CN1686827A - Method for producing nano material of alpha-Fe00H and alpha Fe2O3 in one dimension - Google Patents
Method for producing nano material of alpha-Fe00H and alpha Fe2O3 in one dimension Download PDFInfo
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- CN1686827A CN1686827A CN 200510043205 CN200510043205A CN1686827A CN 1686827 A CN1686827 A CN 1686827A CN 200510043205 CN200510043205 CN 200510043205 CN 200510043205 A CN200510043205 A CN 200510043205A CN 1686827 A CN1686827 A CN 1686827A
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Abstract
The production method of one-dimentional alpha-FeOOH and alpha-Fe2O3 nano material. Said method includes the following steps: a. adding soluble strong-base wear-acid salt in the soluble salt solution in which divalent iron is dissolved, stirring them to produce yellow precipitate; b. placing the above-mentioned material into a reactor, heating, after the reaction is completed, cooling to room temperature and c. washing and drying so as to obtain one-dimensional alpha-FeOOH nano material, then calcining said one-dimentional alpha-FeOOH nano material at 240-360 deg.C to obtain one-dimentional alpha-Fe2O3 nano material.
Description
Technical field
The invention belongs to technical field of inorganic chemical industry, relate in particular to a kind of one dimension alpha-feooh and α-Fe
2O
3The production method of nano material.
Background technology
The oxide-based nanomaterial of transition metal (Fe, Co, Ni etc.) is an important directions of nanometer material science research and discovery owing to have character such as special light, electricity, heat, magnetic.Wherein, the nanometer alpha-feooh itself can be used as pigment, and it is preparation α-Fe
2O
3Important presoma; α-Fe
2O
3Have a wide range of applications at industrial circles such as magnetic recording material, fine ceramics, plastics, coating, catalyzer and to be worth and development prospect: nanometer α-Fe
2O
3Have magnetic and good hardness, can be used as magneticsubstance and magnetic recording material; Nanometer α-Fe
2O
3Having good weathering resistance, photostabilization and chemical stability, is a kind of important mineral dye and fine ceramics raw material; Nanometer α-Fe
2O
3Have huge specific surface area, surface effects is remarkable, is a kind of good catalyzer; Nanometer α-Fe
2O
3Have characteristic of semiconductor, its electricity is led temperature, humidity and gas geometric ratio responsive, is a kind of sensitive material with development potentiality.Monodimension nanometer material is because its anisotropic existence may produce novel light, electricity, magnetic property.Therefore, the multiple preparation method of the one dimension transition metal oxide nano-material of exploitation different-shape has very important realistic meaning undoubtedly.At one dimension α-Fe
2O
3Preparation aspect people done a few thing: gas phase synthesis method [Y.Y.Fu, R.M.Wang, J.Xu; J.Chen, Y.Yan, A.V.Narlikar and H.Zhang Chemical Physics Letters; 2003,379, (3-4); 373-379.Yunyi Fu, Jing Chen and Han Zhang, Chemical Physics Letters; 2001,350 (5-6), 491-494.] template [Feng Jiao; Bin Yue, Kake, Zhu; DongyuanZhao; Heyong He, Chemistry Letters, 2003; 32; (8), 770-771.], monocrystalline or polycrystalline are matrix growth method [Lionel; Vayssieres; Niclas, Beermann, Sten-EricLindquist; Anders; Hagfeldt, Chemistry ofMaterials, 2001; 13 (2); 233-235.] sol-gel method [Cairong Gong, Dairong Chen, Xiuling Jiao andQilong Wang; J.Mater.Chem.; 2004,14 (5), 905-907.]. vapor phase process needs special equipment and higher temperature of reaction usually; adopt template or matrix can make operation steps complicated; the cost height, and can introduce impurity, be difficult to realize large-scale industrial production.Thereby, be badly in need of exploring easier production method.
Summary of the invention
Purpose of the present invention is intended to overcome the deficiencies in the prior art, provides a kind of simple for process, and cost is low, and the purity height helps the one dimension alpha-feooh and the α-Fe that realize that large-scale industrial is produced
2O
3The production method of nano material.
Purpose of the present invention can realize by following technical measures:
The production method of this one dimension alpha-feooh is carried out as follows:
A. in being dissolved with ferrous soluble salt solution, add the solubility strong base-weak acid salt, be stirred to the generation yellow mercury oxide; Then
B. insert reactor, reaction finishes postcooling to room temperature under heating; Again
C. through washing and dry, get the one dimension alpha-FeOOH nano material.
Purpose of the present invention also can realize by following technical measures:
Described ferrous, the iron protochloride of ferrous soluble salt preferably sulfuric acid, the preferred sodium-acetate of described strong base-weak acid salt, the Potassium ethanoate of being dissolved with; Reacting by heating temperature in the described reactor is 60-110 ℃, and the reacting by heating time is 5-12 hour.
Aforesaid one dimension alpha-FeOOH nano material was calcined 1.5-2.5 hour down at 240-360 ℃, obtained one dimension α-Fe
2O
3Nano material.
Stirring of the present invention is to carry out in normal air, is generally 5-30 minute; Described drying adopts conventional vacuum-drying usually; Described washing is to adopt deionized water to wash unreacted unnecessary ion off.
The present invention is a raw material with ferrous soluble salt and strong base-weak acid salt, under the situation of not introducing any tensio-active agent or template, has produced the one dimension alpha-FeOOH nano material by the low-temperature hydrothermal reaction.The one dimension alpha-FeOOH nano material of gained can obtain one dimension α-Fe by calcining
2O
3Nano material, the pattern of nanometer rod can be kept preferably.This method is not used any tensio-active agent or template, and technology is simple, and is raw materials used cheap and easy to get, with low cost, and productive rate is higher, can realize large-scale industrial production.One dimension α-the Fe that is produced
2O
3Nano material is expected to obtain to use widely in fields such as electricity, magnetic, catalysis owing to anisotropic existence.
Description of drawings:
Fig. 1 is the XRD figure of the alpha-FeOOH nano material produced of the present invention;
Fig. 2 is α-Fe that the present invention produces
2O
3The XRD figure of nano material;
Fig. 3 is the TEM figure of the alpha-FeOOH nano material produced of the present invention;
Fig. 4 is α-Fe that the present invention produces
2O
3The TEM figure of nano material.
Embodiment:
Embodiment 1:
Take by weighing the 0.0005mol ferrous sulfate and the 0.001mol sodium acetate, anhydrous adds the 20ml water dissolution, induction stirring 20min in air, transfer in the 20ml stainless steel cauldron, 110 ℃ of following hydro-thermal reactions 8 hours, again the product that reacts completely is cooled to room temperature, after deionized water wash and conventional vacuum-drying obtain product alpha-feooh nanometer rod.Resulting alpha-feooh nanometer rod with 240 ℃ of calcinings 2 hours, gets α-Fe in retort furnace
2O
3Nanometer rod.
Embodiment 2:
Take by weighing the 0.0005mol iron protochloride and the 0.001mol sodium acetate, anhydrous adds the 20ml water dissolution, induction stirring 5min in air, transfer in the 20ml stainless steel cauldron, 80 ℃ of following hydro-thermal reactions 5 hours, again the product that reacts completely is cooled to room temperature, after deionized water wash and conventional vacuum-drying obtain product alpha-feooh nanometer rod.Resulting alpha-feooh nanometer rod with 300 ℃ of calcinings 1.5 hours, gets α-Fe in retort furnace
2O
3Nanometer rod.
Embodiment 3:
Take by weighing the 0.001mol ferrous sulfate and 0.002mol Glacial acetic acid potassium adds the 20ml water dissolution, induction stirring 30min in air, transfer in the 20ml stainless steel cauldron, 60 ℃ of following hydro-thermal reactions 12 hours, again the product that reacts completely is cooled to room temperature, after deionized water wash and conventional vacuum-drying obtain the alpha-feooh nanometer rod.Resulting alpha-feooh nanometer rod with 360 ℃ of calcinings 1.5 hours, gets α-Fe in retort furnace
2O
3Nanometer rod.
Embodiment 4:
Take by weighing the 0.001mol iron protochloride and 0.002mol Glacial acetic acid potassium adds the 20ml water dissolution, induction stirring 15min in air, transfer in the 20ml stainless steel cauldron, 70 ℃ of following hydro-thermal reactions 9 hours, again the product that reacts completely is cooled to room temperature, after deionized water wash and conventional vacuum-drying obtain the alpha-feooh nanometer rod.Resulting alpha-feooh nanometer rod with 280 ℃ of calcinings 2 hours, gets α-Fe in retort furnace
2O
3Nanometer rod.
Claims (4)
1, the production method of one dimension alpha-FeOOH nano material is characterized in that this method carries out as follows:
A. in being dissolved with ferrous soluble salt solution, add the solubility strong base-weak acid salt, be stirred to the generation yellow mercury oxide; Then
B. insert reactor, reaction finishes postcooling to room temperature under heating; Again
C. through washing and dry, get the one dimension alpha-FeOOH nano material.
2, the production method of one dimension alpha-FeOOH nano material according to claim 1 is characterized in that described ferrous, the iron protochloride of ferrous soluble salt preferably sulfuric acid that is dissolved with, the preferred sodium-acetate of described strong base-weak acid salt, Potassium ethanoate.
3. the production method of one dimension alpha-FeOOH nano material according to claim 1 is characterized in that the reacting by heating temperature in the described reactor is 60-110 ℃, and the reacting by heating time is 5-12 hour.
4, produce one dimension α-Fe with the one dimension alpha-FeOOH nano material of claim 1 or 2
2O
3The method of nano material is characterized in that the one dimension alpha-FeOOH nano material was calcined 1.5-2.5 hour down at 240-360 ℃, obtains one dimension α-Fe
2O
3Nano material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100432059A CN1315734C (en) | 2005-03-30 | 2005-03-30 | Method for producing nano material of alpha-Fe00H and alpha Fe2O3 in one dimension |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100432059A CN1315734C (en) | 2005-03-30 | 2005-03-30 | Method for producing nano material of alpha-Fe00H and alpha Fe2O3 in one dimension |
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| Publication Number | Publication Date |
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| CN1686827A true CN1686827A (en) | 2005-10-26 |
| CN1315734C CN1315734C (en) | 2007-05-16 |
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| CNB2005100432059A Expired - Fee Related CN1315734C (en) | 2005-03-30 | 2005-03-30 | Method for producing nano material of alpha-Fe00H and alpha Fe2O3 in one dimension |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101314524B (en) * | 2008-07-04 | 2011-06-08 | 北京工业大学 | Method for preparing alpha type ferric oxide film |
| CN103420429A (en) * | 2013-07-26 | 2013-12-04 | 重庆绿色智能技术研究院 | Preparation method of nano magnetic iron oxide |
| CN104005015A (en) * | 2014-06-12 | 2014-08-27 | 哈尔滨工业大学 | Method for conducting in-situ growth of alpha-Fe2O3 nano arrays on surface of steel |
| CN105039938A (en) * | 2015-06-19 | 2015-11-11 | 许昌学院 | Method for preparing photoelectrode of alpha-iron oxide film by single-source precursor |
| CN105800693A (en) * | 2016-05-19 | 2016-07-27 | 青岛大学 | Preparation method for alpha-FeOOH three-dimensional multi-grade microsphere |
| CN106966433A (en) * | 2017-04-25 | 2017-07-21 | 福建船政交通职业学院 | A kind of goethite nanometer rods for solid propellant |
| CN108217750A (en) * | 2018-03-09 | 2018-06-29 | 东北大学 | A kind of α-Fe2O3/ FeOOH composite functional materials and its preparation method and application |
| CN108502932A (en) * | 2018-06-06 | 2018-09-07 | 江苏大学 | A kind of FeOOH microns of octahedral preparation method |
| CN109046228A (en) * | 2018-07-12 | 2018-12-21 | 华中农业大学 | A kind of goethite and its preparation method and application |
| CN111661878A (en) * | 2019-03-05 | 2020-09-15 | 中国石油天然气股份有限公司 | Preparation method of nano alpha-iron oxide hydroxide |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102637869A (en) * | 2012-05-02 | 2012-08-15 | 中国科学院长春应用化学研究所 | Fe2O3 nanorod and manufacturing method and usages of Fe2O3 nanorod |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4251504A (en) * | 1979-09-20 | 1981-02-17 | Tdk Electronics, Co. Ltd. | Process for producing acicular goethite |
| EP0604849B1 (en) * | 1992-12-29 | 1996-10-16 | Ishihara Sangyo Kaisha, Ltd. | Cobalt-containing magnetic iron oxide and process for producing the same |
| CN1222544A (en) * | 1997-11-19 | 1999-07-14 | 拜尔公司 | Non-silking iron oxide yellow pigments with high colour density |
| DE10010940A1 (en) * | 2000-03-06 | 2001-09-13 | Bayer Ag | Production of iron oxide yellow, useful for pigmenting building material, e.g. concrete, or plastics or as disperse dye, involves adding iron-II sulfate or chloride solution to alkaline solution and oxidation under specified conditions |
-
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101314524B (en) * | 2008-07-04 | 2011-06-08 | 北京工业大学 | Method for preparing alpha type ferric oxide film |
| CN103420429A (en) * | 2013-07-26 | 2013-12-04 | 重庆绿色智能技术研究院 | Preparation method of nano magnetic iron oxide |
| CN104005015A (en) * | 2014-06-12 | 2014-08-27 | 哈尔滨工业大学 | Method for conducting in-situ growth of alpha-Fe2O3 nano arrays on surface of steel |
| CN104005015B (en) * | 2014-06-12 | 2016-03-02 | 哈尔滨工业大学 | A kind of method of steel surface growth in situ α-Fe2O3 nano-array |
| CN105039938A (en) * | 2015-06-19 | 2015-11-11 | 许昌学院 | Method for preparing photoelectrode of alpha-iron oxide film by single-source precursor |
| CN105039938B (en) * | 2015-06-19 | 2018-10-02 | 许昌学院 | The method that a kind of list source presoma prepares the optoelectronic pole of α-ferric oxide film |
| CN105800693A (en) * | 2016-05-19 | 2016-07-27 | 青岛大学 | Preparation method for alpha-FeOOH three-dimensional multi-grade microsphere |
| CN106966433A (en) * | 2017-04-25 | 2017-07-21 | 福建船政交通职业学院 | A kind of goethite nanometer rods for solid propellant |
| CN108217750A (en) * | 2018-03-09 | 2018-06-29 | 东北大学 | A kind of α-Fe2O3/ FeOOH composite functional materials and its preparation method and application |
| CN108502932A (en) * | 2018-06-06 | 2018-09-07 | 江苏大学 | A kind of FeOOH microns of octahedral preparation method |
| CN109046228A (en) * | 2018-07-12 | 2018-12-21 | 华中农业大学 | A kind of goethite and its preparation method and application |
| CN111661878A (en) * | 2019-03-05 | 2020-09-15 | 中国石油天然气股份有限公司 | Preparation method of nano alpha-iron oxide hydroxide |
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| CN1315734C (en) | 2007-05-16 |
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