CN103626238A - Method for preparing nano iron oxide with firing method - Google Patents
Method for preparing nano iron oxide with firing method Download PDFInfo
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- CN103626238A CN103626238A CN201310534141.7A CN201310534141A CN103626238A CN 103626238 A CN103626238 A CN 103626238A CN 201310534141 A CN201310534141 A CN 201310534141A CN 103626238 A CN103626238 A CN 103626238A
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- iron oxide
- organic solvent
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- molysite
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Abstract
The invention discloses a method for preparing nano iron oxide with a firing method. The method for preparing nano iron oxide with the firing method is a novel method, and comprises the following specific steps: dissolving raw materials for preparing a nanometer material into an organic solvent, and igniting with fire after complete dissolving till complete combustion; collecting a produced product, and washing to obtain the needed nanometer material. In the preparation process of nano iron oxide, lignosulfonate serving as a surfactant is added; the lignosulfonate is a by-product in the production of paper pulp, contains abundant functional groups, and is high in diffusivity. According to the method, iron oxide is prepared with the firing method, and the lignosulfonate serving as the surfactant is added to obtain red oblique hexagonal crystal alpha-Fe2O3 which has the advantages of uniform particles, small particle size and high dispersity; the method is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of calcination legal system for the method for nano-sized iron oxide, the sulfonated lignin of particularly take are prepared the method for nano-sized iron oxide as tensio-active agent.
Background technology
α-Fe
2o
3in the oxide compound of iron, be the most stable a kind of compound, its band gap width is narrower, is only 2.2 eV.In visible region, there is very strong light absorpting ability, can absorb approximately 30% solar energy, and there is photostabilization and thermotolerance.Nanometer α-Fe
2o
3crystal has caused people's especially concern because of advantages such as its stable in properties, abundant, the with low cost and nontoxicitys in source, at photochemical catalysis, stealth material, pigment preparation, gas sensor, and the field such as photoelectrochemicalcell cell demonstrates extensive and tempting application prospect.
Lignosulfonic acid molecules of salt is the spherical three-dimensional net structure body that is similar to of nearly 50 phenylpropyl alcohol alkane unit composition, centre is the script xylogen three-dimensional network molecular structure of unsulfonated, the side chain that central periphery is distributing and is being hydrolyzed and contains sulfonate radical, outermost layer is the electric double layer that the gegenion by sulfonate radical forms, its main functional group has sulfonate radical, phenolic hydroxyl, methoxyl group and carboxyl etc., and these functional groups are bases of sulfonated lignin application.Sulfonated lignin are that a kind of nontoxic, biodegradable, the abundant renewable resources of originating makes it in field of material preparation, be widely used.
Calcination legal system is a kind of comparatively novel method for nano material, and its concrete grammar is that the presoma that will prepare nano material is dissolved in organic solvent, after fully dissolving, with fire, lights and makes its perfect combustion.Products therefrom is collected to washing afterwards and obtained required nano material.Adopt calcination legal system for nano-sized iron oxide, operational condition is easy to control, and equipment is simple, and preparation cost is low, made product even particle distribution, and particle performance is high, and Particle dispersity is good, and split reunion degree is less, and pattern is better, is easy to realize industrialization.
summary of the invention
The object of the invention is to adopt sulfonated lignin is tensio-active agent, and by calcination method synthesis of nano ferric oxide, technique is simple, and raw material is easy to obtain, with low cost, of reduced contamination, is suitable for suitability for industrialized production.
Technical scheme of the present invention is as follows:
Under A, room temperature, get molysite and join in organic solvent, wherein the add-on ratio of molysite and organic solvent is (0.003-0.009): 30mol/ml;
B, will walk poly-A gained solution ultrasonic 20min in ultrasonic apparatus, and make molysite fully be dissolved in organic solvent;
C, in B solution, add sulfonated lignin, continue ultrasonic 20min, wherein in the add-on of sulfonated lignin and the poly-A of step, the ratio of organic solvent is (0.01-0.05): 30g/ml;
D, above-mentioned solution is lighted with fire;
E, after perfect combustion by washed with de-ionized water 4 times for gained solid, then with dehydrated alcohol, clean 1 time centrifugation;
F, the solid after separation is put into the dry 12h of thermostatic drying chamber, the temperature of described thermostatic drying chamber is 60 ℃;
In a more excellent open example of the present invention, described sulfonated lignin are sodium lignosulfonates.
In a more excellent open example of the present invention, molysite used is FeCl
3.6H
2o, Fe (NO
3)
3.9H
2o.
In a more excellent open example of the present invention, organic solvent used is ethanol.
This is tested reagent used and is all analytical pure, is commercially available.
beneficial effect
The present invention is a kind of comparatively novel method with calcination legal system for nano-sized iron oxide, and preparation method is simple, easy handling, preparation cost are low, made product even particle distribution, particle performance is high, and Particle dispersity is good, and split reunion degree is less, pattern is better, is easy to realize industrialization.
Accompanying drawing explanation
The X ray diffracting spectrum of Fig. 1 sample (XRD), in figure, a is the XRD figure spectrum of embodiment 1 sample; In figure, b is the XRD figure spectrum of embodiment 2 samples; In figure, c is the XRD figure spectrum of embodiment 6 samples.
embodiment
Below in conjunction with concrete embodiment, the present invention will be further described, so that those skilled in the art understand the present invention better, but the present invention is not limited to following examples.
embodiment 1
Under room temperature, get the FeCl that molar mass is 0.009mol
3.6H
2o, is dissolved in the alcohol solvent of 30ml.In ultrasonic apparatus, ultrasonic 20min, makes FeCl
3.6H
2o is fully dissolved in ethanol.Add sodium lignosulfonate 0.01g, continue ultrasonic 20min.Above-mentioned solution is lighted with fire, after perfect combustion, by washed with de-ionized water 4 times for gained solid, then with dehydrated alcohol, cleaned 1 time centrifugation.Solid after separation is put into the dry 12h of thermostatic drying chamber, and the temperature of described thermostatic drying chamber is 60 ℃.The XRD figure of sample is as Fig. 1 a.
embodiment 2
Under room temperature, getting molar mass is the Fe (NO of 0.009mol
3)
3.9H
2o, is dissolved in the alcohol solvent of 30ml.Ultrasonic 20min in ultrasonic apparatus, makes Fe (NO
3)
3.9H
2o is fully dissolved in ethanol.Add sodium lignosulfonate 0.01g, continue ultrasonic 20min.Above-mentioned solution is lighted with fire, after perfect combustion, by washed with de-ionized water 4 times for gained solid, then with dehydrated alcohol, cleaned 1 time centrifugation.Solid after separation is put into the dry 12h of thermostatic drying chamber, and the temperature of described thermostatic drying chamber is 60 ℃.The XRD figure of sample is as Fig. 1 b.
embodiment 3
Under room temperature, get the FeCl that molar mass is 0.009mol
3.6H
2o, is dissolved in the alcohol solvent of 30ml.In ultrasonic apparatus, ultrasonic 20min, makes FeCl
3.6H
2o is fully dissolved in ethanol.Add sodium lignosulfonate 0.05g, continue ultrasonic 20min.Above-mentioned solution is lighted with fire, after perfect combustion, by washed with de-ionized water 4 times for gained solid, then with dehydrated alcohol, cleaned 1 time centrifugation.Solid after separation is put into the dry 12h of thermostatic drying chamber, and the temperature of described thermostatic drying chamber is 60 ℃.
embodiment 4
Under room temperature, get the FeCl that molar mass is 0.003mol
3.6H
2o, is dissolved in the alcohol solvent of 30ml.In ultrasonic apparatus, ultrasonic 20min, makes FeCl
3.6H
2o is fully dissolved in ethanol.Add sodium lignosulfonate 0.04g, continue ultrasonic 20min.Above-mentioned solution is lighted with fire, after perfect combustion, by washed with de-ionized water 4 times for gained solid, then with dehydrated alcohol, cleaned 1 time centrifugation.Solid after separation is put into the dry 12h of thermostatic drying chamber, and the temperature of described thermostatic drying chamber is 60 ℃.
embodiment 5
Under room temperature, get the FeCl that molar mass is 0.006mol
3.6H
2o, is dissolved in the alcohol solvent of 30ml.In ultrasonic apparatus, ultrasonic 20min, makes FeCl
3.6H
2o is fully dissolved in ethanol.Add sodium lignosulfonate 0.01g, continue ultrasonic 20min.Above-mentioned solution is lighted with fire, after perfect combustion, by washed with de-ionized water 4 times for gained solid, then with dehydrated alcohol, cleaned 1 time centrifugation.Solid after separation is put into the dry 12h of thermostatic drying chamber, and the temperature of described thermostatic drying chamber is 60 ℃.
embodiment 6
Under room temperature, getting molar mass is the Fe (NO of 0.006mol
3)
3.9H
2o, is dissolved in the alcohol solvent of 30ml.Ultrasonic 20min in ultrasonic apparatus, makes Fe (NO
3)
3.9H
2o is fully dissolved in ethanol.Add sodium lignosulfonate 0.04g, continue ultrasonic 20min.Above-mentioned solution is lighted with fire, after perfect combustion, by washed with de-ionized water 4 times for gained solid, then with dehydrated alcohol, cleaned 1 time centrifugation.Solid after separation is put into the dry 12h of thermostatic drying chamber, and the temperature of described thermostatic drying chamber is 60 ℃.The XRD figure of sample is as Fig. 1 c.
Claims (4)
1. calcination legal system, for a method for nano-sized iron oxide, is carried out according to following step:
Under A, room temperature, get in the organic solvent that molysite adds, wherein the add-on ratio of molysite and organic solvent is (0.003-0.009): 30mol/ml;
B, in ultrasonic apparatus ultrasonic 20min, make molysite fully be dissolved in organic solvent;
C, add sulfonated lignin, continue ultrasonic 20min, wherein in the add-on of sulfonated lignin and the poly-A of step, the ratio of organic solvent is (0.01-0.05): 30g/ml;
D, above-mentioned solution is lighted with fire;
E, after perfect combustion by washed with de-ionized water 4 times for gained solid, then with dehydrated alcohol, clean 1 time centrifugation;
F, the solid after separation is put into the dry 12h of thermostatic drying chamber, the temperature of described thermostatic drying chamber is 60 ℃.
2. calcination legal system according to claim 1, for the method for nano-sized iron oxide, is characterized in that: described molysite is FeCl
3.6H
2o or Fe (NO
3)
3.9H
2o.
3. calcination legal system according to claim 1, for the method for nano-sized iron oxide, is characterized in that: described Sulfite lignin are sodium lignosulfonate.
4. calcination legal system according to claim 1, for the method for nano-sized iron oxide, is characterized in that: described organic solvent is ethanol.
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| CN201310534141.7A CN103626238B (en) | 2013-11-01 | 2013-11-01 | Method for preparing nano iron oxide with firing method |
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| CN103626238B CN103626238B (en) | 2015-06-10 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104909412A (en) * | 2015-05-12 | 2015-09-16 | 江苏大学 | Preparation method of magnetic Fe2O3/Fe3O4 nano-heteroplasmon particles |
-
2013
- 2013-11-01 CN CN201310534141.7A patent/CN103626238B/en not_active Expired - Fee Related
Non-Patent Citations (1)
| Title |
|---|
| Y.T. PRABHU ET AL.: ""Surfactant- Assisted Combustion Method for the Synthesis of α-Fe2O3 Nanocrystalline Powders"", 《INTERNATIONAL JOURNAL OF PURE AND APPLIED SCIENCES AND TECHNOLOGY》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104909412A (en) * | 2015-05-12 | 2015-09-16 | 江苏大学 | Preparation method of magnetic Fe2O3/Fe3O4 nano-heteroplasmon particles |
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