CN105776348A - Simple preparation method for micron-order magnetic alpha-iron trioxide particles - Google Patents
Simple preparation method for micron-order magnetic alpha-iron trioxide particles Download PDFInfo
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- CN105776348A CN105776348A CN201610300123.6A CN201610300123A CN105776348A CN 105776348 A CN105776348 A CN 105776348A CN 201610300123 A CN201610300123 A CN 201610300123A CN 105776348 A CN105776348 A CN 105776348A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 239000002245 particle Substances 0.000 title claims abstract description 22
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 17
- JZQOJFLIJNRDHK-CMDGGOBGSA-N alpha-irone Chemical compound CC1CC=C(C)C(\C=C\C(C)=O)C1(C)C JZQOJFLIJNRDHK-CMDGGOBGSA-N 0.000 title claims abstract description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910052742 iron Inorganic materials 0.000 claims abstract description 14
- 150000001875 compounds Chemical class 0.000 claims abstract description 9
- FRHBOQMZUOWXQL-UHFFFAOYSA-L ammonium ferric citrate Chemical compound [NH4+].[Fe+3].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O FRHBOQMZUOWXQL-UHFFFAOYSA-L 0.000 claims description 4
- 229960004642 ferric ammonium citrate Drugs 0.000 claims description 4
- 235000000011 iron ammonium citrate Nutrition 0.000 claims description 4
- 239000004313 iron ammonium citrate Substances 0.000 claims description 4
- 229960002413 ferric citrate Drugs 0.000 claims description 3
- NPFOYSMITVOQOS-UHFFFAOYSA-K iron(III) citrate Chemical compound [Fe+3].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NPFOYSMITVOQOS-UHFFFAOYSA-K 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 23
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 2
- 239000011147 inorganic material Substances 0.000 abstract description 2
- 239000000696 magnetic material Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000000197 pyrolysis Methods 0.000 abstract 1
- 229910003145 α-Fe2O3 Inorganic materials 0.000 description 17
- 239000000463 material Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 238000009826 distribution Methods 0.000 description 4
- 238000005979 thermal decomposition reaction Methods 0.000 description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 230000005415 magnetization Effects 0.000 description 3
- 239000004570 mortar (masonry) Substances 0.000 description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 2
- 240000007817 Olea europaea Species 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 229960005191 ferric oxide Drugs 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 2
- 230000002787 reinforcement Effects 0.000 description 2
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 229910001448 ferrous ion Inorganic materials 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000007210 heterogeneous catalysis Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- LDHBWEYLDHLIBQ-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide;hydrate Chemical compound O.[OH-].[O-2].[Fe+3] LDHBWEYLDHLIBQ-UHFFFAOYSA-M 0.000 description 1
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 238000007144 microwave assisted synthesis reaction Methods 0.000 description 1
- 239000002077 nanosphere Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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]
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention discloses a simple preparation method for micron-order magnetic alpha-iron trioxide particles, belonging to the technical field of preparation processes of inorganic materials. To satisfy a heavy demand of magnetic materials in technological development and industrialization process, according to the method disclosed by the invention, an organic iron-containing compound is taken as an iron source, the micron-order magnetic alpha-iron trioxide particles which are uniform in size diameter and high in magnetic intensity are prepared by a simple high-temperature pyrolysis method, so that the preparation procedure of the magnetic alpha-iron trioxide is greatly simplified and is easy for industrial production. The method disclosed by the invention is expected to be widely applied in numerous fields, such as energy and chemical industry, environment protection and biotechnology.
Description
Technical field
The invention belongs to technical field of preparation for inorganic material, open one prepares micron order magnetic α-iron sesquioxide particle
Short-cut method.
Technical background
α-iron sesquioxide is a kind of n-type semiconductor, and visible ray shows the response of preferable Optical Electro-Chemistry,
The aspects such as the process of heterogeneous catalysis, sunlight absorbing material, lithium ion battery, chemical sensor and Organic Pollutants in Wastewater
All it is widely used.
At present, the preparation method of magnetic α-iron sesquioxide is more, has microemulsion method, hydro-thermal method, Hydrolyze method, colloidal sol-solidifying
Glue method, chemical precipitation method, pyrolysismethod, Microwave-assisted synthesis method, Radiation Synthesis Method and solid phase method etc..In all these preparations
In method, thermal decomposition method technique is the simplest, and more convenient operation, cost is relatively low, applies wider.Reinforcement very waits Fe (NO3)3·9H2O
Alcoholic solution thermal decomposition, prepared finely dispersed Nano red α-Fe2O3Powder (reinforcement is strange, Li Li, Wang Ling, Wang Wei,
Thermal decomposition process of preparing nano α-Fe2O3, Wuhan University Of Technology's journal, 2001,24 (3): 251-252)；Ma Zhenye etc. with
Fe2(SO4)3·5H2O is source of iron, prepares, by coprecipitation, the submicron alpha-Fe that specific surface area is higher2O3(Ma Zhenye, Li Feng
Raw, bigger serface α-Fe2O3Preparation and catalytic performance research, solid-rocket technology, 2006,29 (4): 286-288)；
Patent also has several preparation α-Fe in addition2O3Method, a kind of is the water generated by co-precipitation with oxalic acid solution with ferrous ion
Conjunction Ferrox. is precursor, then roasting, it is thus achieved that pore-size distribution is narrower, the nanometer α-Fe that specific surface area is higher2O3(Wang Qihua,
Wang Dewei, Wang Tingmei, the preparation method of a kind of α-phase ferricoxide, CN 102649587 A)；One is with FeCl3·6H2O
For source of iron, by solvent thermal decomposition method, prepare α-Fe2O3Nanosphere (Guo Xiaohui, Zhang Ji, a kind of α-Fe2O3Preparation method,
CN 103922421 A)；Also having one is also with FeCl3·6H2O is source of iron, prepares a kind of micron order olive by hydrothermal synthesis method
Olive globular α-Fe2O3Material (Wang Zhiguo, Li Zhijie, Lin Zhijie, a kind of micron order American football shape iron oxide material and preparation side thereof
Method, CN 105129864 A).In a word, at α-Fe2O3In numerous preparation methoies of material, some complicated process of preparation, cost
Height, some use materials are poisonous, harmful, and have produces pollutant etc., many defects in preparation process, hinders preparation method
Extensive application.Therefore α-Fe is explored2O3The greenization of material preparation method, preparation technology simplification imperative.
Summary of the invention
It is an object of the invention to provide a kind of micron order magnetic α-Fe2O3Simple and convenient process for preparing, expand α-Fe2O3's
Range of application.The organic iron containing compounds ground is put in Muffle furnace, by high-temperature roasting, lower the temperature, cool down after obtain granularity
Uniform micron order magnetic α-iron sesquioxide particle.
The concrete operation method of the present invention includes following key step:
1) organic iron containing compounds is ground to certain particle size, puts into crucible, be then placed in Muffle furnace；
2) with certain programming rate under oxygen or air atmosphere by step 1) in Muffle furnace rise to 500-800 DEG C,
Insulation 2-6h, then allows Muffle furnace naturally be down to room temperature；
3) by step 2) in crucible after cooling take out, obtain having micron order magnetic α-three oxidation two of uniform particle size
Iron particle.
Organic iron containing compounds mentioned by the present invention can be the one in ferric citrate or ferric ammonium citrate.
Iron containing compounds sample granularity mentioned by the present invention is less than 100 mesh.
Programming rate mentioned by the present invention is 1-10 DEG C/min.
The major advantage of preparation method involved in the present invention: be that preparation technology is very simple, so can significantly contract
Short preparation time.Through micron order magnetic α-Fe prepared by this method2O3Particle, even particle size distribution, mean diameter is 1.3 μm,
Saturation magnetization is 19.52eum/g.
Accompanying drawing explanation
Magnetic α-the Fe of preparation in Fig. 1: embodiment 12O3The x-ray diffraction pattern of particle.
Magnetic α-the Fe of preparation in Fig. 2: embodiment 12O3The grain size distribution of particle.
Magnetic α-the Fe of preparation in Fig. 3: embodiment 12O3The hysteresis curve figure of particle.
Detailed description of the invention
Following embodiment is further illustrating rather than limiting the scope of the present invention of the present invention.
Embodiment 1
2g ferric ammonium citrate is put in mortar and grind, put into crucible, place in Muffle furnace, with 10 DEG C/min's
Programming rate rises to 550 DEG C from room temperature under air conditions, is incubated 3h, then naturally cools to room temperature, obtain micron order magnetic
α-Fe2O3Sample, its mean diameter is 1.3 μm, and saturation magnetization is 19.52emu/g.
From Fig. 1 it can be seen that preparation magnetic α-Fe2O3The X-ray diffraction of particle occurs in the range of 20-80 °
Diffraction maximum, respectively corresponding (012), (104), (110), (006), (113), (202), (024), (116), (018),
(214), (300), (208), (1010), (220) and (036) peak, be α-Fe2O3Absworption peak, illustrate by this method
The material of preparation is typical α-Fe2O3Magnetic material；From Fig. 2 it can be seen that preparation α-Fe2O3The particle diameter distribution of particle
Narrower, mean diameter concentrates on about 1.3 μm；From Fig. 3 it can be seen that preparation α-Fe2O3The magnetic hysteresis loop tool of particle
Having narrower Magnetic hysteresis ring, its saturation magnetization is 19.52emu/g.
Embodiment 2
2g ferric citrate granule is ground in mortar, puts into crucible, place in Muffle furnace, with 10 DEG C/min's
Programming rate rises to 650 DEG C from room temperature under air conditions, is incubated 2h, then naturally cools to room temperature, obtain micron order magnetic
α-Fe2O3Sample.
Embodiment 3
3g ferric ammonium citrate granule is ground in mortar, puts into crucible, place in Muffle furnace, with 5 DEG C/min's
Programming rate rises to 600 DEG C from room temperature under air conditions, is incubated 4h, then naturally cools to room temperature, obtain micron order magnetic
α-Fe2O3Sample.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, those skilled in the art can
So that the raw material used in the present invention and proportioning are modified without departing from the spirit and scope of the present invention.So, if originally
These variations of invention belong within the scope of the claims in the present invention and equivalent technologies thereof, then the present invention is also intended to comprise these and changes
Including moving.
Claims (5)
1. the simple and convenient process for preparing of micron order magnetic α-iron sesquioxide particle, it is characterised in that:
The organic iron containing compounds ground is put in Muffle furnace, by high-temperature roasting, lower the temperature, cool down after obtain even-grained
Micron order magnetic α-iron sesquioxide particle.
2. the preparation method as described in right 1 requires, it is characterised in that comprise the steps:
1) organic iron containing compounds is ground to certain particle size, puts into crucible, be then placed in Muffle furnace；
2) with certain programming rate, by step 1 under oxygen or air atmosphere) in Muffle furnace rise to 500-800 DEG C, protect
Temperature 2-6h, then allows Muffle furnace naturally be down to room temperature；
3) by step 2) in cooling after crucible take out, obtain even-grained micron order magnetic α-iron sesquioxide particle.
3. the preparation method as described in right 1 or 2 requires, it is characterised in that above-mentioned mentioned organic iron containing compounds can be
One in ferric citrate or ferric ammonium citrate.
4. the preparation method as described in right 1 or 2 requires, it is characterised in that above-mentioned mentioned iron containing compounds sample granularity is low
In 100 mesh.
5. the preparation method as described in right 1 or 2 requires, it is characterised in that above-mentioned mentioned programming rate is 1-10 DEG C/min.
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| CN201610300123.6A CN105776348A (en) | 2016-05-03 | 2016-05-03 | Simple preparation method for micron-order magnetic alpha-iron trioxide particles |
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| CN201610300123.6A CN105776348A (en) | 2016-05-03 | 2016-05-03 | Simple preparation method for micron-order magnetic alpha-iron trioxide particles |
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| CN105776348A true CN105776348A (en) | 2016-07-20 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107746081A (en) * | 2017-11-10 | 2018-03-02 | 河南理工大学 | A kind of preparation method of two-dimensional nano piece form α Fe2O3 materials |
| CN111499370A (en) * | 2020-05-20 | 2020-08-07 | 中国科学院重庆绿色智能技术研究院 | Preparation method of coated ferromagnetic material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101898749B (en) * | 2010-08-02 | 2014-07-02 | 武汉理工大学 | Method for preparing metal oxide hollow particles or fibers |
-
2016
- 2016-05-03 CN CN201610300123.6A patent/CN105776348A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101898749B (en) * | 2010-08-02 | 2014-07-02 | 武汉理工大学 | Method for preparing metal oxide hollow particles or fibers |
Non-Patent Citations (1)
| Title |
|---|
| 严新: "固相法制备氧化铁纳米粒子", 《盐城工学院学报（自然科学版）》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107746081A (en) * | 2017-11-10 | 2018-03-02 | 河南理工大学 | A kind of preparation method of two-dimensional nano piece form α Fe2O3 materials |
| CN107746081B (en) * | 2017-11-10 | 2019-06-18 | 河南理工大学 | A kind of two-dimensional nano piece form α-Fe2O3The preparation method of material |
| CN111499370A (en) * | 2020-05-20 | 2020-08-07 | 中国科学院重庆绿色智能技术研究院 | Preparation method of coated ferromagnetic material |
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Application publication date: 20160720 |