CN102886527B - Method for preparing cubic crystal form nano-silver material by using oleic acid silver as raw material based on oil-water interface method - Google Patents
Method for preparing cubic crystal form nano-silver material by using oleic acid silver as raw material based on oil-water interface method Download PDFInfo
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- CN102886527B CN102886527B CN201210385250.2A CN201210385250A CN102886527B CN 102886527 B CN102886527 B CN 102886527B CN 201210385250 A CN201210385250 A CN 201210385250A CN 102886527 B CN102886527 B CN 102886527B
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Abstract
The invention relates to a method for preparing cubic crystal form nano-silver material by using oleic acid silver as raw material based on an oil-water interface method. The method comprises the steps of: (1) dissolving the oleic acid silver into cyclohexane at the temperature of 80 DEG C, adding surface active agent into the solution, and stirring until the solution is clear and transparent to obtain silver precursor; dissolving sodium borohydride into deionized water at the room temperature, and evenly stirring to obtain borohydride precursor; and (2) adding the obtained borohydride precursor into the silver precursor, electrically stirring upper layer oil phase and stirring lower layer water phase by magnetic force at the temperature of 80 DEG C, separating and washing the obtained product, and drying to obtain the cubic crystal form nano-silver material. The method is simple in operation and mild in reaction conditions, and the obtained cubic crystal form nano-silver particles are even and stable in dispersion, thus having good application prospect.
Description
Technical field
The invention belongs to the preparation field of nano silver material, particularly a kind of with oleic acid silver for the method for the preparing cubic crystal nano silver material by oil-water interface of raw material.
Background technology
Recently, researcher not only to preparing single dispersing, have good uniformity, the research of nano-Ag particles that size is controlled has keen interest, and they also improve a class the application of Nano Silver.Oil-soluble nano-Ag particles purposes is very extensive, such as, and can by the laboratory materials of oil-soluble nano-Ag particles as Ge great colleges and universities and research institute; For at nonpolar and comparatively catalysts in low pole solution; Antibacterial additives is extruded for low pole plastic master batch spiral shell; For Nano silver conductive ink, conducting resinl, plated film, stealth material etc.Meanwhile, the range of application of water-soluble nano Argent grain is also very extensive.Donghua University Materials Academy professor Zhu Meifang combines the independent research of other institutes and goes out Nano Silver antimicrobial socks, and effectively can treat beriberi, and reach industrialization, annual return reaches more than 900 ten thousand.We can connect biological micromolecule on the Nano Silver surface that surfactant is coated, carry out the fields such as the catalytic reaction in biomarker, biological monitoring, medicament transport and the aqueous solution.Following research direction will be some compound nano particle, such as Ag-TiO of synthesis
2, Ag-Fe
3o
4, Ag-ZnS, Ag-NaYF
4deng.Character exclusive for silver nano-grain is combined with the character of other nano particles, purport in play both common advantage, such as Ag-TiO
2the effect of existing double sterilization, can do again catalyst and degraded macromolecular pollutant; Ag-Fe
3o
4both there is magnetic location effect, medicament transport aspect can be applied to, sterilization etc. can have been carried out at drug effect position again simultaneously.
The method preparing nano silver material conventional at present mainly contains hydro-thermal method and microemulsion method.The particle purity of hydro-thermal method inconvenient operation, preparation is lower and easily reunite, and granularity is wayward, and grain diameter is comparatively large, and loss of product is many, and output is lower.The nano material of microemulsion method synthesis has a lot of excellent character, but the output of synthesis is relatively low, and crystallinity is poor.Oil-water interfaces method refers to that the raw material of reactant is in oil phase and aqueous phase respectively, forms the fabulous lipophilic nano particle of the less uniformity of particle diameter under lower temperature at oil-water interface; Then nano particle coated by surfactant after under three kinds of surface tension (solid, the γ profit of γ oil and γ water solid) and concentration diffusion (because the Action of Gravity Field impact of particle is very little, can ignore), pull in upper oil phase, and good dispersion also can steady in a long-termly be preserved in oil phase.Oil-water interfaces method has reaction condition gentleness, simple to operate, size tunable, and product purity is high, and productive rate is high, good crystallinity, good dispersion, and particle diameter is little, and cost is low, the advantage that efficiency is high.2008, Zhou Xingping etc. adopted oil-water interfaces method [Zhou Xingping etc., Donghua University's journal: natural science edition, 2008,35 (4): 441-444], successfully synthesize CdS quantum dot, the CdS quantum dot quantum efficiency prepared is high, 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 again oil-water interfaces method [Zhou Xingping etc., nanosecond science and technology; 2010,12:Vol7, No.6], successfully synthesize ZnS quantum dot, and some rare metals that adulterate, fluorescence property is good, is a kind of well semi-conducting material.
Adopt oleic acid silver to make presoma, compared with stearic acid silver, oleic acid silver is more readily dissolved in organic phase, and rate of dissolution is fast, reaction temperature is low, effectively can improve reaction rate.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method being the preparing cubic crystal nano silver material by oil-water interface of raw material with oleic acid silver, the method is simple to operate, reaction condition is gentle, the cubic crystal type nano Argent grain obtained is uniformly dispersed, stable, has a good application prospect.
Of the present invention a kind of with oleic acid silver for the method for the preparing cubic crystal nano silver material by oil-water interface of raw material, comprising:
(1) oleic acid silver is dissolved in cyclohexane at 80 DEG C, adds surfactant, be stirred to the oil phase that solution clear must contain oleic acid silver and cyclohexane; Dissolved at normal temperatures in deionized water by sodium borohydride, stir to obtain the aqueous phase of sodium borohydride;
(2) aqueous phase of sodium borohydride is joined containing oleic acid silver and cyclohexane oil phase in, upper oil phase electric stirring, lower floor aqueous phase magnetic agitation 2 ~ 3h at 80 DEG C, the product obtained is carried out separating, washing, finally product is drying to obtain cubic crystal type nano ag material.
Oleic acid silver cyclohexane solution concentration in described step (1) is 0.025-0.0375M.
Surfactant in described step (1) is lauryl amine, cetylamine or zinc oleate.
Surfactant in described step (1) and the proportioning of oleic acid silver are 1:1.88.
Sodium borohydride aqueous solution concentration in described step (2) is 0.075-0.1M.
In described step (2) is 1:1 containing oleic acid silver and the oil phase of cyclohexane and the aqueous phase volume ratio of sodium borohydride.
Sodium borohydride in described step (2) add containing oleic acid silver and cyclohexane oil phase in speed be 160ml/h.
Separating, washing in described step (2) is specially successively with after absolute ethyl alcohol and after deionized water rinsing, and solution layering obviously and after lower floor's aqueous phase clarification, isolate upper oil phase solution, centrifugation 15min under 11000rmp.
Drying in described step (2) is in 65 ~ 70 DEG C of drying 2 ~ 4h.
The average diameter in the cubic crystal type nano silver granuel footpath in described step (2) is 8.5-9.5nm.
beneficial effect
(1) the present invention is simple to operate, reaction condition is gentle, and experimental raw is cheap, good economy performance;
(2) the cubic crystal type nano Argent grain size obtained is about 8.5-9.5nm, is uniformly dispersed, stable, has a good application prospect.
Accompanying drawing explanation
Fig. 1 is the process chart of embodiment 1;
Fig. 2 is the transmission electron microscope picture of embodiment 1 products therefrom;
Fig. 3 is the transmission electron microscope picture of embodiment 2 products therefrom;
Fig. 4 is the transmission electron microscope picture of embodiment 3 products therefrom;
Detailed description of the invention
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
(1) 0.99g(0.00253mol is taken) oleic acid silver, be dissolved completely at 80 DEG C in 85ml cyclohexane, add 0.25g(1.345 × 10
-3mol) lauryl amine, magnetic agitation is transparent to solution, saves backup;
(2) 0.3g(0.00792mol is taken) sodium borohydride, be dissolved in 80ml deionized water at normal temperatures, magnetic agitation is even, saves backup;
(3) join in oleic acid silver cyclohexane solution prepared by step 1 in the sodium borohydride 30min prepared by step 2, upper oil phase electric stirring at 80 DEG C, the volume ratio of lower floor's aqueous phase magnetic agitation 2h(oil phase and aqueous phase is 1:1), add 100ml absolute ethyl alcohol, the Nano Silver of generation is made to be dispersed in upper oil phase, then remove lower floor's aqueous phase, then use 100ml deionized water rinsing, isolate upper oil phase solution.Take out 1ml oil phase, with the dilution of 25ml cyclohexane, ultrasonic, do TEM test.Residue oil phase centrifugation 15min under 11000rmp, with absolute ethyl alcohol cleaning deposit twice, then under 11000rmp centrifugation 15min, finally very by deposit in vacuum drying chamber, dry 2h at 65 DEG C, finally obtains the nano silver material that purity is very high.TEM figure shows, product average grain diameter is about 10.25nm, and dispersion is relatively more even, and does not almost have agglomeration.
Embodiment 2
(1) 0.99g(0.00253mol is taken) oleic acid silver, be dissolved completely at 80 DEG C in 85ml cyclohexane, add 0.5g(1.345 × 10
-3mol) cetylamine, magnetic agitation is transparent to solution, saves backup;
(2) 0.3g(0.00792mol is taken) sodium borohydride, be dissolved in 80ml deionized water at normal temperatures, magnetic agitation is even, saves backup;
(3) join in oleic acid silver cyclohexane solution prepared by step 1 in the sodium borohydride 30min prepared by step 2, upper oil phase electric stirring at 80 DEG C, the volume ratio of lower floor's aqueous phase magnetic agitation 3h(oil phase and aqueous phase is 1:1), add 100ml absolute ethyl alcohol, the Nano Silver of generation is made to be dispersed in upper oil phase, then remove lower floor's aqueous phase, then use 100ml deionized water rinsing, isolate upper oil phase solution.Take out 1ml oil phase, with the dilution of 25ml cyclohexane, ultrasonic, do TEM test.Residue oil phase centrifugation 15min under 11000rmp, with absolute ethyl alcohol cleaning deposit twice, then under 11000rmp centrifugation 15min, finally very by deposit in vacuum drying chamber, dry 4h at 70 DEG C, finally obtains the nano silver material that purity is very high.TEM figure shows, product average grain diameter is about 8.76nm, and dispersion is relatively more even, and does not almost have agglomeration.
Embodiment 3
(1) 0.99g(0.00253mol is taken) oleic acid silver, be dissolved completely at 80 DEG C in 85ml cyclohexane, add 0.5252g(1.345 × 10
-3mol) zinc oleate, magnetic agitation is transparent to solution, saves backup;
(2) 0.3g(0.00792mol is taken) sodium borohydride, be dissolved in 80ml deionized water at normal temperatures, magnetic agitation is even, saves backup;
(3) join in oleic acid silver cyclohexane solution prepared by step 1 in the sodium borohydride 30min prepared by step 2, upper oil phase electric stirring at 80 DEG C, the volume ratio of lower floor's aqueous phase magnetic agitation 3h(oil phase and aqueous phase is 1:1), add 100ml absolute ethyl alcohol, the Nano Silver of generation is made to be dispersed in upper oil phase, then remove lower floor's aqueous phase, then use 100ml deionized water rinsing, isolate upper oil phase solution.Take out 1ml oil phase, with the dilution of 25ml cyclohexane, ultrasonic, do TEM test.Residue oil phase centrifugation 15min under 11000rmp, with absolute ethyl alcohol cleaning deposit twice, then under 11000rmp centrifugation 15min, finally very by deposit in vacuum drying chamber, dry 4h at 70 DEG C, finally obtains the nano silver material that purity is very high.TEM figure shows, product average grain diameter is about 9.04nm, and dispersion is relatively more even, and does not almost have agglomeration.
Claims (10)
1., with the method that oleic acid silver is the preparing cubic crystal nano silver material by oil-water interface of raw material, comprising:
(1) oleic acid silver is dissolved in cyclohexane at 80 DEG C, adds surfactant, be stirred to the oil phase that solution clear must contain oleic acid silver and cyclohexane; Dissolved at normal temperatures in deionized water by sodium borohydride, stir to obtain the aqueous phase of sodium borohydride;
(2) aqueous phase of sodium borohydride is joined containing oleic acid silver and cyclohexane oil phase in, upper oil phase electric stirring, lower floor aqueous phase magnetic agitation 2 ~ 3h at 80 DEG C, the product obtained is carried out separating, washing, finally product is drying to obtain cubic crystal type nano ag material.
2. according to claim 1 a kind of with oleic acid silver for the method for the preparing cubic crystal nano silver material by oil-water interface of raw material, it is characterized in that: the oleic acid silver cyclohexane solution concentration in described step (1) is 0.025-0.0375M.
3. according to claim 1 a kind of with oleic acid silver for the method for the preparing cubic crystal nano silver material by oil-water interface of raw material, it is characterized in that: the surfactant in described step (1) is lauryl amine, cetylamine or zinc oleate.
4. according to claim 1 a kind of with oleic acid silver for the method for the preparing cubic crystal nano silver material by oil-water interface of raw material, it is characterized in that: the surfactant in described step (1) and the proportioning of oleic acid silver are 1:1.88.
5. according to claim 1 a kind of with oleic acid silver for the method for the preparing cubic crystal nano silver material by oil-water interface of raw material, it is characterized in that: the sodium borohydride aqueous solution concentration in described step (2) is 0.075-0.1M.
6. according to claim 1 a kind of with oleic acid silver for the method for the preparing cubic crystal nano silver material by oil-water interface of raw material, it is characterized in that: in described step (2) is 1:1 containing oleic acid silver and the oil phase of cyclohexane and the aqueous phase volume ratio of sodium borohydride.
7. according to claim 1 a kind of with oleic acid silver for the method for the preparing cubic crystal nano silver material by oil-water interface of raw material, it is characterized in that: it is 160ml/h that the sodium borohydride in described step (2) adds containing the speed in the oil phase of oleic acid silver and cyclohexane.
8. according to claim 1 a kind of with oleic acid silver for the method for the preparing cubic crystal nano silver material by oil-water interface of raw material, it is characterized in that: the separating, washing in described step (2) is specially successively with after absolute ethyl alcohol and deionized water rinsing, solution layering is obviously and after lower floor's aqueous phase clarification, isolate upper oil phase solution, centrifugation 15min under 11000rmp.
9. according to claim 1 a kind of with oleic acid silver for the method for the preparing cubic crystal nano silver material by oil-water interface of raw material, it is characterized in that: the drying in described step (2) is in 65 ~ 70 DEG C of drying 2 ~ 4h.
10. according to claim 1 a kind of with oleic acid silver for the method for the preparing cubic crystal nano silver material by oil-water interface of raw material, it is characterized in that: the average diameter in the cubic crystal type nano silver granuel footpath in described step (2) is 8.5-9.5nm.
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Effective date of registration: 20180712 Address after: 313000 A level 1, No. 29, No. 1888 Dai Shan Road, Wuxing District, Huzhou, Zhejiang. Patentee after: Huzhou Kevin Micro Technology Co., Ltd. Address before: 201620 No. 2999 North Renmin Road, Songjiang new town, Songjiang District, Shanghai. Patentee before: Donghua University |