CN101345111A - Novel method of manufacturing Fe3O4/Pt magnetic complex nano particle - Google Patents
Novel method of manufacturing Fe3O4/Pt magnetic complex nano particle Download PDFInfo
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- CN101345111A CN101345111A CNA2008100313496A CN200810031349A CN101345111A CN 101345111 A CN101345111 A CN 101345111A CN A2008100313496 A CNA2008100313496 A CN A2008100313496A CN 200810031349 A CN200810031349 A CN 200810031349A CN 101345111 A CN101345111 A CN 101345111A
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Abstract
The invention discloses a novel method used for synchronizing Fe3O4/Pt magnetic composite nanometer particles, which is characterized in that under the ultrasonic condition, by hydrazine hydrate, platinum ion is reduced onto amido or mercapto functional magnetic nanometer particles, thus realizing the preparation of samples. The method of the invention requires no purification of product, is quick and visible, and is a novel synthesis method with simple and quick operation and high yield.
Description
Affiliated technical field
The present invention relates to a kind of Fe of preparation
3O
4The new method of/Pt magnetic composite nanoparticles.
Background technology
Metal or nonmetal functionalization ferriferous oxide nano particle can be protected the ferriferous oxide nano particle preferably; make it more stable; and extended its scope of application greatly; especially enlarge its biomedical applications scope, and the metal simple-substance in the preparation research of metal simple-substance (or non-metal simple-substance) functional magnetic ferriferous oxide composite nanoparticle mainly concentrates on gold, silver, cobalt, platinum, palladium (Au, Ag; Co; Pt Pd) waits on the simple substance, is carbon (C) simple substance and non-metal simple-substance is mainly studied.For precious metals pt, platinum catalyst is widely used in aspects such as chemical, petrochemical industry, environmental improvement, fuel cell.The consumption of nano platinum particle energy Effective Raise catalytic activity, catalytic efficiency, reduction platinum, thus significant to its research.Consider magnetic platinum composite nanoparticle a kind of good solution of can yet be regarded as based on the recovery aspect of precious metals platinum catalyst.Yet at present main in the majority with preparation and the application study of Fe/Pt alloy.In addition, Teng etc. have prepared Pt/ ferriferous oxide magnetic composite nanoparticles, but the research report of ferriferous oxide/Pt magnetic composite nanoparticles is also seldom found.
In addition, sonochemical method be utilize the high temperature that cavitation effect of ultrasonic waves moment produces (〉=5000K), high pressure (〉=20MPa) and cooldown rate (10
10K/s) etc. extreme condition is impelled the nano particle for preparing of reactions such as oxidation, reduction, decomposition and hydrolysis.The main cause that ultrasonic wave works to chemical reaction is " the ultrasonic wave vaporization bubble " that ultrasonic wave produces, and it forms local high temperature and high pressure environment and the microjet with intense impact power.The ultrasonic cavitation effect is compared with traditional stirring technique, and easier realization homogeneous media is mixed, and eliminates the local concentration inequality, improves reaction speed, promotes the formation of cenotype, and can also play shear action to reuniting, and is conducive to the formation of molecule.In 2003, Li etc. prepared the Fe-Co magnetic composite nanoparticles with nucleocapsid structure with regard to the method for utilizing sonochemistry, and Nikitenko etc. have prepared Fe-Fe by the method for sonochemistry
3The nanocrystalline particle of C, we have synthesized ferriferous oxide/Au magnetic composite nanoparticles in 2007 with the method for sonochemistry, but do not find to utilize the relevant report of the synthetic ferriferous oxide/Pt of this method as yet.
Goal of the invention
The objective of the invention is for a kind of new method of composite magnetic nano particle preparation is provided, so that preparation has monodispersity, the Fe that saturation magnetization is high
3O
4/ Pt magnetic compound particles realizes that platinum coats thickness and magnetic saturation intensity is controlled, and the composite magnetic nano particle of the advantage such as it is simple to have reactions steps, and the reaction time is short, and is easy and simple to handle.
Summary of the invention
Purpose of the present invention realizes by following proposal:
Fe
3O
4The sonochemical method preparation of/Pt magnetic compound particles comprises the steps:
1) getting molal weight respectively is 1: 2 FeCl
24H
2O and FeCl
36H
2O is dissolved in the water, and ultrasonic deoxidation is added to above drips of solution in the NaOH solution then, and all are reflected at uniform temperature, stirring condition and N
2Carry out under the protection.Along with the carrying out of reaction, the precipitation of black appears in the reactant liquor.
2) after reaction finishes, utilize externally-applied magnetic field that the gained precipitation is separated from reaction medium, and successively clean with deionized water and ethanol.At last with Fe
3O
4Nano particle is made into certain density ethanolic solution.
3) in order to disperse better Fe
3O
4Particle, with the second alcohol and water that above gained solution dilution is also further ultrasonic.Drip a certain amount of APTES then in above mixed solution, stir under the room temperature.At last, the Fe that utilizes centrifuge that APTES is modified
3O
4Nano particle separates from reaction medium, and with ethanolic solution it is cleaned.Before next step reaction, the Fe that APTES modifies
3O
4Nano particle is made into certain density ethanolic solution.
4) solution and the chloroplatinic acid aqueous solution with above preparation is distributed in the deionized water, stirs, and drips hydrazine hydrate solution, under certain frequency, under the room temperature ultrasonic up to the reaction solution color by the light yellow black that becomes gradually, last precipitation solution becomes colorless.
5) after reaction finishes, utilize permanent magnet that magnetic nanoparticle is isolated from solution, and with washed with de-ionized water 3 times, the residual solution after the separation present colourless.
The present invention has following advantage compared to existing technology:
1, the present invention has used sonochemical method to prepare the composite magnetic nano particle of the tri-iron tetroxide that platinum coats, and overcome the defective of conventional method cost height, time-consuming, effort, moreover the present invention can realize the preparation of trace platinum magnetic compound particle.Therefore, the present invention has low, quick, easy, the advantage accurately of cost.
2, the present invention can adopt the supersonic frequency realization to the control of reaction speed in whole experimentation, is conducive to the remarkable shortening in reaction time.
3, the composite magnetic nano particle of the tri-iron tetroxide of the platinum coating of the present invention's preparation has monodispersity, and high saturation and magnetic intensity can be realized the control of platinum coating thickness by the number of repetition of step (3), and then realizes the control of particle magnetic.
Description of drawings
Fig. 1 is the flow chart of embodiment I.
Embodiment
Embodiment 1:
The present invention relates to a kind of sonochemical method and prepare Fe
3O
4/ Pt magnetic compound particles.Specific as follows: as 1) to get 2gFeCl respectively
24H
2O and 5.2g FeCl
36H
2The concentrated hydrochloric acid 0.85mL of O and 12.1mol/L is dissolved in 200mL H
2Among the O, ultrasonic deoxidation is added to 250mL with above drips of solution then, and in the 0.75mol/L NaOH solution, all are reflected at temperature is 80 ℃, stirs N
2Carry out under the protection.Along with the carrying out of reaction, the precipitation of black appears in the reactant liquor.After reaction finishes, utilize externally-applied magnetic field that the gained precipitation is separated from reaction medium, and successively use washed with de-ionized water 3 times, ethanol cleans 2 times.At last with Fe
3O
4Nano particle is made into the ethanolic solution that concentration is 5g/L.2) with ethanol and 1mL water with the above gained solution dilution of 25mL to 150mL, in order to disperse better Fe
3O
4Particle needs the further ultrasonic 30min of this solution.Drip then 0.4mL APTES in above mixed solution, stir 7h under the room temperature.At last, utilize centrifuge 10000r/min, the Fe that 30min modifies APTES
3O
4Nano particle separates from reaction medium, and with ethanolic solution it is cleaned 5 times.Before next step reaction, the Fe that APTES modifies
3O
4Nano particle is made into the ethanolic solution that concentration is 1g/L.3) with 15mLAPTES-Fe
3O
4The chloroplatinic acid aqueous solution 10mL of solution (5g/L), 0.1mol/L is distributed in the 100mL deionized water, stir, drip the 16mL hydrazine hydrate solution, be under the 80kHz condition in supersonic frequency, ultrasonic until reaction solution color by the light yellow flocculence material that becomes gradually, becomes atrament again and follows the generation of bubble under the room temperature.
Claims (4)
1, a kind of Fe for preparing
3O
4The new method of/Pt magnetic composite nanoparticles comprises the steps:
(a) getting molal weight respectively is 1: 2 FeCl
24H
2O and FeCl
36H
2O is dissolved in the water, and ultrasonic deoxidation is added to above drips of solution in the NaOH solution then, and all are reflected at uniform temperature, stirring condition and N
2Carry out under the protection.Along with the carrying out of reaction, the precipitation of black appears in the reactant liquor.
(b) after reaction finishes, utilize externally-applied magnetic field that the gained precipitation is separated from reaction medium, and successively clean with deionized water and ethanol.At last with Fe
3O
4Nano particle is made into certain density ethanolic solution.
(c) use the second alcohol and water with above gained solution dilution, in order to disperse better Fe
3O
4Particle needs this solution is further ultrasonic.Drip a certain amount of APTES then in above mixed solution, stir under the room temperature.At last, the Fe that utilizes centrifuge that APTES is modified
3O
4Nano particle separates from reaction medium, and with ethanolic solution it is cleaned.Before next step reaction, the Fe that APTES modifies
3O
4Nano particle is made into certain density ethanolic solution.
(d) solution and the chloroplatinic acid aqueous solution with above preparation is distributed in the deionized water, stir, drip citric acid and receive solution, under certain frequency, under the room temperature ultrasonic up to the reaction solution color by the light yellow black that becomes gradually, solution becomes colorless after the last black precipitate.
(e) after reaction finishes, utilize permanent magnet that magnetic nanoparticle is isolated from solution, and with washed with de-ionized water 3 times, the residual solution after the separation present colourless.
2, the method for tri-iron tetroxide preparation according to claim 1 is characterized in that improving traditional coprecipitation method.
3, according to claim 1,2 described a kind of Fe that prepare
3O
4The new method of/Pt magnetic composite nanoparticles is characterized in that the method for labeled primer in the described step (c) for amino, by the complexation reaction combination between amino-platinum ion, realizes that the platinum of magnetic nano-particle coats, and compound particle is in conjunction with very firm.
4, according to claim 1,3 described a kind of Fe that prepare
3O
4The new method of/Pt magnetic composite nanoparticles is characterized in that the ultrasonic frequency range that adopts can realize the direct control to the reaction time.
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| CNA2008100313496A CN101345111A (en) | 2008-05-20 | 2008-05-20 | Novel method of manufacturing Fe3O4/Pt magnetic complex nano particle |
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|---|---|---|---|
| CNA2008100313496A CN101345111A (en) | 2008-05-20 | 2008-05-20 | Novel method of manufacturing Fe3O4/Pt magnetic complex nano particle |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101791702A (en) * | 2010-03-04 | 2010-08-04 | 西安交通大学 | Method for preparing nano sheets of platinum |
| CN102211201A (en) * | 2011-05-16 | 2011-10-12 | 西安交通大学 | Method for preparing Pt, Pd and Pt-M (M is Cu, Ag and Pd) alloy nanoparticles |
| CN102225785A (en) * | 2011-04-26 | 2011-10-26 | 东华大学 | Preparation method of APTS (aminopropyltriethoxysilane)-modified iron oxide magnetic nanoparticles |
| CN102554263A (en) * | 2012-02-23 | 2012-07-11 | 河南大学 | Preparation method for Cu/Fe3O4 composite nanoparticles having good dispersity in organic medium |
| CN103657643A (en) * | 2013-10-10 | 2014-03-26 | 南京工业大学 | Method for preparing nano palladium metal catalyst |
| CN103706395A (en) * | 2013-12-23 | 2014-04-09 | 南京工业大学 | Nano ruthenium catalyst and application thereof |
| CN104531119A (en) * | 2015-01-09 | 2015-04-22 | 哈尔滨工业大学 | Method for preparing supported metallic catalyst based on Fe3O4 |
| CN104841455A (en) * | 2015-04-24 | 2015-08-19 | 华东理工大学 | Preparation method and application of platinum-loaded ferriferrous oxide catalyst |
| CN109604625A (en) * | 2019-02-20 | 2019-04-12 | 哈尔滨工业大学 | A method of using transition metal oxide and platinum metal nano-particle as precursor preparation platinum base binary alloy nano particle |
| CN110157741A (en) * | 2019-04-29 | 2019-08-23 | 华中科技大学 | A kind of magnetic nano-particle, preparation method and the application in transfection reagent |
| CN110336031A (en) * | 2019-06-28 | 2019-10-15 | 陕西科技大学 | A kind of sulphur load molybdenum oxide/graphene hollow structure electrode material preparation method |
| CN111773245A (en) * | 2020-06-24 | 2020-10-16 | 东南大学 | Composite nano enzyme and preparation method and application thereof |
| CN112893834A (en) * | 2021-01-20 | 2021-06-04 | 东北大学 | L10-FePt@PtBi2Bi core-shell structure nano-particles and one-step synthesis method thereof |
-
2008
- 2008-05-20 CN CNA2008100313496A patent/CN101345111A/en active Pending
Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101791702A (en) * | 2010-03-04 | 2010-08-04 | 西安交通大学 | Method for preparing nano sheets of platinum |
| CN102225785A (en) * | 2011-04-26 | 2011-10-26 | 东华大学 | Preparation method of APTS (aminopropyltriethoxysilane)-modified iron oxide magnetic nanoparticles |
| CN102225785B (en) * | 2011-04-26 | 2013-05-08 | 东华大学 | Preparation method of APTS (aminopropyltriethoxysilane)-modified iron oxide magnetic nanoparticles |
| CN102211201A (en) * | 2011-05-16 | 2011-10-12 | 西安交通大学 | Method for preparing Pt, Pd and Pt-M (M is Cu, Ag and Pd) alloy nanoparticles |
| CN102211201B (en) * | 2011-05-16 | 2012-11-28 | 西安交通大学 | Method for preparing Pt, Pd and Pt-M (M is Cu, Ag and Pd) alloy nanoparticles |
| CN102554263A (en) * | 2012-02-23 | 2012-07-11 | 河南大学 | Preparation method for Cu/Fe3O4 composite nanoparticles having good dispersity in organic medium |
| CN103657643B (en) * | 2013-10-10 | 2015-09-02 | 南京工业大学 | A kind of method preparing nano palladium metal catalyst |
| CN103657643A (en) * | 2013-10-10 | 2014-03-26 | 南京工业大学 | Method for preparing nano palladium metal catalyst |
| CN103706395B (en) * | 2013-12-23 | 2016-08-17 | 南京工业大学 | A kind of nano-ruthenium catalyst and application |
| CN103706395A (en) * | 2013-12-23 | 2014-04-09 | 南京工业大学 | Nano ruthenium catalyst and application thereof |
| CN104531119A (en) * | 2015-01-09 | 2015-04-22 | 哈尔滨工业大学 | Method for preparing supported metallic catalyst based on Fe3O4 |
| CN104841455A (en) * | 2015-04-24 | 2015-08-19 | 华东理工大学 | Preparation method and application of platinum-loaded ferriferrous oxide catalyst |
| CN109604625B (en) * | 2019-02-20 | 2022-03-22 | 哈尔滨工业大学 | Method for preparing platinum-based binary alloy nanoparticles by using transition metal oxide and platinum metal nanoparticles as precursors |
| CN109604625A (en) * | 2019-02-20 | 2019-04-12 | 哈尔滨工业大学 | A method of using transition metal oxide and platinum metal nano-particle as precursor preparation platinum base binary alloy nano particle |
| CN110157741A (en) * | 2019-04-29 | 2019-08-23 | 华中科技大学 | A kind of magnetic nano-particle, preparation method and the application in transfection reagent |
| CN110157741B (en) * | 2019-04-29 | 2021-07-27 | 华中科技大学 | Magnetic nano particle, preparation method thereof and application thereof in transfection reagent |
| CN110336031A (en) * | 2019-06-28 | 2019-10-15 | 陕西科技大学 | A kind of sulphur load molybdenum oxide/graphene hollow structure electrode material preparation method |
| CN111773245A (en) * | 2020-06-24 | 2020-10-16 | 东南大学 | Composite nano enzyme and preparation method and application thereof |
| CN111773245B (en) * | 2020-06-24 | 2022-04-12 | 东南大学 | Composite nano enzyme and preparation method and application thereof |
| CN112893834A (en) * | 2021-01-20 | 2021-06-04 | 东北大学 | L10-FePt@PtBi2Bi core-shell structure nano-particles and one-step synthesis method thereof |
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Open date: 20090114 |