CN103121100B - A kind of method of nano-Ag particles to aqueous phase shifting Coated with Oleic Acid - Google Patents
A kind of method of nano-Ag particles to aqueous phase shifting Coated with Oleic Acid Download PDFInfo
- Publication number
- CN103121100B CN103121100B CN201310048701.8A CN201310048701A CN103121100B CN 103121100 B CN103121100 B CN 103121100B CN 201310048701 A CN201310048701 A CN 201310048701A CN 103121100 B CN103121100 B CN 103121100B
- Authority
- CN
- China
- Prior art keywords
- nano
- aqueous phase
- particles
- oleic acid
- coated
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The present invention relates to a kind of method of nano-Ag particles to aqueous phase shifting Coated with Oleic Acid, comprising: the nano-Ag particles that (1) gets Coated with Oleic Acid adds in solvent, dissolve, ultrasonic disperse, obtains Nano silver solution; (2) by softex kw CTAB and water mixing, stir, heating water bath to 40 DEG C, obtains CTAB solution, then adjust ph; (3) added by Nano silver solution in above-mentioned solution, under 40 DEG C of conditions, stir 0.5-2h, cooling, stratification, aqueous phase carries out centrifugation, and dry, obtain water-soluble nanoparticles, wherein the volume ratio of Nano silver solution and CTAB solution is 1:10.The present invention have simple to operate, the reaction time is short, reaction temperature is low, reproducible, cost is low, efficiency advantages of higher; Nano Silver prepared by the present invention good dispersion in aqueous, stable in properties, its hydrophily performance can be applicable to the fields such as antibacterial and aqueous phase catalyst.
Description
Technical field
The invention belongs to the phase transfer field of nano particle, particularly a kind of method of nano-Ag particles to aqueous phase shifting Coated with Oleic Acid.
Background technology
Nano Silver, as a kind of emerging functional material, because it has very high specific area and surface-active, has extensive use in catalysis, antistatic, low temperature superconducting material and biology sensor material etc.Silver ion is one of bactericidal the strongest active metal ion, and Nano Silver, by the slowly-releasing process of surface atom to Ag+, becomes the most potential anti-biotic material, has excellent antibacterial characteristics.In addition, Nano Silver also has deodorizing and the ultraviolet function of absorption portion, thus also can be applicable to pharmaceuticals industry and cosmetic industry etc.
At present, the method preparing nano material mainly contains microemulsion method, template, electrochemical process, sol-gal process, hydro-thermal method etc., aqueous phase is prepared Nano Silver and is often required that preparation condition is higher, the reaction time is longer, reaction temperature is higher, generates nano particle and there is the shortcomings such as size is comparatively large, particle heterogeneity, dispersiveness are poor.Oil-water interfaces method synthesizing nano-particle is simple to operate, nanoparticle size is little, reaction temperature is low, cost is low can produce in a large number, the dispersed nano-silver particles of the Coated with Oleic Acid of synthesis is good, productive rate is high, good crystallinity, products therefrom is carried out phase transfer, increase its hydrophily, its application in aqueous phase can be expanded.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method of nano-Ag particles to aqueous phase shifting Coated with Oleic Acid, and the method is simple to operate, the reaction time is short, reaction temperature is low, reproducible, cost is low, efficiency advantages of higher; Nano Silver good dispersion stable in properties in aqueous prepared by this invention, its hydrophily performance can be applicable to the fields such as antibacterial and aqueous phase catalyst.
A kind of method of nano-Ag particles to aqueous phase shifting Coated with Oleic Acid of the present invention, comprising:
(1) nano-Ag particles getting Coated with Oleic Acid adds in solvent, and dissolve, ultrasonic disperse, obtains Nano silver solution;
(2) by softex kw CTAB and water mixing, stir, heating water bath, to 40-60 DEG C, obtains CTAB solution, then adjust ph;
(3) added by Nano silver solution in above-mentioned solution, under 40-60 DEG C of condition, stir 0.5-2h, leave standstill after cooling, layering, aqueous phase carries out centrifugation, and dry, obtain water-soluble nanoparticles, wherein the volume ratio of Nano silver solution and CTAB solution is 1:10.
In described step (1), the nano-Ag particles of oleic acid parcel is prepared from by oil-water interfaces method, enuatrol and silver nitrate is adopted to synthesize oleic acid silver, with cyclohexane, oleic acid silver, oleic acid for oil phase, the aqueous solution of sodium borohydride is aqueous phase, and mixing water-oil phase, reacts 2h under 80 DEG C of conditions, after it cools naturally, separated product can obtain cubic crystal type nano Argent grain, granular size average diameter is at about 8.6nm, and granular size is homogeneous, favorable dispersibility.
In described step (1), solvent is cyclohexane.
In described step (1), the ultrasonic disperse time is 10-20min.
In described step (1), the concentration of the Nano Silver of gained is 0.02g/ml.
In described step (2), the concentration of gained CTAB solution is 0.05-0.1mol/ml.
Described step (2) is middle is 8-10.5 by 0.5mol/L ammoniacal liquor adjust ph.
In described step (3), centrifugation is that negate should add acetone by aqueous phase afterwards, and the centrifugal 15-20min of 10000rpm, then uses deionized water 10000rpm eccentric cleaning 15-20min.
In described step (3), baking temperature is 50-60 DEG C, and drying time is 3-4h.
The nano-Ag particles average diameter of described step (3) gained is 10.0nm, better dispersed, does not have obvious agglomeration to occur.
beneficial effect
(1) the present invention have simple to operate, the reaction time is short, reaction temperature is low, reproducible, cost is low, efficiency advantages of higher;
(2) the Nano Silver good dispersion stable in properties in aqueous prepared of the present invention, its hydrophily performance can be applicable to the fields such as antibacterial and aqueous phase catalyst.
Accompanying drawing explanation
Fig. 1 is process chart of the present invention;
Fig. 2 is comparison diagram before and after embodiment 1 phase transfer;
Fig. 3 is embodiment 1, and before 2 transfers, the nano silver particles TEM of Coated with Oleic Acid schemes and domain size distribution;
Fig. 4 is that embodiment 1 gained nano silver particles TEM schemes and domain size distribution;
Fig. 5 is that the UV-Vis of water-oil phase after embodiment 2 phase transfer absorbs spectrogram;
Fig. 6 is that the UV-Vis of embodiment 1,3 gained aqueous phase Nano Silver absorbs spectrogram.
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, get the Nano Silver of Coated with Oleic Acid by oil-water interfaces legal system, after drying, get 0.2g and add the dissolving of 10mL cyclohexane, excusing from death dispersion 15min, makes the cyclohexane solution of 0.02g/mL Nano Silver.
2, get CTAB3.654g in beaker, add 100mL deionized water, magnetic agitation, heating water bath to 40 DEG C, CTAB dissolves, and making concentration is 0.1mol/L CTAB solution, regulates its pH value to 10.5 with 0.5mol/L ammoniacal liquor.
3, by the cyclohexane solution of Nano Silver in step 1, add in step 2, maintain reaction temperature 40 DEG C of lower magnetic forces and stir 1h.Reaction treats that it naturally cools to room temperature after stopping, and solution is divided into two-phase, and upper strata is water white cyclohexane, and lower floor is the Nano Silver after transfer.Directly get 5mL aqueous phase and carry out UV-vis and TEM test.Gained water-phase product adds acetone, 10000rpm centrifugation 15min, and with deionized water 10000rpm eccentric cleaning 15min.Water-soluble nanoparticles is obtained after products therefrom being placed in 60 DEG C of dry 4h of baking oven.The water-soluble nano silver that the method obtains has stability, and can be good at being scattered in deionized water, TEM figure shows that the average grain diameter of product is at about 10.0nm, and particle dispersion is good, size uniformity, close to single dispersing, does not have obvious agglomeration.
Embodiment 2
1, get the Nano Silver of Coated with Oleic Acid by oil-water interfaces legal system, after drying, get 0.2g and add the dissolving of 10mL cyclohexane, excusing from death dispersion 15min, makes the cyclohexane solution of 0.02g/mL Nano Silver.
2, get CTAB1.827g in beaker, add 100mL deionized water, magnetic agitation, heating water bath to 40 DEG C, CTAB dissolves, and making concentration is 0.05mol/L CTAB solution, regulates its pH value to 10.5 with 0.5mol/L ammoniacal liquor.
3, by the cyclohexane solution of Nano Silver in step 1, add in step 2, maintain reaction temperature 40 DEG C of lower magnetic forces and stir 1h.Reaction treats that it naturally cools to room temperature after stopping, and solution is divided into two-phase, and upper strata is water white cyclohexane, and lower floor is faint yellow, is hydrophobic nano silver and is successfully transferred in aqueous phase.Get 5mL aqueous phase and oil phase carries out UV-vis test respectively, relatively after reaction, the ultraviolet-ray visible absorbing peak of water-oil phase is known, after reaction, aqueous phase has obvious absorption peaks at 417nm place, and oil phase absworption peak is more weak, proves that hydrophobic nano silver is successfully transferred in aqueous phase by CTAB.
Embodiment 3
1, get the Nano Silver of Coated with Oleic Acid by oil-water interfaces legal system, after drying, get 0.2g and add the dissolving of 10mL cyclohexane, excusing from death dispersion 15min, makes the cyclohexane solution of 0.02g/mL Nano Silver.
2, get CTAB3.654g in beaker, add 100mL deionized water, magnetic agitation, heating water bath to 40 DEG C, CTAB dissolves, and making concentration is 0.1mol/L CTAB solution, regulates its pH value to 8.0 with 0.5mol/L ammoniacal liquor.
3, by the cyclohexane solution of Nano Silver in step 1, add in step 2, maintain reaction temperature 40 DEG C of lower magnetic forces and stir 1h.Reaction treats that it naturally cools to room temperature after stopping, and solution is divided into two-phase, and upper strata is water white cyclohexane, and lower floor is the Nano Silver after transfer.Directly get 5mL aqueous phase and carry out UV-Vis and TEM test.Gained water-phase product adds acetone, 10000rpm centrifugation 15min, and with deionized water 10000rpm eccentric cleaning 15min.Water-soluble nanoparticles is obtained after products therefrom being placed in 60 DEG C of dry 4h of baking oven.The water-soluble nano silver that the method obtains has stability, can be good at being scattered in deionized water.UV-Vis analyzes display, and pH value is that under 10.5 conditions, phase transfer efficiency is higher.
Claims (8)
1. shift the method for nano-Ag particles to aqueous phase for Coated with Oleic Acid, comprising:
(1) nano-Ag particles getting Coated with Oleic Acid adds in solvent, and dissolve, ultrasonic disperse, obtains Nano silver solution;
(2) by softex kw CTAB and water mixing, stir, be heated to 40-60 DEG C, obtain CTAB solution, then adjust ph; Be wherein 8-10.5 by 0.5mol/L ammoniacal liquor adjust ph;
(3) Nano silver solution is added in above-mentioned CTAB solution, under 40-60 DEG C of condition, stir 0.5-2h, cooling, stratification, aqueous phase carries out centrifugation, drying, obtains water-soluble nanoparticles, and wherein the volume ratio of Nano silver solution and CTAB solution is 1:10.
2. a kind of method of nano-Ag particles to aqueous phase shifting Coated with Oleic Acid according to claim 1, is characterized in that: in described step (1), solvent is cyclohexane.
3. a kind of method of nano-Ag particles to aqueous phase shifting Coated with Oleic Acid according to claim 1, is characterized in that: in described step (1), the ultrasonic disperse time is 10-20min.
4. a kind of method of nano-Ag particles to aqueous phase shifting Coated with Oleic Acid according to claim 1, is characterized in that: in described step (1), the concentration of the Nano Silver of gained is 0.02g/ml.
5. a kind of method of nano-Ag particles to aqueous phase shifting Coated with Oleic Acid according to claim 1, is characterized in that: in described step (2), the concentration of gained CTAB solution is 0.05-0.1mol/ml.
6. a kind of method of nano-Ag particles to aqueous phase shifting Coated with Oleic Acid according to claim 1, it is characterized in that: in described step (3), centrifugation is that negate should add acetone by aqueous phase afterwards, the centrifugal 15min of 10000rpm, then uses deionized water 10000rpm eccentric cleaning 15min.
7. a kind of method of nano-Ag particles to aqueous phase shifting Coated with Oleic Acid according to claim 1, is characterized in that: in described step (3), baking temperature is 50-60 DEG C, and drying time is 3-4h.
8. a kind of method of nano-Ag particles to aqueous phase shifting Coated with Oleic Acid according to claim 1, is characterized in that: the nano-Ag particles average diameter of described step (3) gained is 10.0nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310048701.8A CN103121100B (en) | 2013-02-07 | 2013-02-07 | A kind of method of nano-Ag particles to aqueous phase shifting Coated with Oleic Acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310048701.8A CN103121100B (en) | 2013-02-07 | 2013-02-07 | A kind of method of nano-Ag particles to aqueous phase shifting Coated with Oleic Acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103121100A CN103121100A (en) | 2013-05-29 |
| CN103121100B true CN103121100B (en) | 2015-10-28 |
Family
ID=48452347
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310048701.8A Expired - Fee Related CN103121100B (en) | 2013-02-07 | 2013-02-07 | A kind of method of nano-Ag particles to aqueous phase shifting Coated with Oleic Acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103121100B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116374973A (en) * | 2023-02-08 | 2023-07-04 | 浙江大学 | Method for preparing hydroxyapatite with uniformly dispersed aqueous phase by double-layer oleic acid method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101279231A (en) * | 2007-04-06 | 2008-10-08 | 清华大学 | Method for assembling three-dimensional aqueous dispersion colloid ball from nanocrystalline |
| CN102101173A (en) * | 2009-12-22 | 2011-06-22 | 上海亿金纳米科技有限公司 | Method for preparing novel large-scale oil-soluble nano silver |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2914200B1 (en) * | 2007-03-30 | 2009-11-27 | Inst Francais Du Petrole | PROCESS FOR THE SYNTHESIS OF CUBIC METAL NANOPARTICLES IN THE PRESENCE OF TWO REDUCERS |
-
2013
- 2013-02-07 CN CN201310048701.8A patent/CN103121100B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101279231A (en) * | 2007-04-06 | 2008-10-08 | 清华大学 | Method for assembling three-dimensional aqueous dispersion colloid ball from nanocrystalline |
| CN102101173A (en) * | 2009-12-22 | 2011-06-22 | 上海亿金纳米科技有限公司 | Method for preparing novel large-scale oil-soluble nano silver |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103121100A (en) | 2013-05-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105084372B (en) | The method of the nano particle of carried metal or metal oxide in mesoporous silicon oxide duct | |
| CN101451270B (en) | Method for large scale preparation of noble metal nano wire | |
| CN101792171B (en) | Preparation method of cerium oxide nanoballs | |
| CN101693297B (en) | Preparation method of copper nanoparticles with different particle diameters | |
| CN101302032B (en) | Preparation of cupric oxide nano-material | |
| CN104174864B (en) | The preparation method of a kind of nanometer or submicron order Argent grain powder | |
| CN103273083A (en) | Method for preparing gold nanoparticles | |
| CN103496724B (en) | The preparation method of a kind of nano alumina sol and gel | |
| CN107413354B (en) | Preparation method of silver-loaded copper oxide nanocomposite | |
| CN108817414B (en) | Preparation method of gold nanoflower in ionic liquid aqueous solution | |
| CN102633307A (en) | Method for hydrothermally preparing mono-dispersed hollow magnetic nanometer particles | |
| CN101497135A (en) | Method for preparing spherical silver nano granule | |
| CN103406546A (en) | Method for preparing flower-like gold nanoparticles controllably | |
| CN103387257B (en) | Method for preparing nano cerium dioxide material by utilizing tween-80 as surfactant | |
| CN106141171A (en) | Hud typed superstructure nano material, its preparation method and application | |
| CN104439276A (en) | Method for fast preparing hollow porous silicon dioxide/silver nanoparticle composite and product | |
| Kamarudin et al. | Synthesis of silver nanoparticles stabilised by pvp for polymeric membrane application: a comparative study | |
| He et al. | Hydrothermal synthesis of boehmite nanorods from alumina sols | |
| CN102010707B (en) | Method for preparing magneto-chromism ferroferric oxide sol | |
| CN103121100B (en) | A kind of method of nano-Ag particles to aqueous phase shifting Coated with Oleic Acid | |
| Li et al. | One-pot synthesis of uniform hollow cuprous oxide spheres fabricated by single-crystalline particles via a simple solvothermal route | |
| CN103586480B (en) | One step microwave preparation of bimetallic/carbon-coating shape composite balls | |
| Wojnicki et al. | The influence of dielectric permittivity of water on the shape of PtNPs synthesized in high-pressure high-temperature microwave reactor | |
| CN102451688B (en) | Hollow nanocomposite oxide material and preparation thereof | |
| CN101838460A (en) | Core-shell structure polyaniline / silver conductive nano composite material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20151028 Termination date: 20180207 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |