CN102248175A - Method for preparing homodisperse silver nanoparticles by water-in-oil type microemulsion - Google Patents
Method for preparing homodisperse silver nanoparticles by water-in-oil type microemulsion Download PDFInfo
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- CN102248175A CN102248175A CN2011101422793A CN201110142279A CN102248175A CN 102248175 A CN102248175 A CN 102248175A CN 2011101422793 A CN2011101422793 A CN 2011101422793A CN 201110142279 A CN201110142279 A CN 201110142279A CN 102248175 A CN102248175 A CN 102248175A
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Abstract
The invention relates to a method for preparing homodisperse silver nanoparticles by water-in-oil type microemulsion, comprising the following steps of: (1) dissolving silver stearate in toluene at 100-110 DEG C, adding a surfactant, stirring until the solution is clear to obtain a silver stearate toluene solution; diluting hydrazine hydrate by deionized water at ordinary temperature, adding a surfactant, stirring uniformly to obtain a hydrazine hydrate solution; and (2) adding the hydrazine hydrate solution to the silver stearate toluene solution, stirring at 110-120 DEG C for 2-4 hours, and separating, washing and drying the obtained product to obtain the homodisperse silver nanoparticles. The invention has the advantages of simplicity of operation, mild reaction conditions, low cost of experimental raw materials, good economical efficiency and good application prospects, and the obtained silver nanoparticles are 8.7+/-1.1nm and 10.6+/-1.3nm in size, are uniformly dispersed and stably exist in the oil phase.
Description
Technical field
The invention belongs to the preparation field of nano silver particles, the method for the homodisperse nano silver particles of particularly a kind of water-in-oil type prepared with microemulsion reactor.
Background technology
Single dispersed nano silver shows the excellent properties that dimensional effect, skin effect etc. are different from body phase material because of the size of its homogeneous, also is simultaneously the ideal structure primitive that assembling has the functional characteristic nano structural material.Therefore, synthetic single dispersed nano silver has crucial meaning.Oil-soluble nano-Ag particles purposes is very extensive, for example, and can be with the laboratory materials of oil-soluble nano-Ag particles as each big colleges and universities and research institute; Be used for nonpolar and than low pole solution catalysts; Be used for low pole plastic master batch spiral shell and extrude antibacterial additives; Be used for nano-silver conductive printing ink, conducting resinl, plated film, stealth material etc.Meanwhile, the range of application of water-soluble nano silver particle also is very extensive.Materials Academy professor Zhu Meifang of Donghua University unites the independent research of other institutes and goes out the Nano Silver antimicrobial socks, can effectively treat beriberi, and has reached industrialization, and annual return reaches more than 900 ten thousand.We can connect biological micromolecule on the Nano Silver surface that surfactant coats, and carry out the fields such as catalytic reaction in biomarker, biological monitoring, medicament transport and the aqueous solution.
The method for preparing the Nano Silver material commonly used at present mainly contains hydro-thermal method and reverse micelle microemulsion method.Lower and the easy reunion of the particle purity of hydro-thermal method inconvenient operation, preparation, granularity is wayward, and grain diameter is bigger, and the product loss is many, and output is lower.The synthetic nano material of reverse micelle microemulsion method has the character of a lot of excellences, but output is not high, crystallinity is poor.For this reason, need to explore a kind of more efficiently method, synthesize the Nano Silver of good dispersion, output height, good crystallinity.2008, Zhou Xingping etc. adopted oil-water interfaces method [Zhou Xingping etc., Donghua University's journal: natural science edition, 2008,35 (4): 441-444], success synthesizes CdS quantum dot, the CdS quantum dot quantum efficiency height of preparing, narrow diameter distribution, monodispersity is good, and synthetic method is simple, and temperature requirement is low, can produce in a large number, cost is less.2010, Zhou Xingping etc. adopt oil-water interfaces method [Zhou Xingping etc., nanosecond science and technology again; 2010,12:Vol7, No.6], success synthesize the ZnS quantum dot, and some rare metals that mix, fluorescence property is good, is a kind of good semi-conducting material.
Summary of the invention
Technical problem to be solved by this invention provides the method for the homodisperse nano silver particles of a kind of water-in-oil type prepared with microemulsion reactor, and this method is simple to operate, reaction condition is gentle, and the nano-Ag particles that obtains is uniformly dispersed, and is stable, has a good application prospect.
The method of a kind of water-in-oil type prepared with microemulsion reactor nano silver particles of the present invention comprises:
(1) silver stearate is dissolved in the toluene under 100～110 ℃, adds mol ratio with silver stearate and be 1: 10～12 surfactant, be stirred to solution clarify the silver stearate toluene solution; Hydrazine hydrate at normal temperatures with deionized water dilution, is added mol ratio with hydrazine hydrate and is 1: 18～20 surfactant, stir hydrazine hydrate solution;
(2) above-mentioned hydrazine hydrate solution is joined in the above-mentioned silver stearate toluene solution,, the product that obtains is carried out separating, washing, drying, promptly get homodisperse nano silver particles at 110～120 ℃ of electronic stirrings of following upper oil phase, the water magnetic agitation 2～4h of lower floor.
Silver stearate toluene solution concentration in the described step (1) is 0.03-0.05M.
Hydrazine hydrate solution concentration in the described step (1) is 0.0075-0.0125M.
Surfactant in the described step (1) is lauryl sodium sulfate (SDS) or enuatrol.
Silver stearate toluene solution in the described step (2) and hydrazine hydrate solution volume ratio are 1: 1～2.
Separating, washing in the described step (2) is specially successively with behind the absolute ethyl alcohol and behind the deionized water rinsing, isolates upper oil phase solution, and centrifugation 15min under 11000rmp uses the absolute ethyl alcohol wash products, again centrifugation 15min under 11000rmp.
Drying in the described step (2) is in 65～70 ℃ of drying 2～4h.
The average diameter of Nano Silver is 7.6～9.8nm and 9.3～11.9nm in the described step (2).
Beneficial effect
(1) the present invention is simple to operate, reaction condition is gentle, and experimental raw is cheap, good economy performance;
(2) the nano-Ag particles size that obtains of the present invention is 8.7 ± 1.1nm and 10.6 ± 1.3nm, is uniformly dispersed, and in the stable existence oil phase, has a good application prospect.
Description of drawings
Fig. 1 is the process chart of embodiment 1 and 2;
Fig. 2 is the transmission electron microscope picture of embodiment 1 products therefrom at oil phase;
Fig. 3 is the particle diameter distribution map of embodiment 1 products therefrom at oil phase;
Fig. 4 is the transmission electron microscope picture of embodiment 1 products therefrom at water;
Fig. 5 is the particle diameter distribution map of embodiment 1 products therefrom at water;
Fig. 6 is the ultraviolet absorpting spectrum of embodiment 1 products therefrom, and the product absworption peak appears at 412nm in the oil phase; Water-phase product absworption peak position appears at the 414nm place;
Fig. 7 is the transmission electron microscope picture of embodiment 2 products therefroms;
Fig. 8 is the particle diameter distribution map of embodiment 2 products therefroms.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
1, take by weighing 0.99g (0.00253mol) silver stearate, be dissolved in fully in the 85ml toluene under 110 ℃, take by weighing 8.2368g (0.0286mol) SDS and join in the toluene, magnetic agitation is transparent to solution, preserves standby;
2, measure 0.25ml (10.3M) hydrazine hydrate solution and be diluted in the 105ml deionized water, be made into the hydrazine hydrate solution that concentration is about 0.0125M, take by weighing in the hydrazine hydrate solution after 7.2g (0.025mol) SDS joins dilution, magnetic agitation is even, preserves standby;
3, join in the hydrazine hydrate solution 30min with step 2 preparation in the silver stearate toluene solution of step 1 preparation, 110 ℃ of electronic stirrings of following upper oil phase, the water magnetic agitation 2h of lower floor (volume ratio of oil phase and water is 1: 1.2).After reaction finished, solution was divided into significantly two-layer; The upper strata is dark red brown, and lower floor is almost transparent.Then profit two is separated.Take out 1ml oil phase and water respectively, with 25ml toluene and deionized water dilution, ultrasonic respectively, do the test of TEM and ultraviolet.In the residue oil phase, add the 50ml absolute ethanol washing, centrifugation 15min under 11000rmp then, clear up deposit twice with absolute ethyl alcohol again, centrifugation 15min under 11000rmp again, at last very with deposit in vacuum drying chamber, dry 2h under 65 ℃ finally obtains the higher Nano Silver material of purity.TEM figure shows that the product average grain diameter is 8.7 ± 1.1nm, spherical in shape, almost approaching single dispersion, and almost do not have agglomeration.
Embodiment 2
1, take by weighing 0.99g (0.00253mol) silver stearate, be dissolved in fully in the 85ml toluene under 110 ℃, take by weighing 8.2368g (0.0286mol) SDS and join in the toluene, magnetic agitation is transparent to solution, preserves standby;
2, measuring 0.25ml (10.3M) hydrazine hydrate solution is diluted in the 105ml deionized water, be made into concentration and be about the hydrazine hydrate solution of 0.0125M, take by weighing in the hydrazine hydrate solution after 8.208g (0.027mol) enuatrol joins dilution, magnetic agitation is even, preserves standby;
3, join in the hydrazine hydrate solution 30min with step 2 preparation in the silver stearate toluene solution of step 1 preparation, 110 ℃ of electronic stirrings of following upper oil phase, the water magnetic agitation 2h of lower floor (volume ratio of oil phase and water is 1: 1.2).After reaction finished, solution was divided into significantly two-layer; The upper strata is dark red brown, and lower floor is almost transparent.Then profit two is separated.Take out 1ml oil phase and water respectively, with 25ml toluene and deionized water dilution, ultrasonic respectively, do the TEM test.In the residue oil phase, add the 50ml absolute ethanol washing, centrifugation 15min under 11000rmp then, clear up deposit twice with absolute ethyl alcohol again, centrifugation 15min under 11000rmp again, at last very with deposit in vacuum drying chamber, dry 2h under 65 ℃ finally obtains the higher Nano Silver material of purity.TEM figure shows that the product average grain diameter is 10.6 ± 1.3nm, spherical in shape, almost approaching single dispersion, and almost do not have agglomeration.
Embodiment 3
1, take by weighing 1.9941g (0.0051mol) silver stearate, be dissolved in fully in the 100ml toluene under 100 ℃, take by weighing 14.4g (0.05mol) SDS and join in the toluene, magnetic agitation is transparent to solution, preserves standby;
2, measuring 0.07ml (10.3M) hydrazine hydrate solution is diluted in the 101ml deionized water, be made into concentration and be about the hydrazine hydrate solution of 0.0075M, take by weighing in the hydrazine hydrate solution after 4.56g (0.015mol) enuatrol joins dilution, magnetic agitation is even, preserves standby;
3, join in the hydrazine hydrate solution 30min with step 2 preparation in the silver stearate toluene solution of step 1 preparation, 120 ℃ of electronic stirrings of following upper oil phase, the water magnetic agitation 4h of lower floor (volume ratio of oil phase and water is 1: 2).After reaction finished, solution was divided into significantly two-layer; The upper strata is dark red brown, and lower floor is almost transparent.Then profit two is separated.Take out 1ml oil phase and water respectively, with 25ml toluene and deionized water dilution, ultrasonic respectively.In the residue oil phase, add the 50ml absolute ethanol washing, centrifugation 15min under 11000rmp then, clear up deposit twice with absolute ethyl alcohol again, centrifugation 15min under 11000rmp again, at last very with deposit in vacuum drying chamber, dry 4h under 70 ℃ finally obtains the higher Nano Silver material of purity.
Claims (8)
1. the method for the homodisperse nano silver particles of water-in-oil type prepared with microemulsion reactor comprises:
(1) silver stearate is dissolved in the toluene under 100～110 ℃, adds mol ratio with silver stearate and be 1: 10～12 surfactant, be stirred to solution clarify the silver stearate toluene solution; Hydrazine hydrate at normal temperatures with deionized water dilution, is added mol ratio with hydrazine hydrate and is 1: 18～20 surfactant, stir hydrazine hydrate solution;
(2) above-mentioned hydrazine hydrate solution is joined in the above-mentioned silver stearate toluene solution,, the product that obtains is carried out separating, washing, drying, promptly get homodisperse nano silver particles at 110～120 ℃ of electronic stirrings of following upper oil phase, the water magnetic agitation 2～4h of lower floor.
2. the method for the homodisperse nano silver particles of a kind of water-in-oil type prepared with microemulsion reactor according to claim 1 is characterized in that: the silver stearate toluene solution concentration in the described step (1) is 0.03-0.05M.
3. the method for the homodisperse nano silver particles of a kind of water-in-oil type prepared with microemulsion reactor according to claim 1, it is characterized in that: the hydrazine hydrate solution concentration in the described step (1) is 0.0075-0.0125M.
4. the method for the homodisperse nano silver particles of a kind of water-in-oil type prepared with microemulsion reactor according to claim 1, it is characterized in that: the surfactant in the described step (1) is lauryl sodium sulfate or enuatrol.
5. the method for the homodisperse nano silver particles of a kind of water-in-oil type prepared with microemulsion reactor according to claim 1, it is characterized in that: silver stearate toluene solution in the described step (2) and hydrazine hydrate solution volume ratio are 1: 1～2.
6. the method for the homodisperse nano silver particles of a kind of water-in-oil type prepared with microemulsion reactor according to claim 1, it is characterized in that: the separating, washing in the described step (2) is specially successively with behind the absolute ethyl alcohol and behind the deionized water rinsing, isolate upper oil phase solution, centrifugation 15min under 11000rmp, use the absolute ethyl alcohol wash products, again centrifugation 15min under 11000rmp.
7. the method for the homodisperse nano silver particles of a kind of water-in-oil type prepared with microemulsion reactor according to claim 1 is characterized in that: the drying in the described step (2) is in 65～70 ℃ of drying 2～4h.
8. the method for the homodisperse nano silver particles of a kind of water-in-oil type prepared with microemulsion reactor according to claim 1 is characterized in that: the average diameter of Nano Silver is 7.6～9.8nm and 9.3～11.9nm in the described step (2).
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Cited By (5)
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| CN102886529A (en) * | 2012-10-30 | 2013-01-23 | 东华大学 | Method for preparing oil soluble nano silver particles by adopting oil-water interface method with hydrazine hydrate as reducing agent |
| CN105057690A (en) * | 2015-07-20 | 2015-11-18 | 昆明理工大学 | Preparation method of high-dispersibility superfine spherical silver powder |
| CN105268994A (en) * | 2015-12-02 | 2016-01-27 | 广东南海启明光大科技有限公司 | Preparation method for emulsion containing nano-silver particles |
| CN107457502A (en) * | 2017-07-06 | 2017-12-12 | 桂林电子科技大学 | A kind of process that nano mattisolda is prepared based on Reverse Microemulsion System |
| CN108568530A (en) * | 2018-05-04 | 2018-09-25 | 青岛科技大学 | A method of by surfactant-free microemulsion reaction methods Nano silver grain |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102886529A (en) * | 2012-10-30 | 2013-01-23 | 东华大学 | Method for preparing oil soluble nano silver particles by adopting oil-water interface method with hydrazine hydrate as reducing agent |
| CN105057690A (en) * | 2015-07-20 | 2015-11-18 | 昆明理工大学 | Preparation method of high-dispersibility superfine spherical silver powder |
| CN105057690B (en) * | 2015-07-20 | 2017-08-25 | 昆明理工大学 | A kind of preparation method of polymolecularity superfine spherical silver powder |
| CN105268994A (en) * | 2015-12-02 | 2016-01-27 | 广东南海启明光大科技有限公司 | Preparation method for emulsion containing nano-silver particles |
| CN107457502A (en) * | 2017-07-06 | 2017-12-12 | 桂林电子科技大学 | A kind of process that nano mattisolda is prepared based on Reverse Microemulsion System |
| CN107457502B (en) * | 2017-07-06 | 2019-08-20 | 桂林电子科技大学 | A kind of process preparing nano mattisolda based on Reverse Microemulsion System |
| CN108568530A (en) * | 2018-05-04 | 2018-09-25 | 青岛科技大学 | A method of by surfactant-free microemulsion reaction methods Nano silver grain |
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