CN101172665A - Method for producing monodisperse Fe*O* nanocrystal assisted with surface active agent - Google Patents
Method for producing monodisperse Fe*O* nanocrystal assisted with surface active agent Download PDFInfo
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- CN101172665A CN101172665A CNA2006100325066A CN200610032506A CN101172665A CN 101172665 A CN101172665 A CN 101172665A CN A2006100325066 A CNA2006100325066 A CN A2006100325066A CN 200610032506 A CN200610032506 A CN 200610032506A CN 101172665 A CN101172665 A CN 101172665A
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- ethylene glycol
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Abstract
The invention relates to an assistant monodisperse Fe3O4 preparation method of surface activating agent, belonging to the technical filed of the non-metallic material preparation technology. The invention has the technical proposal that dissoluble trivalence malysite is used as the raw material; ethylene glycol is used as reducer; and the monodisperse Fe3O4 nanometer crystal is obtained in the protection effect of double surface activating agents of polyethylene glycol and dodecyl sodium sulfate for reacting for 6 to 96 hours under temperature ranging from 160 DEGC to 180 DEG C, and the grain diameter of the monodisperse Fe3O4 nanometer crystal can be accurately adjusted within 10 to 150nm. The invention has the advantages of low raw material cost, simple device, no pollution during the production process, therbey being capable of producing on scale quickly.
Description
Technical field
The present invention relates to the single Fe of dispersion of a kind of tensio-active agent aid preparation
3O
4Nanocrystalline method, the particularly a kind of couple of single Fe that disperses of tensio-active agent aid preparation
3O
4Nanocrystalline method.
Background technology
Z 250 is extensive in catalyzer, energy and industrial application such as magnetic information storage, magnetic fluid owing to having excellent electromagnetic performance.In recent years, nanocrystalline with magnetic such as Z 250s is kernel, is the key subjects that research that shell is formed the magnetic targeting drug delivery system becomes treatment malignant tumour research field with active drug composition and auxiliary.But studies show that, only less than the particle of 50nm just can pass the liver endotheliocyte or by lymphsystem be sent to spleen and marrow and arrive tumor tissues (Yang Wensheng etc., " nano material and biotechnology ", Chemical Industry Press, 2005.7,160-162).Therefore, prepare that particle diameter is little and controlled, the ferriferrous oxide nano-particle of good evenness and polymolecularity just becomes the precondition of this research field.
The preparation method of Z 250 has three classes at present, i.e. physics method, biological process and chemical method.With the mechanical ball milling method is that the physics method of representative is that particle with micron or submicron order carries out (being generally a week or longer) for a long time and grinds, and is distributed to then in the oil-based media and gets.Although this method is simple to operate, gained particle size distribution broad (nano-micrometre) is not suitable for the magnetic Nano material of bio-medical.Biological process is to utilize biotechnology directly to extract the method for its magnetic particle in the organism that contains the magnetic oxide particle, this method gained magnetic particle has good bio-compatibility, but leaching process is loaded down with trivial details, is difficult for a large amount of the acquisition, and particle diameter is can not system controlled.Chemical method is the main path of preparation Z 250, can be divided into the synthetic and synthetic two lines of solvent thermal of hydro-thermal.Because iron nearly exists 15 kinds of oxide compounds and oxyhydroxide at occurring in nature, and very easy each other conversion, so it is comparatively difficult to obtain purified Z 250 by methods such as hydrolysis or co-precipitation in the aqueous solution.Angew.Chem.Int.Ed.2005,44,2782-2785 and Crystal Growth ﹠amp; Design, 2005,5,393 have reported respectively with solvent-thermal method and have prepared wustite or Z 250, though that they have prepared particle diameter is even, the Z 250 particle of good dispersity, the former gained particle diameter is between 200-800nm; The latter can prepare the very little Z 250 particle of particle diameter, but uses toxic reagent normal hexane and amino dodecane in the preparation process, and tangible Biosafety hidden danger is arranged.
Summary of the invention
The objective of the invention is to problem, a kind of couple of tensio-active agent aid preparation Fe is provided at existing technology of preparing existence
3O
4Method, synthetic Fe
3O
4Nano particle diameter is adjustable in the 10-150nm scope, good dispersity, and building-up process is simple and pollution-free.
The single Fe that disperses of a kind of tensio-active agent aid preparation
3O
4Nanocrystalline method adds solubility trivalent iron salt, sodium-acetate, polyoxyethylene glycol and sodium laurylsulfonate that ultra-sonic dispersion becomes mashed prod in the ethylene glycol successively, and reaction is 6-96 hour under 160-180 ℃ of air tight condition, gained black ferroferric oxide sodium rice corpuscles.
Described trivalent iron salt comprises: iron(ic) chloride, ferric sulfate or iron acetate, add-on are 0.03-0.24mol/L ethylene glycol;
The add-on of described sodium-acetate is a 0.1-0.6mol/L ethylene glycol;
The add-on of described polyoxyethylene glycol (PEG, 6000) is a 20-240g/L ethylene glycol;
The add-on of described sodium laurylsulfonate (SDS) is a 0.04-0.48mol/L ethylene glycol;
The ultrasonic power of described ultra-sonic dispersion is 600-2400W, and ultrasonic frequency is 19-80KHz.
In order to obtain the composite particles of higher degree, can wash with dehydrated alcohol or deionized water particle, to remove various impurity.
The ferriferrous oxide nano crystalline substance of the present invention preparation can be in ethanol ultra-sonic dispersion, adopt nanocrystalline structure and the pattern of scanning electron microscope or transmission electron microscope observation then.The brilliant purity height of the ferriferrous oxide nano that synthesizes (100% is Z 250), the possess hydrophilic property surface, particle diameter is even, good dispersity, the diameter of particle diameter can be in the 10-150 nanometer range accuracy controlling.
The related preparation method's step of the present invention is simple, the scale production that can have high input rapidly, no scale restriction; Temperature of reaction is lower, helps save energy; Equipment is easily purchased, and operation is simple; The synthetic particle diameter is very little and even, is expected to be applied in the magnetic targeting drug delivery system of treatment malignant tumour.
Description of drawings
Fig. 1 is the transmission electron microscope photo of ferriferrous oxide nano crystalline substance;
Fig. 2 is the stereoscan photograph of ferriferrous oxide nano crystalline substance.
Embodiment
The preparation of embodiment 1, ferriferrous oxide nano crystalline substance
3mmol six Ferric Chloride Hydrateds are added in the 25ml ethylene glycol, ultra-sonic dispersion 15 minutes, add 15mmol sodium-acetate, 0.4g polyoxyethylene glycol and 6mmol sodium laurylsulfonate more successively, ultra-sonic dispersion 2 hours, make mixture form uniform sorrel mashed prod, this mixture is transferred to reactor, reacted 24 hours down at 180 ℃, the cooling back obtains atrament at the bottom of still; With dehydrated alcohol or deionized water wash several, the black product that obtains is Z 250 sodium rice crystalline substance.
Synthetic Z 250 sodium rice crystalline substance as shown in Figure 1, nanocrystalline diameter homogeneous is 10nm.
The preparation of embodiment 2, ferriferrous oxide nano crystalline substance
Weighing 3mmol ferric sulfate adds in the 25ml ethylene glycol, ultra-sonic dispersion 15 minutes, add 15mmol sodium-acetate, 0.4g polyoxyethylene glycol and 4mmol sodium laurylsulfonate more successively, ultra-sonic dispersion 2 hours, make mixture form uniform sorrel mashed prod, this mixture is transferred to reactor, reacted 48 hours down at 160 ℃, the cooling back obtains atrament at the bottom of still; With dehydrated alcohol or deionized water wash several, the black product that obtains is Z 250 sodium rice crystalline substance.
Synthetic Z 250 sodium rice crystalline substance as shown in Figure 2, nanocrystalline uniform particle diameter is 130nm.
Claims (1)
1. a tensio-active agent aid preparation list disperses Fe
3O
4Nanocrystalline method, it is characterized in that: solubility trivalent iron salt, sodium-acetate, polyoxyethylene glycol and sodium laurylsulfonate are added successively ultra-sonic dispersion becomes mashed prod in the ethylene glycol, reaction is 6-96 hour under 160-180 ℃ of air tight condition, gets Z 250 sodium rice corpuscles;
Described trivalent iron salt comprises: iron(ic) chloride, ferric sulfate or iron acetate, add-on are 0.03-0.24mol/L ethylene glycol;
The add-on of described sodium-acetate is a 0.1-0.6mol/L ethylene glycol;
The add-on of described polyoxyethylene glycol is a 20-240g/L ethylene glycol;
The add-on of described sodium laurylsulfonate is a 0.04-0.48mol/L ethylene glycol.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100325066A CN100537436C (en) | 2006-11-01 | 2006-11-01 | Method for producing monodisperse Fe3O4 nanocrystal assisted with surface active agent |
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| CNB2006100325066A CN100537436C (en) | 2006-11-01 | 2006-11-01 | Method for producing monodisperse Fe3O4 nanocrystal assisted with surface active agent |
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| CN101172665A true CN101172665A (en) | 2008-05-07 |
| CN100537436C CN100537436C (en) | 2009-09-09 |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101880065A (en) * | 2010-06-04 | 2010-11-10 | 哈尔滨工程大学 | Method for preparing porous ferroferric oxide nano granules for absorbing high-frequency electromagnetic wave |
| CN101901659A (en) * | 2010-07-30 | 2010-12-01 | 北京化工大学 | Preparation method of magnetic nanoparcles modified with surface functional groups |
| CN102097194A (en) * | 2010-12-10 | 2011-06-15 | 北京化工大学 | Method for preparing core-shell structured SiO2/Fe3O4 compound magnetic particle |
| CN102531068A (en) * | 2010-12-31 | 2012-07-04 | 湖南工业大学 | Method for synthesizing lot of mono-dispersed ferroferric oxide (Fe3O4) nano-crystals |
| CN103204547A (en) * | 2012-01-16 | 2013-07-17 | 中国科学院化学研究所 | Ferrum oxyhydroxide and ferrum oxide hierarchical nanostructured material, preparation methods and applications thereof |
| CN103318974A (en) * | 2013-07-04 | 2013-09-25 | 南通宝聚颜料有限公司 | Preparation method of ferroferric oxide magnetic carrier |
| CN106328906A (en) * | 2016-11-03 | 2017-01-11 | 深圳市沃特玛电池有限公司 | Nano spherical lithium iron phosphate positive electrode material and preparation method thereof, lithium iron phosphate positive electrode sheet and lithium iron phosphate battery |
| CN107720832A (en) * | 2017-11-16 | 2018-02-23 | 成都华田生物技术有限公司 | Efficient nanoparticle body emulsion |
| CN110261600A (en) * | 2019-07-02 | 2019-09-20 | 济南大学 | It is a kind of based on ferroso-ferric oxide/prussian blue nano enzyme marker preparation method and application |
| CN114524463A (en) * | 2022-03-18 | 2022-05-24 | 中南大学 | Super-large-size high-length-diameter-ratio ferroferric oxide two-dimensional nanosheet and preparation method thereof |
-
2006
- 2006-11-01 CN CNB2006100325066A patent/CN100537436C/en not_active Expired - Fee Related
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101880065A (en) * | 2010-06-04 | 2010-11-10 | 哈尔滨工程大学 | Method for preparing porous ferroferric oxide nano granules for absorbing high-frequency electromagnetic wave |
| CN101901659A (en) * | 2010-07-30 | 2010-12-01 | 北京化工大学 | Preparation method of magnetic nanoparcles modified with surface functional groups |
| CN102097194A (en) * | 2010-12-10 | 2011-06-15 | 北京化工大学 | Method for preparing core-shell structured SiO2/Fe3O4 compound magnetic particle |
| CN102531068A (en) * | 2010-12-31 | 2012-07-04 | 湖南工业大学 | Method for synthesizing lot of mono-dispersed ferroferric oxide (Fe3O4) nano-crystals |
| CN102531068B (en) * | 2010-12-31 | 2015-02-25 | 湖南工业大学 | Method for synthesizing lot of mono-dispersed ferroferric oxide (Fe3O4) nano-crystals |
| CN103204547A (en) * | 2012-01-16 | 2013-07-17 | 中国科学院化学研究所 | Ferrum oxyhydroxide and ferrum oxide hierarchical nanostructured material, preparation methods and applications thereof |
| CN103318974B (en) * | 2013-07-04 | 2014-12-17 | 南通宝聚颜料有限公司 | Preparation method of ferroferric oxide magnetic carrier |
| CN103318974A (en) * | 2013-07-04 | 2013-09-25 | 南通宝聚颜料有限公司 | Preparation method of ferroferric oxide magnetic carrier |
| CN106328906A (en) * | 2016-11-03 | 2017-01-11 | 深圳市沃特玛电池有限公司 | Nano spherical lithium iron phosphate positive electrode material and preparation method thereof, lithium iron phosphate positive electrode sheet and lithium iron phosphate battery |
| CN107720832A (en) * | 2017-11-16 | 2018-02-23 | 成都华田生物技术有限公司 | Efficient nanoparticle body emulsion |
| CN110261600A (en) * | 2019-07-02 | 2019-09-20 | 济南大学 | It is a kind of based on ferroso-ferric oxide/prussian blue nano enzyme marker preparation method and application |
| CN114524463A (en) * | 2022-03-18 | 2022-05-24 | 中南大学 | Super-large-size high-length-diameter-ratio ferroferric oxide two-dimensional nanosheet and preparation method thereof |
| CN114524463B (en) * | 2022-03-18 | 2023-05-26 | 中南大学 | Super-large-size high-length-diameter-ratio ferroferric oxide two-dimensional nano sheet and preparation method thereof |
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|---|---|
| CN100537436C (en) | 2009-09-09 |
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