CN101434412A - Preparation of alpha-FeOOH nano-rod - Google Patents
Preparation of alpha-FeOOH nano-rod Download PDFInfo
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- CN101434412A CN101434412A CNA2008100428697A CN200810042869A CN101434412A CN 101434412 A CN101434412 A CN 101434412A CN A2008100428697 A CNA2008100428697 A CN A2008100428697A CN 200810042869 A CN200810042869 A CN 200810042869A CN 101434412 A CN101434412 A CN 101434412A
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Abstract
The invention relates to a preparation method of an alpha-FeOOH nano rod with uniform appearance, which belongs to the technical field of inorganic nonmetal nano material preparation. The preparation method of the alpha-FeOOH nano rod provided by the invention comprises the steps of: adding ethanol and the triblock copolymer of polyoxyethylene-polyoxypropylene-polyoxyethylene (PEO-PPO-PEO) into the mixed aqueous solution of Fe<3> and Fe<2+>, then adding an NaOH solution until the pH of the mixed solution is 10-11, stirring and aging the mixed solution for 24 hours at room temperature to obtain a suspension, filtering or centrifugalizing the suspension to obtain solid precipitate, washing and then drying the precipitate at 30-50 DEG C to obtain the alpha-FeOOH nano rod. The alpha-FeOOH nano rod has uniform appearance, diameter of 20nm and length of 200-300nm, and can be used in the fields of dyeing, catalysis, gas detection, magnetic record, and the like. The preparation method which is simple and accessible can be implemented at normal temperature and normal pressure, thus remarkably reducing production cost.
Description
Technical field
The present invention relates to a kind of preparation method of uniform morphology alpha-feooh nanometer rod, belong to the preparing technical field of inorganic nonmetallic nanometer material.
Background technology
Alpha-feooh claims iron oxide yellow again, is the important source material in the Chemical Manufacture, is widely used at dyestuff, catalysis, gas detection, magnetic recording and aspects such as soft magnetism, hard magnetic material.Alpha-feooh is used as pigment always or is used as preparation α-Fe
2O
3And γ-Fe
2O
3Raw material.Needle-like or bar-shaped alpha-feooh particle are used in many fields such as fundamental research, chemical industry and colloid and surface chemistry.For example, the alpha-feooh nanometer rod has shown good prospects for application in inorganic liquid crystal material research.Industrial, as the magnetic of magnetic recording media basic raw material, use at present is at most needle-like γ-Fe
2O
3And coating, generally making by the dehydration of needle-like alpha-feooh, the integrity of the shape of iron oxide yellow, granularity and crystalline structure has determined final γ-Fe
2O
3The over-all properties of magnetic is so preparation needle-like profile, perfect crystalline, particle is little and the alpha-feooh that do not have a branch is to obtain high-performance γ-Fe
2O
3The key point of magnetic.
The production technology of iron oxide yellow has several different methods, and classic methods is with ferrous sulfate (FeSO
4) be raw material, bubbling air oxidation and make iron oxide yellow.Now existing patents relate to the technology of preparing of iron oxide yellow.For example: it is the method for feedstock production high purity iron oxide yellow with the byproduct ferrous sulfate of titanium dioxide that Chinese patent CN1766005 provides a kind of, this method is lower than in temperature under 60 ℃ the condition, byproduct ferrous sulfate of titanium dioxide solution is carried out refining and edulcoration, under the condition that has oxygenant to exist, by adjusting the pH value of solution, reach hydrolysis removes metal ions such as dezincify, manganese except that titanium and co-precipitation purpose, control the pH value of solution then, blowing air carries out oxidation under normal temperature condition, under different reaction conditionss, obtain iron oxide yellow, purity reaches 99.5%.Chinese patent CN1056668 provides a kind of method of utilizing washed metal exhausted spent acid solution directly to make iron oxide yellow.It is the production method that fired slags is made ferric oxide yellow pigment with producing the vitriolic waste residue that Chinese patent CN1143611 provides a kind of.Chinese patent CN1699476 provides a kind of preparation method of nano iron oxide yellow pigment, the solution that this method will contain ferric ion Fe3+ joins in the solution of hydroxyl-containing ion OH-, fully reaction under the alkaline condition that heating is constantly stirred simultaneously, in the reaction process, heating makes reaction solution remain on slight boiling condition and constantly stirs, stirring velocity is 800～10000r/pm, after the precipitation that generates is stable, filters, wash, vacuumize heat drying and be prepared into nano level ferric oxide yellow pigment.Chinese patent CN1415664 provides a kind of preparation method of nano iron oxide yellow, this method is a raw material with the refining green vitriol (FeSO4) that purifies, under certain temperature and stirring velocity, a certain amount of mixed additive Sodium hexametaphosphate 99 and alkylphenol polyoxyethylene (OP-10) are joined in the refining green vitriol FeSO4 solution, the Na2CO3 solution of dropping 10% is to pH value 3.5-6.5, and keep 20-40 ℃ of certain reaction temperature, react preparation nano iron oxide yellow crystal seed then with aerating oxygen under the logical oxygen flow of 0.12-0.18m3/h; And then be warming up to 50-60 ℃, and again with the flow aerating oxygen of 0.12-0.18m3/h, in the solution that contains crystal seed, dripping 10% Na2CO3 solution, maintenance system pH value was reacted 8 hours in the 3.0-5.5 scope, made seeded growth; After reaction finishes, will contain the nano iron oxide yellow supernatant liquid filter, dry, pulverize and obtain the nano iron oxide yellow particle.Yet aforesaid method does not all relate to the preparation of uniform morphology alpha-feooh nanometer rod.
Based on the peculiar property that one-dimentional structure produced, the synthetic of one dimension alpha-feooh nanometer rod all paid close attention in many research work.The preparation method of nanometer alpha-feooh has multiple, industrial air oxidation process, oxymuriate oxidation method, hydroxyl oxidize method and the peptisation of mainly containing.The above two are many to be raw material with the ferrous sulfate, and production cost is low, but quality product is difficult to control; Both good product qualities of back, but production cost height.Therefore, exploitation alpha-feooh nanometer rod new cheaply, uniform morphology has great practical significance.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of pattern homogeneous, simple alpha-feooh nanometer rod.
For realizing above-mentioned purpose, adding and the control of the solvent composition formation that realizes uniform morphology alpha-feooh of the present invention by organic additive, the preparation method is simple and easy, the pattern homogeneous of alpha-feooh nanometer rod, the about 20nm of the diameter of alpha-feooh nanometer rod, length is between 200～300nm.The present invention adopts following technical scheme, now is described in detail as follows.
The concrete operations step:
The first step raw material is prepared
Raw material is FeCl
36H
2O (analytical pure), FeSO
47H
2O (analytical pure), NaOH (analytical pure), organic additive polyoxyethylene-poly-oxypropylene polyoxyethylene (PEO-PPO-PEO) triblock copolymer Pluronic F127 (being called for short F127) (analytical pure), ethanol (chemical pure).
The preparation of the second step reaction solution
Preparation Fe
3+And Fe
3+The molysite mixed aqueous solution, Fe in the molysite mixed aqueous solution
3+Ionic concentration is 0.08～0.8mol/L, Fe
2+Ionic concentration is 0.04～0.4mol/L, Fe
3+Ion and Fe
2+The ionic concentration ratio is 2, adds 5 times of volume of ethanol and a spot of F127, and the concentration of F127 is 8～15g/L, makes Fe
3+And Fe
2+Molysite/tensio-active agent blended water/ethanolic soln; The preparation NaOH aqueous solution, the concentration of NaOH is 0.5～2mol/L;
The preparation of the 3rd step alpha-feooh nanometer rod
Getting the molysite mixing water/ethanolic soln of second step preparation, is the NaOH solution of 0.5～2mol/L to mixed solution and dripping concentration at room temperature, stirs, pH=10～11 to mixing solutions, continued stir about 1 hour, with the uncovered air that places of solution that obtains, ageing is 24 hours under the room temperature;
The separation and the washing of the 4th step product
With suspension liquid suction filtration or the centrifugal solid precipitation that obtains that the 3rd step made, use deionized water wash, repeat 2～3 times;
The drying of the 5th step product
Collect the solid sediment that the 4th step obtained, put into vacuum drying oven, 30～50 ℃ of oven dry down obtain powder-product, the about 20nm of diameter, the alpha-feooh nanometer rod of the uniform morphology of length between 200～300nm.
Compare with background technology, the present invention has following beneficial effect:
1, Fa Ming alpha-feooh nanometer rod pattern homogeneous, the about 20nm of diameter, length can be used for fields such as dyestuff, catalysis, gas detection, magnetic recording between 200～300nm.
2, preparation method of the present invention is simple, can prepare at normal temperatures and pressures, can reduce production costs significantly.
Below in conjunction with specific embodiment, the invention will be further elaborated.The invention is not restricted to these specific embodiments.
Embodiment
All embodiment all operate by above-mentioned preparation method's operation steps.
Embodiment 1
Preparation 10mL Fe
3+And Fe
2+The molysite mixed aqueous solution, Fe in the molysite mixed aqueous solution
3+Ionic concentration is 0.08mol/L, Fe
2+Concentration be 0.04mol/L, add 50mL ethanol and 0.5g F127, stir, at room temperature be the NaOH solution of 0.5mol/L to mixed solution and dripping concentration, pH=10～11 to mixing solutions, continued stir about 1 hour, with the uncovered air that places of reaction system, ageing is 24 hours under the room temperature.Sample is collected through suction filtration or centrifuge washing and is obtained product, i.e. the about 20nm of diameter, the alpha-feooh nanometer rod of the uniform morphology of length between 200～300nm.
Embodiment 2
Preparation 10mL Fe
3+And Fe
2+The molysite mixed aqueous solution, Fe in the molysite mixed aqueous solution
3+Ionic concentration is 0.2mol/L, Fe
2+Concentration be 0.1mol/L, add 50mL ethanol and 0.8g F127, stir, at room temperature be the NaOH solution of 0.5mol/L to mixed solution and dripping concentration, pH=10～11 to mixing solutions, continued stir about 1 hour, with the uncovered air that places of reaction system, ageing is 24 hours under the room temperature.Sample is collected through suction filtration or centrifuge washing and is obtained product, i.e. the about 20nm of diameter, the alpha-feooh nanometer rod of the uniform morphology of length between 200～300nm.
Embodiment 3
Preparation 20mL Fe
3+And Fe
2+The molysite mixed aqueous solution, Fe in the molysite mixed aqueous solution
3+Ionic concentration is 0.48mol/L, Fe
2+Concentration be 0.24mol/L, add 100mL ethanol and 1.0g F127, stir, at room temperature be the NaOH solution of 1mol/L to mixed solution and dripping concentration, pH=10～11 to mixing solutions, continued stir about 1 hour, with the uncovered air that places of reaction system, ageing is 24 hours under the room temperature.Sample obtains the about 20nm of diameter, the alpha-feooh nanometer rod of the uniform morphology of length between 200～300nm through suction filtration or centrifuge washing collection.
Embodiment 4
Preparation 30mL Fe
3+And Fe
2+The molysite mixed aqueous solution, Fe in the molysite mixed aqueous solution
3+Ionic concentration is 0.8mol/L, Fe
2+Concentration be 0.4mol/L, add 150mL ethanol and 2.0g F127, stir, at room temperature be the NaOH solution of 1mol/L to mixed solution and dripping concentration, pH=10～11 to mixing solutions, continued stir about 1 hour, with the uncovered air that places of reaction system, ageing is 24 hours under the room temperature.Sample obtains the about 20nm of diameter, the alpha-feooh nanometer rod of the uniform morphology of length between 200～300nm through suction filtration or centrifuge washing collection.
Claims (1)
1. the preparation method of an alpha-feooh nanometer rod is characterized in that comprising the steps:
The first step: in concentration is the Fe of 0.08～0.8mol/L
3+With concentration be the Fe of 0.04～0.4mol/L
2+Mixed aqueous solution in add 5 times of volume of ethanol, and concentration is polyoxyethylene-poly-oxypropylene polyoxyethylene (PEO-PPO-PEO) triblock copolymer of 8～15g/L, wherein Fe3
+Ion and Fe
2+The ionic concentration ratio is 2, prepare Fe
3+And Fe
2+Molysite/tensio-active agent blended water/ethanolic soln;
Second step: at the Fe of the first step preparation
3+And Fe
2+Molysite/tensio-active agent blended water/ethanolic soln in, dripping concentration is the NaOH solution of 0.5～2mol/L, pH=10～11 to mixing solutions, stir, ageing got suspension liquid in 24 hours under the room temperature, suction filtration or the centrifugal solid precipitation that obtains, washing is dried down for 30～50 ℃ and is obtained the alpha-feooh nanometer rod.
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|---|---|---|---|
| CNA2008100428697A CN101434412A (en) | 2008-09-12 | 2008-09-12 | Preparation of alpha-FeOOH nano-rod |
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|---|---|---|---|
| CNA2008100428697A CN101434412A (en) | 2008-09-12 | 2008-09-12 | Preparation of alpha-FeOOH nano-rod |
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| Publication Number | Publication Date |
|---|---|
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ID=40709072
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102134102A (en) * | 2011-02-15 | 2011-07-27 | 江苏大学 | Preparation method of iron oxide nanorod |
| CN103273078A (en) * | 2013-05-12 | 2013-09-04 | 山东理工大学 | Preparation method of anisotropy silver nanorod |
| CN104209534A (en) * | 2014-07-30 | 2014-12-17 | 苏州铉动三维空间科技有限公司 | Preparation method for hybrid structure of iron hydroxide nanorods-gold nanoparticles |
| CN104495946A (en) * | 2014-12-11 | 2015-04-08 | 上海烟草集团有限责任公司 | Preparation and application of different-crystal-phase FeOOH nanometer materials |
| CN108439477A (en) * | 2018-06-07 | 2018-08-24 | 安徽工业大学 | A kind of preparation method of order mesoporous FeOOH nanometer rods |
-
2008
- 2008-09-12 CN CNA2008100428697A patent/CN101434412A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102134102A (en) * | 2011-02-15 | 2011-07-27 | 江苏大学 | Preparation method of iron oxide nanorod |
| CN102134102B (en) * | 2011-02-15 | 2013-07-17 | 江苏大学 | Preparation method of iron oxide nanorod |
| CN103273078A (en) * | 2013-05-12 | 2013-09-04 | 山东理工大学 | Preparation method of anisotropy silver nanorod |
| CN104209534A (en) * | 2014-07-30 | 2014-12-17 | 苏州铉动三维空间科技有限公司 | Preparation method for hybrid structure of iron hydroxide nanorods-gold nanoparticles |
| CN104495946A (en) * | 2014-12-11 | 2015-04-08 | 上海烟草集团有限责任公司 | Preparation and application of different-crystal-phase FeOOH nanometer materials |
| CN108439477A (en) * | 2018-06-07 | 2018-08-24 | 安徽工业大学 | A kind of preparation method of order mesoporous FeOOH nanometer rods |
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Open date: 20090520 |