CN100999349A - Silver/magnetic nanometer particle and its preparation method - Google Patents
Silver/magnetic nanometer particle and its preparation method Download PDFInfo
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- CN100999349A CN100999349A CN 200710034246 CN200710034246A CN100999349A CN 100999349 A CN100999349 A CN 100999349A CN 200710034246 CN200710034246 CN 200710034246 CN 200710034246 A CN200710034246 A CN 200710034246A CN 100999349 A CN100999349 A CN 100999349A
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Abstract
This invention discloses a silver / magnetic nanometer particle that has bacteriostatic effect and its preparation method. In aqueous phase of antiphase micro emulsion liquid system, silver nitrate cream uses magnetic ferroso-ferric oxide nanometer particle as inside core. Deposit simple substance silver on surface of ferroso-ferric oxide nanometer particle, prepare silver / magnetic nanometer particle having nucleocapsid structure. Silver / magnetic nanometer particle of this invention is of easy preparation method, good particle dispersibility, and uniform particle diameter. Simple substance silver of nanometer particle surface has good bacteriostatic effect. Ferroso-ferric oxide inside core of particle makes this nanometer particle have good magnetism by outside magnetic field effect. It can be convenient to reclaim and reuse from sample product that is bacteriostaticly processed.
Description
Technical field
The invention belongs to water conditioner.Be specifically related to a kind of silver/magnetic nanometer particle with fungistatic effect,
Background technology
Infect the multiple transmissible disease that is caused by microorganisms such as bacterium, viruses and threatening human beings'health always.In order to improve people's level, effectively stop the cross infection of microorganism between person to person, people and thing, thing and the thing, farthest prevent the generation of all kinds of communicable diseases, just must higher requirement be proposed to the sterile state of daily life environment.In order to create the living environment of cleaning, health, all kinds of novel anti-biotic materials and medicine are continually developed out, and the demand of antimicrobial prod also constitutes a potential great market.Silver and compound thereof just are used for daily life by the mankind as antiseptic-germicide since ancient times owing to have the excellent antibiotic performance.In recent years, along with the development of nanotechnology, the antimicrobial nano material of various silver series is also continually developed out, various silver base inorganic antibacterial agents on the market, and nano silver colloidal sol is widely used in fields such as plastics, coating, textiles, medical treatment.Its goods mainly comprise all kinds of antibacterial plastic products, ceramic, antibacterial fiber, instruments etc.
But EPDML research shows that silver and compound thereof still have certain side effect effect to human body, and silver long-term accumulated in human body may cause argyria, can make skin or eyes permanent pewter spot (argyria) occur as argyria.Many cases were once arranged clinically because take colloidal silver for a long time or drip the case that causes argyria with containing the collunarium liquid medicine of colloidal silver, therefore the relevant departments of many countries have worked out strict silver and compound safety standards thereof in the world, for example just stipulate among " Drinking Water water quality standard " (G B 5749-85) of Ministry of Health of the People's Republic of China's issue that the content of silver and compound in the Drinking Water must be less than 0.05 mg/litre.Therefore, when using silver effect antiseptic-germicide treatment soln, need as far as possible silver to be removed from solution, avoid allowing silver enter human body.Yet the antiseptic-germicide of at present seen on the market silver series especially nano silver colloidal sol when the treating water and the aqueous solution, because the particle diameter very little (usually less than 10nm) of nanometer silver thereby be difficult to remove.This has limited nano silver colloidal sol greatly and has quoted application prospect in the water treatment in life, therefore presses for the recovery problem of silver-colored Series Water Treatment Chemicals after use that solve.
Summary of the invention
The present invention aims to provide a kind of hud typed silver/magnetic nanometer particle, both solution is carried out antibacterial processing, can reclaim nano particle again.
The technical scheme that realizes the foregoing invention purpose is:
This nano particle is to be kernel with the magnetic ferroferric oxide, nano grain surface deposition simple substance silver, and particle diameter is the silver/magnetic nanometer particle of the hud typed structure of 60nm ± 20nm.
The preparation method of described silver/magnetic nanometer particle, comprise the preparation of magnetic ferroferric oxide kernel, the preparation process of silver/magnetic nanometer particle is: the ferroferric oxide magnetic nanoparticle for preparing is added in the microemulsion stirs, add a small amount of silver nitrate aqueous solution again and stir; Add the right amount of boron sodium hydride solution at last, reduction reaction continues 2 hours, adds the acetone breakdown of emulsion after reaction is finished, dehydrated alcohol and ultrapure water centrifuge washing, and obtaining kernel is Z 250, shell is the silver/magnetic nanometer particle of simple substance silver.
Be described in further detail the present invention below in conjunction with accompanying drawing:
Description of drawings
Fig. 1 is the transmission electron microscope photo figure of silver/magnetic nanometer particle.
Fig. 2 is X-ray energy spectrum (EDS) figure of silver/magnetic nanometer particle.
Fig. 3 is that the magnetic hysteresis of silver/magnetic nanometer particle returns line chart.
After from water, separating under the effect of Fig. 4 silver/magnetic nanometer particle outside magnetic field, silver-colored residual quantity in the water and the dependency of time.
Fig. 5 is the bacteriostasis rate figure after silver/magnetic nanometer particle repeatedly reuses.
The present invention utilizes the bacteriostatic action of the simple substance silver of nano grain surface to carry out antibacterial to containing bacterium solution; Utilize the magnetic of this nano particle to realize removing the silver/magnetic nanometer particle of having finished bacteriostatic action in the solution simply, fast, realize the purpose that antibacterial material can reuse.
The preparation method that the present invention has the silver/magnetic nanometer particle of fungistatic effect is: oil phase hexanaphthene, tensio-active agent triton x-100 (TritonX-100) and cosurfactant n-hexyl alcohol were mixed in 4.2: 1: 1 by volume, with suitable quantity of water as disperse phase, be stirred to solution and be the bright water-in-oil microemulsion of clarification, add the good ferroferric oxide magnetic nanoparticle of a small amount of prepared beforehand, stir; Add a small amount of silver nitrate aqueous solution again and stir; Add the right amount of boron sodium hydride solution at last and carry out reduction reaction, reaction continues 2 hours.After finishing, reaction adds the acetone breakdown of emulsion, dehydrated alcohol and ultrapure water centrifuge washing, and obtaining kernel is Z 250, shell is the silver/magnetic nanometer particle of simple substance silver.
A kind of silver/magnetic nanometer particle with fungistatic effect disclosed by the invention and preparation method thereof has following advantage:
1, the present invention adopts the reverse microemulsion legal system to be equipped with silver/magnetic nanometer particle, and method is simple, easy handling.
2, the relative homogeneous of nano particle size is better dispersed.
3, nano particle has good fungistatic effect to bacteriums such as the intestinal bacteria of tool kalamycin resistance, staphylococcus epidermidis, subtilises.
4, nano particle has magnetic, utilizes the guide effect of foreign field, nano particle can be imported the intensive position of bacterium, improves the regional area concentrations of nanoparticles, reaches the purpose of directed killing bacteria.
5, the aqueous solution is carried out nano particle after the antibacterial processing, reclaim, can utilize again by foreign field.
Embodiment
One, preparation silver/magnetic nanometer particle
1, the preparation of magnetic ferroferric oxide kernel.2.7 gram FeCl
36H
2O is dissolved in a small amount of ultrapure water, 1.0gFeCl
24H
2O is dissolved in the hydrochloric acid of 2.5 milliliter of 2 mol.Above two kinds of solution are mixed in the there-necked flask, then with the ammoniacal liquor of 125 milliliter of 6 mol under stirring condition, be added drop-wise in the there-necked flask.In the process that drips, solution begins slowly flavescence, last blackening.After dropwising, react half an hour again.Experiment is carried out under protection of nitrogen gas.After reaction finishes, pour the product that obtains into beaker, separate with magnet, after ultrapure water washing 3-5 time, be dissolved in 125 milliliters of ultrapure waters, add about 2 milliliters 25% Tetramethylammonium hydroxide again, vacuum filtration obtains pure magnetic ferroferric oxide particle at last.
2, the preparation of silver/magnetic nanometer particle.With hexanaphthene (7.5mL), tensio-active agent triton x-100 (TritonX-100,1.8mL) and cosurfactant n-hexyl alcohol (1.8mL) mix, add 50 μ L water as disperse phase, be stirred to solution and be the bright water-in-oil microemulsion of clarification, add the magnetic-particle of the above-mentioned preparation of 100 μ L, stir, the Silver Nitrate 200 μ L that add 0.2mol/L, stirred 15 minutes, and added the catalyzer sodium borohydride 150 μ L of 0.1mol/L then, reaction continues 2h.Acetone breakdown of emulsion after reaction is finished is used dehydrated alcohol and ultrapure water difference centrifuge washing 4 times, obtains hud typed silver/magnetic nanometer particle.
Two, the sign of silver/magnetic nanometer particle
The silver/magnetic nanometer particle of above-mentioned steps preparation is dissolved in ultrapure water.Taking a morsel is added drop-wise on the copper mesh, carries out the levies in kind of transmission electron microscope(TEM) and X-ray energy spectrum (EDS) scan table and tests.Shown in the transmission electron microscope(TEM) photo of Fig. 1, the silver/magnetic nanometer particle size is homogeneous relatively, and is better dispersed.Particle diameter is about 60nm ± 20nm.Shown in the EDS energy-spectrum scanning figure of Fig. 2, Ag and Fe element appear in the particle simultaneously.About about 4: 1 of the mol ratio of two kinds of elements.This conforms to theoretical.(appearance of Cu element is because the grid of copper mesh causes.)
The magnetic hysteresis tropic is carried out in the silver/magnetic nanometer particle lyophilize of part to be measured.As shown in Figure 3, silver/magnetic nanometer particle does not have the tangible magnetic hysteresis tropic to occur, and this magnetic hysteresis tropic with pure magnetic nanoparticle is consistent.This shows that this nano particle has superparamagnetism.
Three, the bacteriostatic experiment of silver/magnetic nanometer particle
Measured the minimal inhibitory concentration of silver/magnetic nanometer particle according to the minimal inhibitory concentration measuring method of routine to three kinds of bacteriums such as intestinal bacteria, staphylococcus epidermidis, subtilises.Concrete grammar is as follows: silver/magnetic nanometer particle is diluted to 12 concentration such as 120,110,100,90,80,70,60,50,40,30,20,10 μ g/mL with the LB substratum.Each concentration is respectively got 8 pipes, and every pipe adds the diluent and the cultured bacterium liquid of 250 μ L of the above-mentioned configuration of 15mL, and final inoculum size is 5 * 10
5CFU/mL (CFU is the bacterial flora sum).37 ℃ of shaking culture are after 24 hours, and the libation at an ancient wedding ceremony liquid that takes a morsel is coated on the LB agar culture plate respectively from each pipe, cultivate after 24 hours for 37 ℃ to detect by an unaided eye, and minimum concentration that can bacteria growing inhibiting is the minimal inhibitory concentration of this bacterium.As shown in table 1: silver/magnetic nanometer particle to the minimal inhibitory concentrations of this three kinds of bacteriums about 60 μ g/mL.
Table 1 silver/magnetic nanometer particle is to the minimal inhibitory concentration of three kinds of different bacterium
| Bacterial species | Silver/magnetic nanometer particle (μ g/mL) |
| Intestinal bacteria | 60 |
| Staphylococcus epidermidis | 60 |
| Subtilis | 60 |
Four, silver/magnetic nanometer particle isolating test from water
Utilize the magnetic of silver/magnetic nanometer particle, the test tube that the silver/magnetic nanometer particle aqueous solution is housed is placed in the magnetic field, utilize magnetic attraction that silver/magnetic nanometer particle is adsorbed on the test tube wall to reach the purpose except that residual silver in anhydrating.As shown in Figure 4, along with the increase of storage period in magnetic field of the silver/magnetic nanometer particle aqueous solution, the amount of residual silver constantly descends in the water.Residual silver amount drops to 0.045 μ g/mL in the water after 30 minutes.This value has reached drinking water standard.In the control experiment of being done with silver sol, through after the same treatment, residual silver content is 60 μ g/mL in the water.
Five, the bacteriostatic test that utilizes again after silver/magnetic nanometer particle reclaims
Silver/magnetic nanometer particle can reclaim by magnetic field after the bacterium in the aqueous solution is handled, and the silver/magnetic nanometer particle of recovery can be used further to antibacterial after supersound washing disperses again.As shown in Figure 5, utilize after reclaiming through several times, silver/magnetic nanometer particle also has certain fungistatic effect again.Compare with initial silver/magnetic nanometer particle, the total antibacterial efficient of silver/magnetic nanometer particle after reclaiming through 5 times can also reach initial 50%.
Claims (2)
1, a kind of silver/magnetic nanometer particle is characterized in that: this nano particle is to be kernel with the magnetic ferroferric oxide, nano grain surface deposition simple substance silver, and particle diameter is the silver/magnetic nanometer particle of the hud typed structure of 60nm ± 20nm.
2, a kind of preparation method of silver/magnetic nanometer particle as claimed in claim 1, comprise the preparation of magnetic ferroferric oxide kernel, the preparation method who it is characterized in that silver/magnetic nanometer particle is: the ferroferric oxide magnetic nanoparticle for preparing is added in the microemulsion stirs, add a small amount of silver nitrate aqueous solution again and stir; Add the right amount of boron sodium hydride solution at last, reduction reaction continues 2 hours, adds the acetone breakdown of emulsion after reaction is finished, dehydrated alcohol and ultrapure water centrifuge washing, and obtaining kernel is Z 250, shell is the silver/magnetic nanometer particle of simple substance silver.
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| CN102513066A (en) * | 2012-01-11 | 2012-06-27 | 中国科学院长春应用化学研究所 | Biological adsorbent, preparation method and application thereof |
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| CN102697806A (en) * | 2012-05-17 | 2012-10-03 | 中国科学院长春应用化学研究所 | Biological antibacterial agent, as well as preparation method and application thereof |
| CN101721749B (en) * | 2009-12-04 | 2013-01-23 | 北京化工大学 | Ferroferric oxide/calcium phosphate nuclear shell structure nano particle and preparation method thereof |
| CN103109864A (en) * | 2013-01-30 | 2013-05-22 | 黑龙江大学 | Preparation method of recyclable silver-embedded magnetic compound bacteriostat |
| 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 |
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| CN110934135A (en) * | 2018-09-25 | 2020-03-31 | 中国科学院金属研究所 | Magnetic nano-silver antibacterial composite material with controllable release of silver ions and preparation method and application thereof |
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| CN1183999C (en) * | 2000-09-13 | 2005-01-12 | 王建毅 | Nm-class core-and-shell particles |
| CN1245625C (en) * | 2003-04-30 | 2006-03-15 | 陕西西大北美基因股份有限公司 | Nuclear/shell type superparamagnetism composite particulate, preparation method and application thereof |
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| 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 |
| CN102513066B (en) * | 2012-01-11 | 2013-09-18 | 中国科学院长春应用化学研究所 | Biological adsorbent, preparation method and application thereof |
| CN102513066A (en) * | 2012-01-11 | 2012-06-27 | 中国科学院长春应用化学研究所 | Biological adsorbent, preparation method and application thereof |
| CN102586463A (en) * | 2012-03-20 | 2012-07-18 | 湖南大学 | Biosensing method for DNA (Deoxyribose Nucleic Acid) demethylase based on nanoparticle aggregation |
| CN102697806A (en) * | 2012-05-17 | 2012-10-03 | 中国科学院长春应用化学研究所 | Biological antibacterial agent, as well as preparation method and application thereof |
| CN102697806B (en) * | 2012-05-17 | 2014-06-18 | 中国科学院长春应用化学研究所 | Biological antibacterial agent, as well as preparation method and application thereof |
| CN103109864A (en) * | 2013-01-30 | 2013-05-22 | 黑龙江大学 | Preparation method of recyclable silver-embedded magnetic compound bacteriostat |
| CN105797749A (en) * | 2016-04-06 | 2016-07-27 | 金华科海检测有限公司 | Preparation and application of magnetic nano-photocatalyst adopting multi-layer core-shell structure |
| CN110934135A (en) * | 2018-09-25 | 2020-03-31 | 中国科学院金属研究所 | Magnetic nano-silver antibacterial composite material with controllable release of silver ions and preparation method and application thereof |
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