CN103626238B - 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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- CN103626238B CN103626238B CN201310534141.7A CN201310534141A CN103626238B CN 103626238 B CN103626238 B CN 103626238B CN 201310534141 A CN201310534141 A CN 201310534141A CN 103626238 B CN103626238 B CN 103626238B
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- iron oxide
- organic solvent
- molysite
- drying chamber
- nano iron
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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 the method for a kind of calcination legal system for nano-sized iron oxide, is particularly the method that nano-sized iron oxide prepared by tensio-active agent with sulfonated lignin.
Background technology
α-Fe
2o
3be the most stable a kind of compound in the oxide compound of iron, its band gap width is narrower, is only 2.2 eV.There is in visible region very strong light absorpting ability, the solar energy of about 30% can be absorbed, and there is photostabilization and thermotolerance.Nanometer α-Fe
2o
3crystal causes the especially concern of people because of its stable in properties, abundance, with low cost and advantages such as nontoxicity, at photochemical catalysis, stealth material, pigment preparation, gas sensor, and the field such as photoelectrochemicalcell cell demonstrates extensive and tempting application prospect.
Lignosulfonate molecules be nearly 50 benzene oxide unit composition be similar to spherical three-dimensional net structure body, centre is the script xylogen three-dimensional network molecular structure of unsulfonated, central periphery is dispersed with and is hydrolyzed and containing the side chain of sulfonate radical, outermost layer is the electric double layer formed by the gegenion of sulfonate radical, 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 renewable resources that is nontoxic, biodegradable, abundance makes it be widely used in field of material preparation.
Calcination legal system is a kind of comparatively novel method for nano material, and its concrete grammar is that the presoma will preparing nano material is dissolved in organic solvent, lights make its perfect combustion after fully dissolving with fire.Products therefrom collected after washing and obtain 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, and made product grain is evenly distributed, and particulates' properties 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 to be tensio-active agent, 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:
Getting molysite under A, room temperature joins in organic solvent, and wherein the add-on ratio of molysite and organic solvent is (0.003-0.009): 30mol/ml;
B, step is gathered A gained solution ultrasonic 20min in ultrasonic apparatus, molysite is fully dissolved in organic solvent;
C, in B solution, add sulfonated lignin, continue ultrasonic 20min, wherein the add-on of sulfonated lignin is (0.01-0.05): 30g/ml with the ratio of organic solvent in the poly-A of step;
D, above-mentioned solution fire to be lighted;
E, after perfect combustion by gained solid washed with de-ionized water 4 times, then use washes of absolute alcohol 1 time, centrifugation;
F, by be separated after solid put into the dry 12h of thermostatic drying chamber, the temperature of described thermostatic drying chamber is 60 DEG C;
In a more excellent disclosed example of the present invention, described sulfonated lignin are sodium lignosulfonates.
In a more excellent disclosed example of the present invention, molysite used is FeCl
3.6H
2o, Fe (NO
3)
3.9H
2o.
In a more excellent disclosed 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 method of comparatively novelty for nano-sized iron oxide with calcination legal system, and preparation method is simple, easy handling, preparation cost are low, and made product grain is evenly distributed, particulates' properties 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 (XRD) of Fig. 1 sample, in figure, a is the XRD figure spectrum of embodiment 1 sample; In figure, b is the XRD figure spectrum of embodiment 2 sample; In figure, c is the XRD figure spectrum of embodiment 6 sample.
Embodiment
Below in conjunction with concrete embodiment, the present invention will be further described, and to make those skilled in the art understand the present invention better, but the present invention is not limited to following examples.
embodiment 1
The FeCl that molar mass is 0.009mol is got under room temperature
3.6H
2o, is dissolved in the alcohol solvent of 30ml.In ultrasonic apparatus, ultrasonic 20min, makes FeCl
3.6H
2o fully dissolves in ethanol.Add sodium lignosulfonate 0.01g, continue ultrasonic 20min.Above-mentioned solution fire is lighted, by gained solid washed with de-ionized water 4 times after perfect combustion, then uses washes of absolute alcohol 1 time, centrifugation.Solid after being separated is put into the dry 12h of thermostatic drying chamber, and the temperature of described thermostatic drying chamber is 60 DEG C.The XRD figure of sample is as Fig. 1 a.
embodiment 2
Fe (the NO that molar mass is 0.009mol is got under room temperature
3)
3.9H
2o, is dissolved in the alcohol solvent of 30ml.Ultrasonic 20min in ultrasonic apparatus, makes Fe (NO
3)
3.9H
2o fully dissolves in ethanol.Add sodium lignosulfonate 0.01g, continue ultrasonic 20min.Above-mentioned solution fire is lighted, by gained solid washed with de-ionized water 4 times after perfect combustion, then uses washes of absolute alcohol 1 time, centrifugation.Solid after being separated is put into the dry 12h of thermostatic drying chamber, and the temperature of described thermostatic drying chamber is 60 DEG C.The XRD figure of sample is as Fig. 1 b.
embodiment 3
The FeCl that molar mass is 0.009mol is got under room temperature
3.6H
2o, is dissolved in the alcohol solvent of 30ml.In ultrasonic apparatus, ultrasonic 20min, makes FeCl
3.6H
2o fully dissolves in ethanol.Add sodium lignosulfonate 0.05g, continue ultrasonic 20min.Above-mentioned solution fire is lighted, by gained solid washed with de-ionized water 4 times after perfect combustion, then uses washes of absolute alcohol 1 time, centrifugation.Solid after being separated is put into the dry 12h of thermostatic drying chamber, and the temperature of described thermostatic drying chamber is 60 DEG C.
embodiment 4
The FeCl that molar mass is 0.003mol is got under room temperature
3.6H
2o, is dissolved in the alcohol solvent of 30ml.In ultrasonic apparatus, ultrasonic 20min, makes FeCl
3.6H
2o fully dissolves in ethanol.Add sodium lignosulfonate 0.04g, continue ultrasonic 20min.Above-mentioned solution fire is lighted, by gained solid washed with de-ionized water 4 times after perfect combustion, then uses washes of absolute alcohol 1 time, centrifugation.Solid after being separated is put into the dry 12h of thermostatic drying chamber, and the temperature of described thermostatic drying chamber is 60 DEG C.
embodiment 5
The FeCl that molar mass is 0.006mol is got under room temperature
3.6H
2o, is dissolved in the alcohol solvent of 30ml.In ultrasonic apparatus, ultrasonic 20min, makes FeCl
3.6H
2o fully dissolves in ethanol.Add sodium lignosulfonate 0.01g, continue ultrasonic 20min.Above-mentioned solution fire is lighted, by gained solid washed with de-ionized water 4 times after perfect combustion, then uses washes of absolute alcohol 1 time, centrifugation.Solid after being separated is put into the dry 12h of thermostatic drying chamber, and the temperature of described thermostatic drying chamber is 60 DEG C.
embodiment 6
Fe (the NO that molar mass is 0.006mol is got under room temperature
3)
3.9H
2o, is dissolved in the alcohol solvent of 30ml.Ultrasonic 20min in ultrasonic apparatus, makes Fe (NO
3)
3.9H
2o fully dissolves in ethanol.Add sodium lignosulfonate 0.04g, continue ultrasonic 20min.Above-mentioned solution fire is lighted, by gained solid washed with de-ionized water 4 times after perfect combustion, then uses washes of absolute alcohol 1 time, centrifugation.Solid after being separated is put into the dry 12h of thermostatic drying chamber, and the temperature of described thermostatic drying chamber is 60 DEG C.The XRD figure of sample is as Fig. 1 c.
Claims (1)
1. calcination legal system, for a method for nano-sized iron oxide, is carried out according to following step:
Getting molysite under A, room temperature joins in organic solvent, and wherein the add-on ratio of molysite and organic solvent is (0.003-0.009): 30mol/ml;
B, in ultrasonic apparatus ultrasonic 20min, molysite is fully dissolved in organic solvent;
C, add sulfonated lignin, continue ultrasonic 20min, wherein in the add-on of sulfonated lignin and steps A, the ratio of organic solvent is (0.01-0.05): 30g/ml;
D, above-mentioned solution fire to be lighted;
E, after perfect combustion by gained solid washed with de-ionized water 4 times, then use washes of absolute alcohol 1 time, centrifugation;
F, by be separated after solid put into the dry 12h of thermostatic drying chamber, the temperature of described thermostatic drying chamber is 60 DEG C;
Described molysite is FeCl
36H
2o or Fe (NO
3)
39H
2o;
Described Sulfite lignin are sodium lignosulfonate;
Described organic solvent is ethanol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310534141.7A CN103626238B (en) | 2013-11-01 | 2013-11-01 | Method for preparing nano iron oxide with firing method |
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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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| Publication Number | Publication Date |
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| CN103626238A CN103626238A (en) | 2014-03-12 |
| CN103626238B true CN103626238B (en) | 2015-06-10 |
Family
ID=50207738
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104909412B (en) * | 2015-05-12 | 2016-08-31 | 江苏大学 | A kind of magnetic Fe2o3/ Fe3o4the preparation method of nano heterogeneous body particle |
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2013
- 2013-11-01 CN CN201310534141.7A patent/CN103626238B/en not_active Expired - Fee Related
Non-Patent Citations (1)
| Title |
|---|
| "Surfactant- Assisted Combustion Method for the Synthesis of α-Fe2O3 Nanocrystalline Powders";Y.T. Prabhu et al.;《International Journal of Pure and Applied Sciences and Technology》;20130930;第18卷(第1期);第1-11页 * |
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