CN101293675B - Method for preparing hexagonal disc shaped alpha-Fe2O3 powder - Google Patents
Method for preparing hexagonal disc shaped alpha-Fe2O3 powder Download PDFInfo
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- CN101293675B CN101293675B CN2008100624885A CN200810062488A CN101293675B CN 101293675 B CN101293675 B CN 101293675B CN 2008100624885 A CN2008100624885 A CN 2008100624885A CN 200810062488 A CN200810062488 A CN 200810062488A CN 101293675 B CN101293675 B CN 101293675B
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Abstract
The invention relates to a preparation method of a hexagon-round disciform nanometer powder of alpha-Fe2O3. A water or solvent thermal synthesis is used for respectively dissolving an original reaction material, ferric nitrate and a mineralizer, potassium hydroxide into a mixed solvent which is composed of ethylene glycol and water; then a potassium hydroxide solution is added drop by drop into aferric nitrate solution to get a suspension liquid precursor which is used for the water or solvent thermal reaction; the suspension liquid precursor is sealed into a reactor and is processed by heattreatment for 4 hours to 36 hours at the temperature of 160 DEG C to 240 DEG C to get the hexagonal disciform nanometer powder of alpha-Fe2O3; the thickness of the powder is not more than 150 nanometers and the disk track is not less than 250 nanometers. The products of the invention have the advantages of stable quality, high purity, good particle dispersion and excellent catalyzing property; the preparation process is simple and easy to control, has the advantages of no pollution and low cost and is easy for mass production.
Description
Technical field
The present invention relates to a kind of hexagonal disc shaped alpha-Fe
2O
3The preparation method of nano-powder belongs to field of inorganic nonmetallic material.
Background technology
Nano material is compared with its corresponding block materials, often presents excellent more physics, chemical property.In recent years about nano material studies have shown that the performance of nano-powder material not only is subjected to the influence of its nano-scale, its granule-morphology often also plays decisive influence.Nano oxidized iron material not only has excellent magnetism and catalytic performance more, and has good transparency and to ultraviolet absorption and shielding effect, so as catalyzer, magneticmedium, pigment, in gas sweetening, wastewater treatment, and aspects such as magneticstorage, printing ink, plastics, leather, automobile finish and biomedical engineering are widely used.Wherein, nanometer α-Fe
2O
3As catalyzer, the oxidation or the cracking of high molecular polymer have greatly been promoted.Utilize nanometer α-Fe
2O
3As combustioncatalysts, can make the combustionvelocity of rocket solid propelling agent improve 1～10 times, as catalyst for cracking, can make the rate of cleavage of oil improve 1～5 times.
Solid reaction process, the precipitator method, sol-gel process, hydrolysis method and hydrothermal synthesis method are ferric oxide preparation methods commonly used.Wherein first three methods all need be through the calcining of comparatively high temps, and institute's synthetic powder reuniting is serious, and particle does not have regular appearance.Have only back two kinds of methods, promptly hydrolysis method and hydrothermal method can realize that the control of ferric oxide particles pattern is synthetic.And various granule-morphology α-Fe
2O
3Nano-powder shows different catalytic performances.At present, having only granule-morphology both at home and abroad is spherical, cubes, spindle body, spheroid shape and branch type particulate α-Fe
2O
3Nano-powder synthetic report is not seen hexagonal disc shaped particle α-Fe as yet
2O
3The report of nano-powder.
Summary of the invention
The object of the present invention is to provide a kind of technology simple, the hexagonal disc shaped alpha-Fe that is easy to control
2O
3The preparation method of nano-powder.
Hexagonal disc shaped alpha-the Fe of the present invention's preparation
2O
3Nano-powder, its crystalline network belongs to trigonal system.
The preparation method may further comprise the steps:
1) ethylene glycol and deionized water were mixed the mixed solvent of preparation ethylene glycol and water in 32: 8 by volume～28: 12;
2) iron nitrate is dissolved in the mixed solvent of the ethylene glycol of step 1) preparation and water, compound concentration is the iron nitrate solution of 0.1～0.5mol/L;
3) mol ratio by iron nitrate and potassium hydroxide is 1: 3, and metering takes by weighing potassium hydroxide, potassium hydroxide is dissolved in the mixed solvent of the ethylene glycol of step 1) preparation and water, and compound concentration is the potassium hydroxide solution of 0.3～1.5mol/L;
4) under the state of Jiao Baning, the potassium hydroxide solution of step 3) preparation is added drop-wise to step 2) in the iron nitrate solution of preparation, formation is suspended with iron oxyhydroxide particulate suspension, suspension is transferred in the reactor, make suspension vol account for 2/3～4/5 of reactor volume with the ethylene glycol of step 1) preparation and the mixed solvent adjusting of water, make the suspension in the reactor contain Fe for every liter
3+The mole number of ion and KOH is: 0.15～0.75mol, continue to stir at least 5 minutes;
5) it is airtight to dispose the reactor of reaction mass, 160～240 ℃ down insulation heat-treated in 4～36 hours, then, reduce to room temperature, take out reaction product, filter, clean with deionized water, dehydrated alcohol successively, dry under 60 ℃～100 ℃ temperature, obtain hexagonal disc shaped alpha-Fe
2O
3Nano-powder.
Among the present invention, used iron nitrate, potassium hydroxide, the purity of ethylene glycol and dehydrated alcohol all is not less than chemical pure.
Adopt the prepared α-Fe of the inventive method
2O
3Particle is hexagonal disc shaped, or near discoid.Hexagonal disc shaped alpha-Fe
2O
3Grain thickness is not more than 150 nanometers, and disk track is not less than 250 nanometers.
The present invention is reaction mass with the iron nitrate, and potassium hydroxide is mineralizer, and the mixed solvent of ethylene glycol and water is a reaction solvent, by the volume ratio of ethylene glycol and water in the adjusting mixed solvent, and temperature and time, α-Fe in the regulation and control heat treatment process
2O
3Nanocrystalline crystallization and growth realize hexagonal disc shaped alpha-Fe
2O
3Water/the solvent thermal of nano-powder is synthetic.The present invention is nitrate ion and mineralizer KOH and the synthetic α-Fe that introduces for reaction mass to the cleaning of water/solvent thermal synthetic product
2O
3Nano-powder fully separates, and obtains the α-Fe of pure phase
2O
3Nano-powder.Adopting the dehydrated alcohol dehydration and be not higher than 100 ℃ oven dry, is in order to obtain the α-Fe of favorable dispersity
2O
3Nano-powder.
Technological process of the present invention is simple, is easy to control, non-environmental-pollution, and cost is low, is easy to large-scale production.Hexagonal disc shaped alpha-the Fe that makes
2O
3Grain thickness is not more than 150 nanometers, and disk track is not less than 250 nanometers.Constant product quality, the purity height, the powder granule good dispersity has excellent catalytic performance.
Description of drawings
Fig. 1 synthetic hexagonal disc shaped alpha-Fe of the present invention
2O
3The X-ray diffraction of nano-powder (XRD) collection of illustrative plates;
Fig. 2 synthetic hexagonal disc shaped alpha-Fe of the present invention
2O
3The scanning electronic microscope of nano-powder (SEM) photo;
The pure ammoniumper chlorate of Fig. 3 and be mixed with synthetic hexagonal disc shaped alpha-Fe of the present invention
2O
3Performance for Decomposition of Ammonium Perchlorate differential thermal analysis (DTA) curve of nano-powder.
Embodiment
Further specify the present invention below in conjunction with embodiment.
Example 1
The synthetic thickness of water/solvent thermal is about 100 nanometers, and disk track is about the hexagonal disc shaped alpha-Fe of 300 nanometers
2O
3Nano-powder.
By the synthetic hexagonal disc shaped alpha-Fe of following processing step
2O
3Nano-powder.
1) is respectively to measure ethylene glycol and deionized water at 30: 10 by volume,, obtains ethylene glycol and water volume ratio and be 30: 10 mixed solvent the two mixing.
2) take by weighing 0.005mol (2.05g) iron nitrate (Fe (NO
3)
39H
2O), it is dissolved in the mixed solvent of ethylene glycol that 20ml prepares previously and water, and regulates formed iron nitrate liquid concentration and be: 0.25mol/L (every liter of mole).
3) mol ratio by iron nitrate and potassium hydroxide is 1: 3, metering takes by weighing potassium hydroxide (KOH), promptly take by weighing 0.015mol (1.03g) KOH, it is dissolved in the mixed solvent of ethylene glycol that 20ml prepares previously and water, regulate formed potassium hydroxide solution concentration and be: 0.75mol/L.
4) under the state of Jiao Baning, potassium hydroxide solution is added drop-wise in the iron nitrate solution, forms and be suspended with iron oxyhydroxide particulate suspension presoma.It is transferred in the reactor that useful volume is 50ml, and the mixed solvent of spent glycol and water is regulated and is made its volume account for 4/5 of reactor volume.At this moment Fe
3+The molecular volume mark of ion and KOH is: 0.375mol/L.Continue to stir 30 minutes.
5) it is airtight to dispose the reactor of reaction mass, 200 ℃ down insulation heat-treated in 16 hours.Then, reduce to room temperature, take out reaction product, filter, clean with deionized water, dehydrated alcohol successively, dry under 80 ℃ of temperature, obtain hexagonal disc shaped alpha-Fe2O3 nano-powder.Synthetic hexagonal disc shaped alpha-the Fe of institute
2O
3The X-ray diffraction of nano-powder (XRD) collection of illustrative plates is shown in Fig. 1; Its scanning electronic microscope (SEM) photo is shown in Fig. 2.
With the synthetic hexagonal disc shaped alpha-Fe of institute
2O
3Nano-powder mixes by mass ratio with ammoniumper chlorate at 1: 50, measures the thermolysis differential thermal curve of high ammonium aluminate, observes the variation of ammoniumper chlorate high-temperature decomposition temperature, characterizes its catalytic performance.Find because hexagonal disc shaped alpha-Fe
2O
3The katalysis of nano-powder makes the high-temperature decomposition temperature of ammoniumper chlorate high-temperature decomposition temperature be reduced to 389.2 ℃ by 463.4 ℃, has reduced by 74.2 ℃, and katalysis is remarkable.Fig. 3 is pure ammoniumper chlorate and mixes hexagonal disc shaped alpha-Fe
2O
3Performance for Decomposition of Ammonium Perchlorate differential thermal analysis (DTA) curve of nano-powder.
Example 2
Water/solvent thermal is synthesized hexagonal disc shaped particulate α-Fe
2O
3Nano-powder, thickness are about 80 nanometers, and disk track is about 250 nanometers.
Concrete processing step is identical with example 1, and difference is: the volume ratio of ethylene glycol and water is in the mixed solvent of preparing in the step 1): 28: 12; Step 2) take by weighing the 0.001875mol iron nitrate in, and the iron nitrate solution concentration of preparation is: 0.1mol/L correspondingly take by weighing 0.005625mol potassium hydroxide in the step 3), and the potassium hydroxide solution concentration of preparation is: 0.3mol/L; In the step 4) in the end reaction still reaction precursor liquid suspension account for 3/4 of reactor volume, the molecular volume mark of Fe3+ ion and KOH is in the suspension: 0.15mol/L, stirred then 5 minutes.In the step 5), thermal treatment temp is 160 ℃, is incubated 36 hours.
Example 3
Water/solvent thermal is synthesized hexagonal disc shaped particulate α-Fe
2O
3Nano-powder, thickness are about 150 nanometers, and disk track is about 400 nanometers.
Concrete processing step is identical with example 1, and difference is: the volume ratio of ethylene glycol and water is in the mixed solvent of preparing in the step 1): 32: 8; Step 2) take by weighing the 0.00833mol iron nitrate in, and the iron nitrate solution concentration of preparation is: 0.5mol/L correspondingly take by weighing 0.025mol potassium hydroxide in the step 3), and the potassium hydroxide solution concentration of preparation is: 1.5mol/L; In the step 4) in the end reaction still reaction precursor liquid suspension account for 2/3 of reactor volume, the molecular volume mark of Fe3+ ion and KOH is in the suspension: 0.75mol/L.Stirred then 60 minutes.In the step 5), thermal treatment temp is 240 ℃, is incubated 4 hours.
Claims (2)
1. hexagonal disc shaped alpha-Fe
2O
3The preparation method of nano-powder is characterized in that may further comprise the steps:
1) ethylene glycol and deionized water were mixed the mixed solvent of preparation ethylene glycol and water in 32: 8 by volume～28: 12;
2) iron nitrate is dissolved in the mixed solvent of the ethylene glycol of step 1) preparation and water, compound concentration is the iron nitrate solution of 0.1～0.5mol/L;
3) mol ratio by iron nitrate and potassium hydroxide is 1: 3, and metering takes by weighing potassium hydroxide, potassium hydroxide is dissolved in the mixed solvent of the ethylene glycol of step 1) preparation and water, and compound concentration is the potassium hydroxide solution of 0.3～1.5mol/L;
4) under the state of Jiao Baning, the potassium hydroxide solution of step 3) preparation is added drop-wise to step 2) in the iron nitrate solution of preparation, formation is suspended with iron oxyhydroxide particulate suspension, suspension is transferred in the reactor, make suspension vol account for 2/3～4/5 of reactor volume with the ethylene glycol of step 1) preparation and the mixed solvent adjusting of water, make the suspension in the reactor contain Fe for every liter
3+The mole number of ion and KOH is: 0.15～0.75mol, continue to stir at least 5 minutes;
5) it is airtight to dispose the reactor of reaction mass, 160～240 ℃ down insulation heat-treated in 4～36 hours, then, reduce to room temperature, take out reaction product, filter, clean with deionized water, dehydrated alcohol successively, dry under 60 ℃～100 ℃ temperature, obtain hexagonal disc shaped alpha-Fe
2O
3Nano-powder.
2. according to the described hexagonal disc shaped alpha-Fe of claim 1
2O
3The preparation method of nano-powder is characterized in that used iron nitrate, potassium hydroxide, and the purity of ethylene glycol and dehydrated alcohol all is not less than chemical pure.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101555624B (en) * | 2009-05-06 | 2012-01-11 | 新疆大学 | Synthetic method for uniform mono-dispersion Alpha-Fe2O3 single chip |
| CN103466718A (en) * | 2013-09-06 | 2013-12-25 | 浙江大学 | Method for preparing spindle iron oxide mesoscopic crystal |
| CN106395913B (en) * | 2016-08-26 | 2018-01-09 | 天津大学 | A kind of ferromagnetic nano α Fe with iron defect2O3And preparation method thereof |
| CN107500363B (en) * | 2017-08-16 | 2018-12-28 | 青岛大学 | A kind of preparation method of prism hexa-prism nano iron oxide |
| CN107935055B (en) * | 2018-01-10 | 2020-01-31 | 合肥学院 | layered α -Fe with visible light absorption enhancement2O3Preparation method of nano round cake |
| CN112897592B (en) * | 2021-01-25 | 2022-12-02 | 中国科学院广州地球化学研究所 | Micro-nano iron oxide mineral color developing agent and preparation method and application thereof |
| CN113201766B (en) * | 2021-05-06 | 2022-03-29 | 云南大学 | Preparation method of hematite photoanode |
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