CN101373652A - Novel method for preparing Fe3O4/Ag magnetic compound nanometer particle - Google Patents
Novel method for preparing Fe3O4/Ag magnetic compound nanometer particle Download PDFInfo
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- CN101373652A CN101373652A CNA2008100316329A CN200810031632A CN101373652A CN 101373652 A CN101373652 A CN 101373652A CN A2008100316329 A CNA2008100316329 A CN A2008100316329A CN 200810031632 A CN200810031632 A CN 200810031632A CN 101373652 A CN101373652 A CN 101373652A
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Abstract
The invention discloses a novel method for synthesizing a composite nanometer particle of ferroferric oxide coating silver (Fe3O4/Ag). The method is characterized in that the specificity reaction principle of sodium formate and silver carboxylate is utilized, silver ions are reduced to magnetic nano particles of amino-group functionalization, so as to realize the preparation of a sample. The method needs no product purification, is quick and directviewing, and is a novel synthesizing method with simple operation, quickness and high yield.
Description
Affiliated technical field
The present invention relates to a kind of Fe of preparation
3O
4The new method of/Ag 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.The eighties, people recognize that silver is real wide spectrum natural antibiotics, and it has no drug resistance, and is nontoxic, do not have advantages such as irritated, the interference of nothing intersection medicine.Big quantity research finds that silver runs into respiratory enzyme, becomes silver ion and its combination, makes bacterium death.Silver is trace element, and content is higher in prostate, and the raising of silver energy Promote immunity function (supporting that the T cell is to the exotic of lying) so silver is sterilization not only, also helps Growth of Cells, wound healing, and the demand of normal person's silver is 0.1mg/ day.The main application fields of silver: photosensitive material; Ornament materials; Contact material; Composite material; Silver alloy solder; The silver slurry; Energy industry is with silver-colored; The application of silver in catalyst; The application of silver in medicine; Serial anti-biotic material of silver or the like.The development of modern science and technology has opened up more wide prospect for the application of silver.This provides major and immediate significance for research of the present invention.
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.
2007, the electroless plating method such as Cao Xiaoguo, take formaldehyde as reducing agent, preparation Fe
3O
4/ Ag coats composite granule.As additive, formaldehyde is as reducing agent, at Ag[(NH with silane coupler sulfydryl propyl trimethoxy silicane for Zhang Qiaoxin etc.
3)
2]
+Prepare the Fe with nucleocapsid structure in the solution
3O
4/ Ag nano-complex particle.And the Fe of the specific reaction gained that utilizes sodium formate and silver carboxylate that reaches of the present invention
3O
4The method of/Ag nano-complex particle does not also have relevant report at present.
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, soft magnetism is Fe preferably
3O
4/ Ag magnetic compound particles realizes that silver 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/Ag magnetic compound particles comprises the steps:
1) gets the FeCl that molal weight is 1:2 respectively
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, carries out under stirring condition and the N2 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) with a certain amount of above solution and CH for preparing
3The COOAg aqueous solution stirs, and drips HCOONa solution, and reaction is carried out under uniform temperature and rotating speed, and along with constantly carrying out of reaction, mixed solution changes black into gradually by sepia, keep stirring a period of time, and cool to room temperature, institute responds all at N
2Carry out under the protection.
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 uses the specificity principle of sodium formate and silver carboxylate, has prepared the composite magnetic nano particle of the tri-iron tetroxide of silver-colored coating.
2, the present invention can realize the preparation of trace silver magnetic compound particle, and the composite magnetic nano particle of the tri-iron tetroxide that prepared silver coats has monodispersity and higher soft magnetism preferably.
Description of drawings
Fig. 1 is the flow chart of embodiment I.
Embodiment
Embodiment I:
The present invention relates to a kind of sonochemical method and prepare Fe
3O
4/ Ag 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 reactions are 80 ℃ in temperature all, 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 0.4mLAPTES then 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 the solution (1g/L, the Fe that prepare more than the 25ml
3O
4), 0.1mol/L CH
3COOAg aqueous solution 20mL stirs, and drips 0.1mol/L HCOONa solution 10mL, and reaction is at T=35 ℃, carry out under the R=500r/min, along with constantly carrying out of reaction, mixed solution changes black into gradually by sepia, keep stirring 1h, and cool to room temperature, institute responds all at N
2Carry out under the protection.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.Obtain target sample by Magnetic Isolation.
Claims (4)
1. one kind prepares Fe
3O
4The new method of/Ag magnetic composite nanoparticles comprises the steps:
(a) get respectively the FeCl that molal weight is 1:2
24H
2O and FeCl
36H
2O is dissolved in the water, and ultrasonic deoxidation is added drop-wise to above solution in the NaOH solution then, and respond is in 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) with a certain amount of above solution and CH for preparing
3The COOAg aqueous solution stirs, and drips a certain amount of HCOONa solution, and reaction is carried out under uniform temperature and rotating speed, along with constantly carrying out of reaction, mixed solution changes black into gradually by sepia, keeps stirring a period of time, and cool to room temperature, institute responds all at N
2Carry out under the protection.
(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.Obtain target sample by Magnetic Isolation.
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/Ag magnetic composite nanoparticles, it is characterized in that the method for labeled primer in the described step (d) is for amino, in conjunction with source of silver ions is provided, generated in-situ Ag ion is fixed to the magnetic Fe of modifying in advance upper APTES by the complexation reaction between amino-silver ion
3O
4Nanoparticle surface.
4. according to claim 1,3 described a kind of Fe that prepare
3O
4The new method of/Ag magnetic composite nanoparticles is characterized in that utilizing the specific reaction of sodium formate and silver carboxylate, with Ag
+Be reduced to Ag
0, realize the coating of the Ag of magnetic nano-particle.
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|---|---|---|---|
| CNA2008100316329A CN101373652A (en) | 2008-07-01 | 2008-07-01 | Novel method for preparing Fe3O4/Ag magnetic compound nanometer particle |
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|---|---|---|---|
| CNA2008100316329A CN101373652A (en) | 2008-07-01 | 2008-07-01 | Novel method for preparing Fe3O4/Ag magnetic compound nanometer particle |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102716721A (en) * | 2012-07-11 | 2012-10-10 | 蒋彩云 | Novel process for treating lead-containing waste water by Fe3O4/Ag magnetic nuclear shell nanometer material |
| CN102087216B (en) * | 2009-12-03 | 2012-11-21 | 中国科学院生态环境研究中心 | Novel paraquat detecting method |
| CN103198913A (en) * | 2012-01-10 | 2013-07-10 | 中国科学院合肥物质科学研究院 | Silver-ferroferric oxide core-shell nano-particles and preparation method thereof |
| CN107778801A (en) * | 2016-09-20 | 2018-03-09 | 成都测迪森生物科技有限公司 | A kind of porous water-absorbing material |
| CN109671514A (en) * | 2017-10-16 | 2019-04-23 | 中国科学院深圳先进技术研究院 | A kind of preparation method of the magnetic core-shell silver nanowires of flexible transparent electrode |
| 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 |
| CN111041014A (en) * | 2019-12-31 | 2020-04-21 | 浙江工业大学 | Magnetic immobilized lipase and application thereof in resolution of 1-methyl-3-amphetamine |
| CN113498791A (en) * | 2021-07-08 | 2021-10-15 | 广西柳州中和高新技术有限公司 | Ag@Fe3O4@SiC/TiO2Synthesis method and application of nano material |
-
2008
- 2008-07-01 CN CNA2008100316329A patent/CN101373652A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102087216B (en) * | 2009-12-03 | 2012-11-21 | 中国科学院生态环境研究中心 | Novel paraquat detecting method |
| CN103198913A (en) * | 2012-01-10 | 2013-07-10 | 中国科学院合肥物质科学研究院 | Silver-ferroferric oxide core-shell nano-particles and preparation method thereof |
| CN103198913B (en) * | 2012-01-10 | 2016-03-02 | 中国科学院合肥物质科学研究院 | Silver-tri-iron tetroxide core shell nanoparticles and preparation method thereof |
| CN102716721A (en) * | 2012-07-11 | 2012-10-10 | 蒋彩云 | Novel process for treating lead-containing waste water by Fe3O4/Ag magnetic nuclear shell nanometer material |
| CN102716721B (en) * | 2012-07-11 | 2014-01-01 | 蒋彩云 | Novel process for treating lead-containing waste water by Fe3O4/Ag magnetic nuclear shell nanometer material |
| CN107778801A (en) * | 2016-09-20 | 2018-03-09 | 成都测迪森生物科技有限公司 | A kind of porous water-absorbing material |
| CN107778801B (en) * | 2016-09-20 | 2019-10-15 | 莆田市城厢区任西贸易有限公司 | A kind of porous water-absorbing material |
| CN109671514A (en) * | 2017-10-16 | 2019-04-23 | 中国科学院深圳先进技术研究院 | A kind of preparation method of the magnetic core-shell silver nanowires of flexible transparent electrode |
| 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 |
| CN111041014A (en) * | 2019-12-31 | 2020-04-21 | 浙江工业大学 | Magnetic immobilized lipase and application thereof in resolution of 1-methyl-3-amphetamine |
| CN113498791A (en) * | 2021-07-08 | 2021-10-15 | 广西柳州中和高新技术有限公司 | Ag@Fe3O4@SiC/TiO2Synthesis method and application of nano material |
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Open date: 20090225 |