvent by 1, stir and obtain clear solution;
Above-mentioned solution is transferred in reactor by 2, at 200 DEG C, react 16h;
3 products are after centrifugation and washing, and drying obtains the α-Fe that the length of side is 0.45-0.53 μm
2o
3cubic block, as shown in Figure 2.
embodiment 4
The ferric chloride hexahydrate of 0.676g, the urea of 1.500g join in 25mL alcohol solvent by 1, stir and obtain clear solution;
Above-mentioned solution is transferred in reactor by 2, at 200 DEG C, react 16h;
3 products are after centrifugation and washing, and drying obtains α-Fe
2o
3cubic block.Respectively as shown in Figures 3 and 4, result shows α-Fe for the microscopic appearance of product and phase structure
2o
3the length of side of cubic block is 0.48-0.70 μm, and X-ray diffraction peak value and JCPDS card (33-0664) are consistent, and product is α-Fe
2o
3phase.
embodiment 5
The ferric chloride hexahydrate of 0.676g, the urea of 1.650g join in 35mL propanol solvent by 1, stir and obtain clear solution;
Above-mentioned solution is transferred in reactor by 2, at 190 DEG C, react 33h;
3 products are after centrifugation and washing, and drying obtains the α-Fe that the length of side is 0.67-0.75 μm
2o
3cubic block.
embodiment 6
The Fe(NO3)39H2O of 1.010g, the urea of 1.400g join in 40mL propanol solvent by 1, stir and obtain clear solution;
Above-mentioned solution is transferred in reactor by 2, at 220 DEG C, react 30h;
3 products are after centrifugation and washing, and drying obtains the α-Fe that the length of side is 0.87-0.95 μm
2o
3cubic block.
embodiment 7
The Fe(NO3)39H2O of 1.010g, the urea of 2.000g join in 18mL alcohol solvent by 1, stir and obtain clear solution;
Above-mentioned solution is transferred in reactor by 2, at 200 DEG C, react 7h;
3 products are after centrifugation and washing, and drying obtains the α-Fe that the length of side is 0.52-0.64 μm
2o
3cubic block.
embodiment 8
The ferric chloride hexahydrate of 0.676g, the urea of 2.100g join in 25mL alcohol solvent by 1, stir and obtain clear solution;
Above-mentioned solution is transferred in reactor by 2, at 200 DEG C, react 16h;
3 products are after centrifugation and washing, and drying obtains the α-Fe that the length of side is 0.40-0.48 μm
2o
3cubic block, as shown in Figure 5.
embodiment 9
The Fe(NO3)39H2O of 1.010g, the urea of 2.390g join in 28mL propanol solvent by 1, stir and obtain clear solution;
Above-mentioned solution is transferred in reactor by 2, at 180 DEG C, react 23h;
3 products are after centrifugation and washing, and drying obtains the α-Fe that the length of side is 0.52-0.61 μm
2o
3cubic block.
comparative example 1
The ferric chloride hexahydrate of 0.676g, the urea of 0.900g join in 25mL alcohol solvent by 1, stir and obtain clear solution;
Above-mentioned solution is transferred in reactor by 2, at 200 DEG C, react 16h;
3 products are after centrifugation and washing, and drying obtains the hollow microsphere structure that diameter is 2.2-2.8 μm, and as shown in Figure 6, its structural unit mostly is Ellipsoid shaped particle.
comparative example 2
The Fe(NO3)39H2O of 1.010g, the urea of 3.050g join in 20mL propanol solvent by 1, stir and obtain clear solution;
Above-mentioned solution is transferred in reactor by 2, at 180 DEG C, react 4h;
3 products are after centrifugation and washing, and drying obtains product, and the sample of synthesis is irregular particle, and without special appearance, particle size distribution range is large.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not by the restriction of embodiment; other is any do not deviate from spirit of the present invention and principle under make change, modification, combination, substitute, simplify and all should be equivalent substitute mode, be included within protection scope of the present invention.
Claims (4)
1. a α-Fe
2o
3the preparation method of cubic block, is characterized in that, comprises the following steps:
A. be source of iron with molysite, urea is hydroxide ion initiator, source of iron and urea are joined in alcohol according to mol ratio 1:7.32-15.92, the concentration of molysite in alcohol is 0.0625-0.147mol/L, by stirring, raw material being mixed, obtaining the precursor liquid of solvent thermal reaction;
B. moved in reactor by above-mentioned precursor liquid, be heated to 180-220 DEG C, insulation 7-33h carries out solvent thermal reaction;
C. by centrifugal after above-mentioned reacted product cooling, the sediment-filled phase of gained is washed, and after washing, drying obtains α-Fe
2o
3cubic block.
2. preparation method according to claim 1, is characterized in that: the molysite in step a is iron halide or iron nitrate.
3. preparation method according to claim 1, is characterized in that: the alcohol in step a is ethanol or propyl alcohol.
4. preparation method according to claim 1, is characterized in that: α-Fe in step c
2o
3the length of side of cubic block is 0.1-1.0 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410467136.3A CN104229900B (en) | 2014-09-15 | 2014-09-15 | A kind of α-Fe 2o 3the preparation method of cubic block |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410467136.3A CN104229900B (en) | 2014-09-15 | 2014-09-15 | A kind of α-Fe 2o 3the preparation method of cubic block |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104229900A CN104229900A (en) | 2014-12-24 |
| CN104229900B true CN104229900B (en) | 2015-12-30 |
Family
ID=52218923
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410467136.3A Expired - Fee Related CN104229900B (en) | 2014-09-15 | 2014-09-15 | A kind of α-Fe 2o 3the preparation method of cubic block |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104229900B (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106698522B (en) * | 2016-09-13 | 2018-03-30 | 济南大学 | A kind of α Fe2O3The preparation method of cubic block and micron ball |
| CN107265509A (en) * | 2017-06-19 | 2017-10-20 | 华南理工大学 | A kind of cubic nano-sized iron oxide and preparation method thereof |
| CN107356635A (en) * | 2017-07-13 | 2017-11-17 | 济南大学 | A kind of NiO nanometer sheets/α Fe applied to gas sensor2O3Nanocube heterojunction material |
| CN107698304A (en) * | 2017-09-22 | 2018-02-16 | 芜湖新达园林绿化集团有限公司 | One kind sustained release and good in economic efficiency epipremnum aureum dedicated fertilizer |
| CN107758748A (en) * | 2017-11-28 | 2018-03-06 | 合肥学院 | A kind of polyhedron di-iron trioxide and preparation method thereof |
| CN112897593B (en) * | 2020-11-04 | 2023-03-10 | 河南海宏科技有限公司 | Regular polyhedral alpha-Fe 2 O 3 Method for preparing self-growing material |
| CN112408494B (en) * | 2020-11-27 | 2022-09-06 | 台州学院 | Preparation method of small-size ferric oxide cube |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101041470A (en) * | 2007-03-23 | 2007-09-26 | 清华大学 | Method for synthesizing block-shaped alpha-ferric oxide nanostructure |
-
2014
- 2014-09-15 CN CN201410467136.3A patent/CN104229900B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101041470A (en) * | 2007-03-23 | 2007-09-26 | 清华大学 | Method for synthesizing block-shaped alpha-ferric oxide nanostructure |
Non-Patent Citations (1)
| Title |
|---|
| Surface-enhanced Raman scattering of 4-mercaptopyridine on sub-monolayers of α-Fe2O3 nanocrystals (sphere, spindle, cube);Xiaoqi Fu等;《J. Raman Spectrosc.》;20090408;第1290-1295页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104229900A (en) | 2014-12-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104229900B (en) | A kind of α-Fe 2o 3the preparation method of cubic block | |
| CN104211127B (en) | A kind of α-Fe 2o 3the preparation method of hollow microsphere | |
| Ghasemzadeh et al. | Fe3O4@ SiO2–NH2 core-shell nanocomposite as an efficient and green catalyst for the multi-component synthesis of highly substituted chromeno [2, 3-b] pyridines in aqueous ethanol media | |
| Moavi et al. | Algal magnetic nickel oxide nanocatalyst in accelerated synthesis of pyridopyrimidine derivatives | |
| Rahimi-Nasrabadi et al. | Influence of capping agents additives on morphology of CeVO 4 nanoparticles and study of their photocatalytic properties | |
| CN103058283B (en) | Preparation method of iron oxides with adjustable size, appearance and compositions | |
| CN103337327B (en) | Heterogeneous Fe3O4/ Co metal-organic framework materials and its preparation method and application | |
| CN106986611A (en) | A kind of preparation method of reguline metal sulfide aeroge | |
| CN105399150B (en) | Sour nickel nano material of a kind of cobalt and its preparation method and application | |
| Cheng et al. | Thermal analysis and infrared emission spectroscopic study of kaolinite–potassium acetate intercalate complex | |
| Khan et al. | Synthesis of ferric oxyhydroxide nanoparticles and ferric oxide nanorods by reflux assisted coprecipitation method and comparative study of their thermal properties | |
| Mosleh et al. | Sonochemical synthesis and characterization of cerium vanadate nanoparticles and investigation of its photocatalyst application | |
| CN107500303A (en) | A kind of mesoporous magnesium silicate microballoon and its hydro-thermal thermal transition preparation method | |
| CN105858733A (en) | Cobaltosic oxide nano flower of multihole hierarchical structure and preparation method thereof | |
| CN105110381A (en) | Method for preparing nanopore alpha-Fe2O3 | |
| Yuan et al. | Preparation of a novel, efficient, and recyclable magnetic catalyst, Cu (II)-OHPC-Fe3O4 nanoparticles, and a solvent-free protocol for the synthesis of coumarin derivatives | |
| CN101863485A (en) | Preparation method for hollow silicate | |
| CN104927760B (en) | A kind of magnetic heterojunction structure fiber and preparation method and application | |
| CN105800693B (en) | A kind of preparation method of α FeOOH three-dimensional multistage microballoons | |
| CN102328960B (en) | Synthesis method of trimanganese tetroxide material with 3D (three-dimensional) flower-shaped structure | |
| CN107188189A (en) | A kind of flower-shaped earth silicon material of porous hierarchical structure and preparation method thereof | |
| CN107043133B (en) | Flower-shaped γ Fe2O3The preparation method of microballoon | |
| Kizilca et al. | Kinetic investigation of reaction between colemanite ore and methanol | |
| CN105948135A (en) | Monodisperse porous magnetic submicrosphere and preparation method thereof | |
| Sadeghzadeh et al. | Sonochemical syntheses and characterization of a new nano-sized 2-D lead (II) coordination polymer as precursor for preparation of PbBr (OH) nano-structure |
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 | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20151230 Termination date: 20210915 |