CN102923787A - Method for preparing gamma-Fe2O3 nano particle powder - Google Patents
Method for preparing gamma-Fe2O3 nano particle powder Download PDFInfo
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- CN102923787A CN102923787A CN2012104432683A CN201210443268A CN102923787A CN 102923787 A CN102923787 A CN 102923787A CN 2012104432683 A CN2012104432683 A CN 2012104432683A CN 201210443268 A CN201210443268 A CN 201210443268A CN 102923787 A CN102923787 A CN 102923787A
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- Prior art keywords
- gamma
- particle powder
- nano particle
- ethylene glycol
- iron acetate
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- 239000002105 nanoparticle Substances 0.000 title claims abstract description 28
- 239000000843 powder Substances 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title abstract description 9
- 229910006297 γ-Fe2O3 Inorganic materials 0.000 title abstract 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 50
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 18
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 12
- 239000000047 product Substances 0.000 claims abstract description 10
- 230000032683 aging Effects 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 239000012065 filter cake Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000000967 suction filtration Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052742 iron Inorganic materials 0.000 claims abstract description 4
- 229910001566 austenite Inorganic materials 0.000 claims description 18
- 239000000725 suspension Substances 0.000 claims description 14
- 238000013019 agitation Methods 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 11
- 235000017550 sodium carbonate Nutrition 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 abstract description 5
- 239000002245 particle Substances 0.000 abstract description 5
- 239000000919 ceramic Substances 0.000 abstract description 3
- 239000011248 coating agent Substances 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract description 3
- 239000004033 plastic Substances 0.000 abstract description 3
- 229920003023 plastic Polymers 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 abstract 1
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 238000000227 grinding Methods 0.000 abstract 1
- 239000000696 magnetic material Substances 0.000 abstract 1
- 239000012716 precipitator Substances 0.000 abstract 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 23
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 7
- 239000000463 material Substances 0.000 description 4
- 239000000049 pigment Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910000859 α-Fe Inorganic materials 0.000 description 3
- 239000001034 iron oxide pigment Substances 0.000 description 2
- 239000002932 luster Substances 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000000176 photostabilization Effects 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 235000010215 titanium dioxide Nutrition 0.000 description 1
Abstract
The invention provides a method for preparing gamma-Fe2O3 nano particle powder. By means of the method, gamma-Fe2O3 nano particles are prepared with iron acetate as the iron source, ethanediol as the dispersing agent and sodium carbonate as the precipitator. The method includes: grinding the iron acetate, and adding the iron acetate into the ethanediol solution to obtain turbid liquid; adding the sodium carbonate solution into the turbid liquid dropwise, continuing stirring for ageing after the dropwise adding is finished, standing for cooling the solution to the room temperature, performing suction filtration, and washing through deionized water and ethanol alternatively; and drying the obtained filter cakes to obtain the prepared gamma-Fe2O3 nano particle powder. The obtained gamma-Fe2O3 nano particle powder is stable in chemical property and high in catalytic activity, has good light resistance, weather resistance and shielding resistance on ultraviolet and can be widely used in the aspects of fine ceramics, plastic products, coating, catalysts, magnetic materials, biomedical engineering and the like. The method for preparing gamma-Fe2O3 nano particle powder is short in technological process, good in operation environment, high in product quality, superfine and even in particle, good in dispersibility and the like.
Description
Technical field
The present invention relates to a kind of γ-Fe
2O
3The preparation method of nanoparticle powder belongs to technical field of nano material.
Background technology
Ferric oxide is important ceramic, is widely used as magnetic pipe recording material, soft magnetic ferrite, rumbling compound and pigment.Very extensive in the range of application aspect pigment, the consumption of whole world iron oxide pigment surpasses 100t, is only second to titanium white, occupies the second of mineral dye.Present most widely used ferric oxide is Fe
3O
4, γ-Fe
2O
3And α-Fe
2O
3, γ-Fe wherein
2O
3And Fe
3O
4Have magnetic, often be used as the magnetic raw material, but because the ferric oxide of traditional method preparation is subjected to the impact of the low and unstable properties of self magnetic, application is very limited, and generally is used for low grade products.
The appearance of nanotechnology for ferric oxide has injected new vitality, further enlarges its range of application.On the one hand, the magnetic Nano iron oxide particles is because its special superparamagnetism, thereby has broad application prospects at aspects such as giant magnetoresistance, magnetic liquid and magnetic recording, soft magnetism, permanent magnetism, magnetic cooling, giant magnetoimpedance material and magnetic-optic devices, magnetic detectors.On the other hand, when nano-sized iron oxide is used as pigment, have the good transparency, in pigment, again it is called transparent ferric oxide.It is except the characteristics such as fast light, corrosion-resistant, nontoxic with common iron oxide pigment, also have high dispersive, color and luster more bright-coloured, ultraviolet ray is had the characteristics such as good absorption and shielding effect, can be widely used in the industries such as luster coating, printing ink, plastics, leather, automobile finish, electronics, optical polish agent and medicine.Discovered in recent years with the nano-powder sintering that iron nickel mixes with ferric oxide, can substitute precious metal and make car tail gas purificant; Nano-sized iron oxide is made gas sensor, then have very high sensitivity.
γ-Fe as magnetic recording material
2O
3Be shaped as aciculiform, and require its long and short footpath than large, this shape has guaranteed that magnetized preferred orientation is consistent with major axis.In general, particle is less, and needle-like is better, and coercive force is also just higher.Because the coercive force of all used particles has comprised different property and crystal anisotropy in the record.Nano-sized iron oxide is the New Magnetic Field Controlled recording materials, and excellent performance is being arranged aspect the high magnetic recording density, and recording density is about 10 times of common ferric oxide.Utilize the Magnetic Sensor of the giant magnetoresistance effect preparation of iron-based nano material to come out, the magnetic liquid that has coated the super-paramagnetism nano particulate also extensively is used in aerospace and the part civil area seals as long-life dynamic rotary.Soft magnetic ferrite at radio communication, broadcast television, automatically control space travel, radar navigation, metrical instrument, computer, printing, household electrical appliance and biomedical sector and all be widely applied.
Along with the development of nanometer synthetic technology, the preparation method of nano-sized iron oxide also constantly updates.But realize suitability for industrialized production, still need to solve some core technology difficult problems, such as equipment, processing condition, productive rate etc.Therefore, the research of nano-sized iron oxide should mainly be considered: the 1) dispersiveness of nano-sized iron oxide, surface modification and morphology control; 2) preparation of the nano-sized iron oxide of low cost, high yield.
Summary of the invention
For overcoming the defective of the aspects such as processing condition, productive rate, the invention provides a kind of γ of preparation-Fe
2O
3The method of nanoparticle powder realizes by following technical proposal.
A kind of γ-Fe
2O
3The preparation method of nanoparticle powder is with iron acetate (Fe (CH
3COO)
3) be that source of iron, ethylene glycol are dispersion agent, yellow soda ash (Na
2CO
3) prepare γ-Fe for precipitation agent
2O
3Nanoparticle, concrete steps are as follows:
(1) iron acetate is ground behind 300～800 ℃ of lower roasting 2～6h, then with under 80～160 ℃ and the agitation condition, join in the ethylene glycol solution, obtain suspension liquid;
(2) compound concentration is the sodium carbonate solution of 0.1～0.8mol/L, is added drop-wise under agitation condition in the suspension liquid of step (1) gained, is added dropwise to complete rear continuation and stirs aging 2h;
(3) after being cooled to room temperature, step (2) gained solution left standstill carries out suction filtration, with deionized water and ethanol exchange washing;
(4) step (3) gained filter cake is carried out freeze-day with constant temperature 10～24h with 110～120 ℃, namely get prepared product γ-Fe
2O
3The nanoparticle powder.
It is to be 2～4 ︰, 1 addings by the mol ratio by iron acetate and ethylene glycol that described step (1) adds ethylene glycol.
It is to be that 1 ︰ 1 adds by volume that described step (2) sodium carbonate solution adds suspension liquid.
The advantage that the present invention possesses and effect: gained γ-Fe
2O
3Stable chemical nature, catalytic activity are high, have good photostabilization, weathering resistance and to ultraviolet shielding, are widely used at aspects such as fine ceramics, plastics, coating, catalyzer, magneticsubstance and medical science and biotechnology.Preparation method's technical process that the present invention proposes is short, good operational environment, and quality product is high, the characteristics such as particle is ultra-fine, even, good dispersity.
Embodiment
The present invention will be further described below by embodiment.
Embodiment 1
(1) the 11.65g iron acetate being ground behind 300 ℃ of lower roasting 6h, then place constant temperature oil bath with under 80 ℃ and the agitation condition, is that 2 ︰ 1 join in the ethylene glycol solution by the mol ratio of iron acetate and ethylene glycol, obtains suspension liquid;
(2) compound concentration is the sodium carbonate solution of 0.1mol/L, is that 1 ︰ 1 is added drop-wise in the suspension liquid of step (1) gained by volume under agitation condition, is added dropwise to complete rear continuation and stirs aging 2h;
(3) after being cooled to room temperature, step (2) gained solution left standstill carries out suction filtration, with deionized water and ethanol exchange washing;
(4) place thermostatic drying chamber to carry out freeze-day with constant temperature 10h with 110 ℃ step (3) gained filter cake, namely get prepared product γ-Fe
2O
3The nanoparticle powder.
Embodiment 2
(1) the 11.65g iron acetate being ground behind 500 ℃ of lower roasting 4h, then place constant temperature oil bath with under 120 ℃ and the agitation condition, is that 3 ︰ 1 join in the ethylene glycol solution by the mol ratio of iron acetate and ethylene glycol, obtains suspension liquid;
(2) compound concentration is the sodium carbonate solution of 0.4mol/L, is that 1 ︰ 1 is added drop-wise in the suspension liquid of step (1) gained by volume under agitation condition, is added dropwise to complete rear continuation and stirs aging 2h;
(3) after being cooled to room temperature, step (2) gained solution left standstill carries out suction filtration, with deionized water and ethanol exchange washing;
(4) place thermostatic drying chamber to carry out freeze-day with constant temperature 104h with 1104 ℃ step (3) gained filter cake, namely get prepared product γ-Fe
2O
3The nanoparticle powder.
Embodiment 3
(1) the 22.3g iron acetate being ground behind 600 ℃ of lower roasting 3h, then place constant temperature oil bath with under 140 ℃ and the agitation condition, is that 4 ︰ 1 join in the ethylene glycol solution by the mol ratio of iron acetate and ethylene glycol, obtains suspension liquid;
(2) compound concentration is the sodium carbonate solution of 0.6mol/L, is that 1 ︰ 1 is added drop-wise in the suspension liquid of step (1) gained by volume under agitation condition, is added dropwise to complete rear continuation and stirs aging 2h;
(3) after being cooled to room temperature, step (2) gained solution left standstill carries out suction filtration, with deionized water and ethanol exchange washing;
(4) place thermostatic drying chamber to carry out freeze-day with constant temperature 24h with 115 ℃ step (3) gained filter cake, namely get prepared product γ-Fe
2O
3The nanoparticle powder.
Embodiment 4
(1) the 22.3g iron acetate being ground behind 800 ℃ of lower roasting 2h, then place constant temperature oil bath with under 160 ℃ and the agitation condition, is that 2 ︰ 1 join in the ethylene glycol solution by the mol ratio of iron acetate and ethylene glycol, obtains suspension liquid;
(2) compound concentration is the sodium carbonate solution of 0.8mol/L, is that 1 ︰ 1 is added drop-wise in the suspension liquid of step (1) gained by volume under agitation condition, is added dropwise to complete rear continuation and stirs aging 2h;
(3) after being cooled to room temperature, step (2) gained solution left standstill carries out suction filtration, with deionized water and ethanol exchange washing;
(4) place thermostatic drying chamber to carry out freeze-day with constant temperature 18h with 120 ℃ step (3) gained filter cake, namely get prepared product γ-Fe
2O
3The nanoparticle powder.
Claims (3)
1. γ-Fe
2O
3The preparation method of nanoparticle powder is characterized in that: take iron acetate as source of iron, ethylene glycol prepares γ-Fe as dispersion agent, yellow soda ash as precipitation agent
2O
3Nanoparticle, concrete steps are as follows:
(1) iron acetate is ground behind 300～800 ℃ of lower roasting 2～6h, then with under 80～160 ℃ and the agitation condition, join in the ethylene glycol solution, obtain suspension liquid;
(2) compound concentration is the sodium carbonate solution of 0.1～0.8mol/L, is added drop-wise under agitation condition in the suspension liquid of step (1) gained, is added dropwise to complete rear continuation and stirs aging 2h;
(3) after being cooled to room temperature, step (2) gained solution left standstill carries out suction filtration, with deionized water and ethanol exchange washing;
(4) step (3) gained filter cake is carried out freeze-day with constant temperature 10～24h with 110～120 ℃, namely get prepared product γ-Fe
2O
3The nanoparticle powder.
2. γ-Fe according to claim 1
2O
3The preparation method of nanoparticle powder is characterized in that: it is to be 2～4 ︰, 1 addings by the mol ratio by iron acetate and ethylene glycol that described step (1) adds ethylene glycol.
3. γ-Fe according to claim 1 and 2
2O
3The preparation method of nanoparticle powder is characterized in that: it is to be that 1 ︰ 1 adds by volume that described step (2) sodium carbonate solution adds suspension liquid.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210443268.3A CN102923787B (en) | 2012-11-08 | 2012-11-08 | Method for preparing gamma-Fe2O3 nano particle powder |
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|---|---|---|---|
| CN201210443268.3A CN102923787B (en) | 2012-11-08 | 2012-11-08 | Method for preparing gamma-Fe2O3 nano particle powder |
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103601254A (en) * | 2013-11-19 | 2014-02-26 | 沈阳工业大学 | Method for preparing gamma-Fe2O3 nano hollow sphere through laser liquid phase |
| CN104829425A (en) * | 2015-04-14 | 2015-08-12 | 浙江师范大学 | Mono-dispersed fusiform nano-sheets and preparation method thereof |
-
2012
- 2012-11-08 CN CN201210443268.3A patent/CN102923787B/en not_active Expired - Fee Related
Non-Patent Citations (1)
| Title |
|---|
| 吴东辉等: ""铁(Ⅱ)无机物热解制备γ-Fe2O3及其机理"", 《硅酸盐学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103601254A (en) * | 2013-11-19 | 2014-02-26 | 沈阳工业大学 | Method for preparing gamma-Fe2O3 nano hollow sphere through laser liquid phase |
| CN103601254B (en) * | 2013-11-19 | 2016-02-17 | 沈阳工业大学 | Laser liquid phase prepares γ-Fe 2o 3the method of nano-hollow ball |
| CN104829425A (en) * | 2015-04-14 | 2015-08-12 | 浙江师范大学 | Mono-dispersed fusiform nano-sheets and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN102923787B (en) | 2014-09-03 |
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