CN101182041A - Preparation method of spherical nano ferric oxide - Google Patents
Preparation method of spherical nano ferric oxide Download PDFInfo
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- CN101182041A CN101182041A CNA2007101585614A CN200710158561A CN101182041A CN 101182041 A CN101182041 A CN 101182041A CN A2007101585614 A CNA2007101585614 A CN A2007101585614A CN 200710158561 A CN200710158561 A CN 200710158561A CN 101182041 A CN101182041 A CN 101182041A
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- ferric oxide
- iron oxide
- cyclodextrin
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a preparation method of spherical nanometer iron oxide, the invention adopts the technical proposal that: cyclodextrine solution is mixed with iron salt solution fully for 1 to 5 hours at normal temperature and pressure and then is filtered, frozen and dried; the obtained products are dried for 10 to 40 hours at the temperature of 30-100 degrees and roasted for 0.5 to 3 hours at the high temperature of 550 to 950 degrees to obtain the spherical nanometer iron oxide particles. The invention has green environmental protection, no pollution, simple and easy operation, good reproducibility and high productivity. The prepared particles of the spherical nanometer iron oxide with defined morphology take the shape of a sphere and have the uniform particle size. Meanwhile, the produced iron oxide of the invention has obvious superior catalytic performance and the COD removal rate thereof reaches 97 percent in the catalytic degradation of phenolic effluent.
Description
Technical field
The present invention relates to the preparation method of ferric oxide, particularly a kind of preparation method of ball shaped nano ferric oxide.
Background technology
Nano material and nanostructure be the most dynamic in the current novel material research field, the future economy and social development are had the very research object of material impact, also be the most active in the nanosecond science and technology, the important component part of approaching application.Nano-sized iron oxide is except the characteristics such as corrosion-resistant, nontoxic with common ferric oxide, also have dispersed height, lovely luster, ultraviolet ray is had characteristics such as good absorption and shielding effect, can be widely used in the industries such as luster coating, printing ink, plastics, leather, automobile finish, gas sensitive, catalyzer, electronics, optical polish agent, biomedical engineering.What usually, have practical value has α-Fe
2O
3, γ-Fe
2O
3, alpha-feooh, Fe
3O
4Deng.Because nano-sized iron oxide has so many advantage and application prospects thereof, in recent years, the investigator has dropped into number of research projects to its preparation and application both at home and abroad.Existing both at home and abroad a lot of different PREPARATION OF NANO FERRIC OXIDE methods, but can be divided into wet method (Wet Method) and dry method (Dry Method) generally.Wet method is many to be raw material with industrial green vitriol, industrial oxidation (Asia) iron or iron nitrate, adopts preparations such as oxidation-precipitation method, hydrothermal method, force water solution or colloid chemistry method; Often [Fe (Co) d or ferrocene (FeCPz) are raw material to dry method, adopt flame thermolysis, vapour deposition, low-temperature plasma chemical Vapor deposition process (PCVD) or the preparation of LASER HEAT decomposition method with iron carbonyl.Because preparation method's complexity, the normal organic substance that uses can pollute environment in the preparation.In addition, preparation has the ferric oxide of certain pattern, needs strict control reaction conditions.
Summary of the invention
The objective of the invention is to overcome the deficiency of above-mentioned prior art, and a kind of green non-pollution, simple to operate, the method for preparing the ball shaped nano ferric oxide that productive rate is high are provided.
Technical scheme of the present invention is: at normal temperatures and pressures, with cyclodextrin soln and iron salt solutions thorough mixing, stir 1～5h after-filtration, lyophilize; Then with the product of gained under 30～100 ℃, behind dry 10～40h,, promptly get the nano oxidized iron particle of spheric 550～950 ℃ of high-temperature roastings 0.5～3 hour.
Described cyclodextrin is: α-ring is stuck with paste or beta-cyclodextrin.
Described molysite is: Fe (NO
3)
39H
2O, K
3Fe (C
2O
4)
33H
2O or Fe (CH
3COO)
24H
2O.
The invention has the beneficial effects as follows: environmental protection of the present invention is pollution-free, and operation is simple, favorable reproducibility, productive rate height.Ball shaped nano iron oxide particles by the present invention's preparation, pass through electron microscopy observation, ferric oxide has specific morphology, be sphere, particle diameter is even, compares with the nano iron oxide catalyst (as the nano particle of no specific morphology, the nano wire of hollow etc.) of existing other structure, and the catalytic performance of ferric oxide of the present invention is obviously superior, when the catalyzed degradation phenolic wastewater, its COD clearance can reach 97%.
Embodiment: the invention will be further elaborated by the following examples.
Embodiment 1: with the Fe (NO of 0.5mmol
3)
39H
2O is dissolved in the 15ml water, joins 15ml and contains in the solution of alpha-cylodextrin of 2.5mmol, and thorough mixing stirs 1h under the room temperature, and gained solution after filtration, obtain yellowish green alpha-cylodextrin and Fe (NO after the freeze-drying
3)
39H
2The inclusion complex of O.With this product dry 15h under 30 ℃, promptly get the nano oxidized iron particle of spheric at 550 ℃ of roasting 0.5h then.
With its as catalyzer in the experiment of catalyzed degradation phenolic wastewater, the clearance that records COD is 92.07%.
Embodiment 2: with the Fe (NO of 0.5mmol
3)
39H
2O is dissolved in the 15ml water, joins 15ml and contains in the solution of beta-cyclodextrin of 1.0mmol, and thorough mixing stirs 2h under the room temperature, and gained solution after filtration, obtain yellowish green beta-cyclodextrin and Fe (NO after the lyophilize
3)
39H
2The inclusion complex of O.With this product dry 10h under 80 ℃, promptly get the nano oxidized iron particle of spheric at 850 ℃ of roasting 1h then.
Is 95.27% with it as catalyzer records COD in the experiment of catalyzed degradation phenolic wastewater clearance.
Embodiment 3: with the K of 0.7mmol
3Fe (C
2O
4)
33H
2O is dissolved in the 15ml water, joins 15ml and contains in the solution of alpha-cylodextrin of 2.0mmol, and thorough mixing stirs 1.5h under the room temperature, and gained solution after filtration, obtain yellowish green alpha-cylodextrin and K after the lyophilize
3Fe (C
2O
4)
33H
2The inclusion complex of O.With this product dry 35h under 60 ℃, promptly get the nano oxidized iron particle of spheric at 650 ℃ of roasting 1.5h then.
Is 96.30% with it as catalyzer records COD in the experiment of catalyzed degradation phenolic wastewater clearance.
Embodiment 4: with the K of 0.4mmol
3Fe (C
2O
4)
33H
2O is dissolved in the 15ml water, joins 15ml and contains in the solution of beta-cyclodextrin of 2.4mmol, and thorough mixing stirs 5h under the room temperature, and gained solution after filtration, obtain yellowish green beta-cyclodextrin and K after the lyophilize
3Fe (C
2O
4)
33H
2The inclusion complex of O.With this product dry 24h under 100 ℃, promptly get the nano oxidized iron particle of spheric at 600 ℃ of roasting 2h then.
Is 97.36% with it as catalyzer records COD in the experiment of catalyzed degradation phenolic wastewater clearance.
Embodiment 5: with the Fe (CH of 0.6mmol
3COO)
24H
2O is dissolved in the 15ml water, joins in the alpha-cylodextrin solution of 15ml 3.0mmol, and thorough mixing stirs 3h under the room temperature, and gained solution after filtration, obtain yellowish green alpha-cylodextrin and Fe (CH after the freeze-drying
3COO)
24H
2The inclusion complex of O.With this product dry 30h under 55 ℃, promptly get the nano oxidized iron particle of spheric at 750 ℃ of roasting 2.5h then.Is 94.61% with it as catalyzer records COD in the experiment of catalyzed degradation phenolic wastewater clearance.
Embodiment 6: with the Fe (CH of 0.3mmol
3COO)
24H
2O is dissolved in the 15ml water, joins 15ml and contains in the solution of beta-cyclodextrin of 3.0mmol, and thorough mixing stirs 3h under the room temperature, and gained solution after filtration, obtain yellowish green beta-cyclodextrin and Fe (CH after the freeze-drying
3COO)
24H
2The inclusion complex of O.With this product dry 40h under 90 ℃, promptly get the nano oxidized iron particle of spheric at 950 ℃ of roasting 3h then.
Is 90.10% with it as catalyzer records COD in the experiment of catalyzed degradation phenolic wastewater clearance.
Claims (4)
1. the preparation method of a ball shaped nano ferric oxide is characterized in that: may further comprise the steps: at normal temperatures and pressures, with cyclodextrin soln and iron salt solutions thorough mixing, stir 1～5h after-filtration, lyophilize; Then with the product of gained under 30～100 ℃, behind dry 10～40h,, promptly get the nano oxidized iron particle of spheric at 550～950 ℃ of high-temperature roasting 0.5～3h.
2. the preparation method of ball shaped nano ferric oxide as claimed in claim 1 is characterized in that: described cyclodextrin is alpha-cylodextrin or beta-cyclodextrin.
3. the preparation method of ball shaped nano ferric oxide as claimed in claim 1 is characterized in that: the mol ratio of cyclodextrin and molysite is 2～10: 1.
4. the preparation method of ball shaped nano ferric oxide as claimed in claim 1 is characterized in that, described molysite is Fe (NO
3)
39H
2O, K
3Fe (C
2O
4)
33H
2O or Fe (CH
3COO)
24H
2O.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007101585614A CN100569661C (en) | 2007-11-27 | 2007-11-27 | A kind of preparation method of ball shaped nano ferric oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007101585614A CN100569661C (en) | 2007-11-27 | 2007-11-27 | A kind of preparation method of ball shaped nano ferric oxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101182041A true CN101182041A (en) | 2008-05-21 |
| CN100569661C CN100569661C (en) | 2009-12-16 |
Family
ID=39447486
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2007101585614A Expired - Fee Related CN100569661C (en) | 2007-11-27 | 2007-11-27 | A kind of preparation method of ball shaped nano ferric oxide |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101366953B (en) * | 2008-10-08 | 2010-10-27 | 东南大学 | Small numerator modified iron oxide nano-granule freeze-dried powder for injection and preparation method thereof |
| CN102172513A (en) * | 2011-03-01 | 2011-09-07 | 上海大学 | Iron-based material with surface modified by cyclodextrin and application thereof |
| RU2453499C2 (en) * | 2009-12-10 | 2012-06-20 | Василий Владимирович Спиридонов | Method of producing water-soluble adducts based on magnetically ordered iron oxides and substituted beta-cyclodextrins |
| CN102730767A (en) * | 2012-06-13 | 2012-10-17 | 湖北工业大学 | Rapid preparation method of nano alpha-iron oxide powder |
| CN106111210A (en) * | 2016-06-24 | 2016-11-16 | 扬州大学 | The preparation method of detachable magnetic microsphere supported precious metal catalyst and method for dismounting thereof |
| WO2018113384A1 (en) * | 2016-12-19 | 2018-06-28 | 山东大学 | One-step method for synthesizing cyclodextrin-modified transition metal oxide material |
| CN108927223A (en) * | 2017-05-25 | 2018-12-04 | 华北电力大学 | A kind of method and its application preparing cyclodextrin@ferroferric oxide/carbon nanotube complex |
-
2007
- 2007-11-27 CN CNB2007101585614A patent/CN100569661C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101366953B (en) * | 2008-10-08 | 2010-10-27 | 东南大学 | Small numerator modified iron oxide nano-granule freeze-dried powder for injection and preparation method thereof |
| RU2453499C2 (en) * | 2009-12-10 | 2012-06-20 | Василий Владимирович Спиридонов | Method of producing water-soluble adducts based on magnetically ordered iron oxides and substituted beta-cyclodextrins |
| CN102172513A (en) * | 2011-03-01 | 2011-09-07 | 上海大学 | Iron-based material with surface modified by cyclodextrin and application thereof |
| CN102730767A (en) * | 2012-06-13 | 2012-10-17 | 湖北工业大学 | Rapid preparation method of nano alpha-iron oxide powder |
| CN106111210A (en) * | 2016-06-24 | 2016-11-16 | 扬州大学 | The preparation method of detachable magnetic microsphere supported precious metal catalyst and method for dismounting thereof |
| CN106111210B (en) * | 2016-06-24 | 2018-06-12 | 扬州大学 | The preparation method and its method for dismounting of detachable magnetic microsphere supported precious metal catalyst |
| WO2018113384A1 (en) * | 2016-12-19 | 2018-06-28 | 山东大学 | One-step method for synthesizing cyclodextrin-modified transition metal oxide material |
| CN108927223A (en) * | 2017-05-25 | 2018-12-04 | 华北电力大学 | A kind of method and its application preparing cyclodextrin@ferroferric oxide/carbon nanotube complex |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100569661C (en) | 2009-12-16 |
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