CN104550995B - A kind of synthetic method of gold silver composite Nano chain antibacterial - Google Patents
A kind of synthetic method of gold silver composite Nano chain antibacterial Download PDFInfo
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- CN104550995B CN104550995B CN201310504812.5A CN201310504812A CN104550995B CN 104550995 B CN104550995 B CN 104550995B CN 201310504812 A CN201310504812 A CN 201310504812A CN 104550995 B CN104550995 B CN 104550995B
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Abstract
The present invention relates to the synthetic method of a kind of gold silver composite Nano chain antibacterial, the method comprises the following steps: (1) takes template and joins AgNO3In solution, the pH value of regulation system is 10, under agitation, instills reducing agent, after at room temperature reaction solution is aged 1-5h, it is thus achieved that Ag gold nanochains in reaction solution；(2) above-mentioned Ag nano chain being added in reactor, with dispersant in deionized water, two fill HAuCl respectively4The test tube of the band semipermeable membrane sealing of solution and hydrazine hydrate solution, being inverted in the reactor filling Ag nano chain, whole system is placed in supersound process 5-10 minute in ultrasonic disperser, gained solution centrifugation, for several times, natural drying i.e. obtains Au/Ag composite Nano chain in washing.Compared with prior art, it is cheap that the present invention has preparation cost, and technique is simple, and without any pollution, product has the advantages such as the structure of good dispersibility and rule.
Description
Technical field
The invention belongs to environmental science, be specifically related to the synthetic method of a kind of gold silver composite Nano chain antibacterial.
Background technology
Nanometer silver is a kind of emerging functional material, has the highest specific surface area and surface activity, is widely used as catalyst material, antistatic material, low temperature superconducting material, electric slurry and biosensor material etc..It addition, nanometer silver also has antibacterial, deodorization and absorbs the functions such as some ultra violet rays, thus can be applicable to pharmaceuticals industry and cosmetic industry.In chemical fibre, add a small amount of nanometer silver, thus it is possible to vary some performance of chemical fabrics, and give the strongest sterilizing ability.The metallic element used in existing inorganic fungicide is mainly to the safer silver of human body, copper, zinc etc., and wherein the sterilizing ability of silver is the strongest, so, it is most important one main kind of in inorganic sterilization material, gets more and more people's extensive concerning.The sterilization mechanism of silver-series antibacterial agent is commonly considered as owing to silver compound or silver metal particle are after touching microorganism, it may occur that following several respects effect: the breathing of suppression microorganism, the synthesis of obstruction enzyme, destruction protein, damaging cells film, the combination of interference DNA.Nano silver particles has the bactericidal activity more excellent than common silver compound or silver metal particle, has been largely used to the fields such as all kinds of washing, health product.
And after Precious Metals-Gold and nanometer silver are combined, the most excellent physicochemical property can be brought, therefore, receive the extensive attention of researcher.nullCurrent reported nanometer gold silver composite Nano antibacterial preparation method has cold-maceration (T.Som，B.Karmakar.CoreShellAuAgNanoparticlesinDielectricNanocom positeswithPlasmon-EnhancedFluorescence:ANewParadigmuinA ntimonyGlasses [J] .NanoRes.，2009，2:607-616)、Organic hot solvent method (C.Wang，S.Peng，R.Chan，S.H.Sun，SynthesisofAuAgAlloyNanoparticlesfromCore/ShellStructuredAg/Au[J].small.，2009，5:567-570)、Bioanalysis (A.Rai，M.Chaudhary，A.Ahmad，S.Bhargava，M.Sastry.SynthesisoftriangularAucore-Agshellnanoparticles[J].MaterialsResearchBulletin，2007.42:1212-1220)、Sol-gel process (Y.Okuno，K.Nishioka，A.Kiya，N.Nakashima，A.Ishibashi.Y.Niidome.UniformandcontrollablepreparationofAu-Agcore-shellnanorodsusinganisotropicsilvershellformationongoldnanorods[J]，Nanoscale，2010，2:1489-1493)、Two-step synthesis method .YOkuno，K.Nishioka，A.Kiya，N.Nakashima，A.Ishibashi，Y.Niidome.UniformandcontrollablepreparationofAu-Agcore-shellnanorodsusinganisotropicsilvershellformationongoldnanorods[J]，Nanoscale，2010，2:1489-1493)、Sonochemistry method (Salkar，R.A.；Jeevanandam, P.；Aruna, S.T.；Koltypin, Y.Gedanken, A.TheSonochemicalPreparationofAmorphousSilverNanoparticl es [J] .J.Mater:Chem.1999,9:1333-1335) etc. method.In above-mentioned synthesis, it is thus achieved that product be mostly nanoparticle or nano bar-shape composite construction, not yet have the report of gold silver nano combined chain material.According to pertinent literature, it is concluded that chain structure nano composite material is when environmental area is applied, due to the advantage in its structure, there is features such as being more easily recycled, bactericidal effect is more preferably excellent.Accordingly, with respect to the preparation of gold silver nano combined chain antibacterial, there is important researching value.
Summary of the invention
Defect that the purpose of the present invention is contemplated to overcome above-mentioned prior art to exist and the synthetic method of the gold silver composite Nano chain antibacterial that a kind of bactericidal effect is good is provided.
The purpose of the present invention can be achieved through the following technical solutions: the synthetic method of a kind of gold silver composite Nano chain antibacterial, it is characterised in that the method comprises the following steps:
(1) take template and join AgNO3In solution, the pH value of regulation system is 10, under agitation, instills reducing agent to no longer producing precipitation, after at room temperature reaction solution is aged 1-5h, it is thus achieved that Ag gold nanochains in reaction solution；
(2) above-mentioned Ag nano chain being added in reactor, with dispersant in deionized water, two fill HAuCl respectively4The test tube of the band semipermeable membrane sealing of solution and hydrazine hydrate solution, it is inverted in the reactor filling Ag nano chain, whole system is placed in supersound process 5-10 minute in ultrasonic disperser, obtain the solution of dark red in the reactor, by this solution centrifugation, and with deionized water and absolute ethanol washing for several times, natural drying i.e. obtains Au/Ag composite Nano chain.
Template described in step (1) includes polyacrylamide, poly-methylcellulose, sodium polyacrylate, polyacrylamide, the addition of template and AgNO3Mass ratio be 1:1.7.
The pH value of the regulation system described in step (1) use ammonia,
Reducing agent described in step (1) includes vitamin c solution.
Dispersant described in step (2) be volume ratio be TGA and the mixture of dehydrated alcohol of 1:20, the addition of dispersant is 50～60ml/molAg.
The semipermeable membrane that the test tube of the band semipermeable membrane sealing described in step (2) uses includes collodion membrane, egg film or Air Bladder pseudosciaenae seu Acipenser.
HAuCl described in step (2)4It is 5～8:20 with the mol ratio of Ag, the consumption excess of hydrazine hydrate.
Compared with prior art, advantage of the present invention is as follows:
(1) the gold silver nano combined chain antibacterial structure that the present invention prepares neatly is unified, and has more more preferable antibacterial effect than gold silver nano-complex particle.
(2) propose to control with semipermeable membrane the transmitting procedure of reactive ion, thus control the nucleation of product, crystalline rate and the thickness of silver particles surface gold, and by the way of ultrasonic disperse, promote the dispersion of ion.
(3) use vitamin C or glucose as reducing agent, produce without waste water, waste gas and waste liquid, belong to green syt category.
(4) method technique is simple, it is not necessary to complex device, and the most whole production process, without any pollution, meets sustainable development requirement.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1:
0.02g polyacrylamide is joined 20mL0.01mol/LAgNO3In solution, being 10 with the pH of ammonia regulation system, instill vitamin c solution as reducing agent to no longer producing precipitation in mechanical agitation downhill reaction solution, solution is at room temperature aged 1 hour, and high speed centrifugation separates, washing, it is thus achieved that elemental silver gold nanochains.
Joining in beaker by the silver nanochains of preparation together with 0.05mL TGA and 10mL dehydrated alcohol, supersound process is after 5 minutes, and high speed centrifugation separates, it is thus achieved that the silver nanochains that surface TGA processed.Surface-treated Ag gold nanochains is joined in beaker, adds the dispersion of 20mL deionized water.7mL0.01mol/LHAuCl will be separately added into4Solution and 5mL hydrazine hydrate (N2H4·H2O, 30wt%) two test tubes seal with collodion membrane after, be inverted in the beaker being to fill silver nanochains.Ultrasonic 10 minutes of whole system, finally obtains the solution of dark red in beaker.High speed centrifugation separates, and with deionized water and absolute ethanol washing each 3 times, natural drying, it is thus achieved that the golden composite Nano chain antibacterial of silver, its length is about 2 microns, and the diameter of Au/Ag composite nanoparticle is about 35 nanometers.
Embodiment 2:
Poly-for 0.02g methylcellulose is joined 20mL0.01mol/LAgNO3In solution, being 10 with the pH of ammonia regulation system, instill vitamin c solution as reducing agent to no longer producing precipitation in mechanical agitation downhill reaction solution, solution is at room temperature aged 1 hour, and high speed centrifugation separates, washing, it is thus achieved that elemental silver nano chain.
Joining in beaker by the silver nanochains of preparation together with 0.5mL TGA and 10mL dehydrated alcohol, supersound process is after 5 minutes, and high speed centrifugation separates, it is thus achieved that the silver nanochains that surface TGA processed.Surface-treated Ag nano chain is joined in beaker, adds the dispersion of 20mL deionized water.8mL0.01mol/LHAuCl will be separately added into4Solution and 6mL hydrazine hydrate (N2H4·H2O, 30wt%) two test tubes seal with egg film after, be inverted in the beaker being to fill silver nanochains.Ultrasonic 10 minutes of whole system, finally obtains the solution of dark red in beaker.High speed centrifugation separates, and with deionized water and absolute ethanol washing each 3 times, natural drying, it is thus achieved that gold silver composite Nano chain antibacterial, its length is about 3 microns, and the diameter of particle is about 40 nanometers.
Embodiment 3:
0.02g sodium polyacrylate is joined 20mL0.01mol/LAgNO3In solution, being 10 with the pH of ammonia regulation system, instill vitamin c solution as reducing agent to no longer producing precipitation in mechanical agitation downhill reaction solution, solution is at room temperature aged 1 hour, and high speed centrifugation separates, washing, it is thus achieved that elemental silver nano chain.
Joining in beaker by the silver nanochains of preparation together with 0.5mL TGA and 10mL dehydrated alcohol, supersound process is after 5 minutes, and high speed centrifugation separates, it is thus achieved that the silver nanochains that surface TGA processed.Surface-treated Ag nano chain is joined in beaker, adds the dispersion of 20mL deionized water.6mL0.01mol/LHAuCl will be separately added into4Solution and 5mL hydrazine hydrate (N2H4·H2O, 30wt%) two test tubes seal with Air Bladder pseudosciaenae seu Acipenser after, be inverted in the beaker being to fill silver nanochains.Ultrasonic 10 minutes of whole system, finally obtains the solution of dark red in beaker.High speed centrifugation separates, and with deionized water and absolute ethanol washing each 3 times, natural drying, it is thus achieved that gold silver composite Nano chain antibacterial, its length is about 2.5 microns, and the diameter of particle is about 33 nanometers.
Embodiment 4
0.02g polyacrylamide is joined 20mL0.01mol/LAgNO3In solution, being 10 with the pH of ammonia regulation system, instill vitamin c solution as reducing agent to no longer producing precipitation in mechanical agitation downhill reaction solution, solution is at room temperature aged 5 hours, and high speed centrifugation separates, washing, it is thus achieved that elemental silver nano chain.
Joining in beaker by the silver nanochains of preparation together with 0.5mL TGA and 10mL dehydrated alcohol, supersound process is after 5 minutes, and high speed centrifugation separates, it is thus achieved that the silver nanochains that surface TGA processed.Surface-treated Ag nano chain is joined in beaker, adds the dispersion of 20mL deionized water.5mL0.01mol/LHAuCl will be separately added into4Solution and 5mL hydrazine hydrate (N2H4·H2O, 30wt%) two test tubes seal with egg film after, be inverted in the beaker being to fill silver nanochains.Ultrasonic 10 minutes of whole system, finally obtains the solution of dark red in beaker.High speed centrifugation separates, and with deionized water and absolute ethanol washing each 3 times, natural drying, it is thus achieved that gold silver composite Nano chain antibacterial, its length is about 3.5 microns, and the diameter of particle is about 28 nanometers.
Claims (7)
1. the synthetic method of a gold silver composite Nano chain antibacterial, it is characterised in that the method comprises the following steps:
(1) take template and join AgNO3In solution, the pH value of regulation system is 10, under agitation, instills reducing agent, after at room temperature reaction solution is aged 1-5h, it is thus achieved that Ag gold nanochains in reaction solution；
(2) above-mentioned Ag nano chain being added in reactor, with dispersant in deionized water, two fill HAuCl respectively4The test tube of the band semipermeable membrane sealing of solution and hydrazine hydrate solution, it is inverted in the reactor filling Ag nano chain, whole system is placed in supersound process 5-10 minute in ultrasonic disperser, obtain the solution of dark red in the reactor, by this solution centrifugation, and with deionized water and absolute ethanol washing for several times, natural drying i.e. obtains Au/Ag composite Nano chain.
The synthetic method of a kind of gold silver composite Nano chain antibacterial the most according to claim 1, it is characterized in that, template described in step (1) includes polyacrylamide, poly-methylcellulose, sodium polyacrylate, polyacrylamide, the addition of template and AgNO3Mass ratio be 1:1.7.
The synthetic method of a kind of gold silver composite Nano chain antibacterial the most according to claim 1, it is characterised in that step (1) uses the pH value of ammonia regulation system.
The synthetic method of a kind of gold silver composite Nano chain antibacterial the most according to claim 1, it is characterised in that the reducing agent described in step (1) includes vitamin c solution.
The synthetic method of a kind of gold silver composite Nano chain antibacterial the most according to claim 1, it is characterized in that, dispersant described in step (2) be volume ratio be TGA and the mixture of dehydrated alcohol of 1:20, the addition of dispersant is 50～60ml/molAg.
The synthetic method of a kind of gold silver composite Nano chain antibacterial the most according to claim 1, it is characterised in that the semipermeable membrane that the test tube of the band semipermeable membrane sealing described in step (2) uses includes collodion membrane, egg film or Air Bladder pseudosciaenae seu Acipenser.
The synthetic method of a kind of gold silver composite Nano chain antibacterial the most according to claim 1, it is characterised in that the HAuCl described in step (2)4It is 5～8:20 with the mol ratio of Ag.
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| CN111590085B (en) * | 2020-06-01 | 2022-11-22 | 中国农业科学院农业质量标准与检测技术研究所 | Au-Ag nano-chain composite SERS substrate and preparation method and application thereof |
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| CN101026030A (en) * | 2006-12-26 | 2007-08-29 | 安徽师范大学 | Magnetic nano chain preparation and use method |
| CN102151840A (en) * | 2011-03-21 | 2011-08-17 | 天津大学 | Method for preparing noble metal alloy nano material with three-dimensional porous network structure |
| CN102851877A (en) * | 2012-09-11 | 2013-01-02 | 中国科学技术大学 | Method for assembling gold and silver one-dimensional nano-material by adopting electrostatic spinning technology and application thereof |
| CN103170646A (en) * | 2013-03-29 | 2013-06-26 | 太原理工大学 | Synthetic method of nanometer materials of cobalt fractal structure |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101026030A (en) * | 2006-12-26 | 2007-08-29 | 安徽师范大学 | Magnetic nano chain preparation and use method |
| CN102151840A (en) * | 2011-03-21 | 2011-08-17 | 天津大学 | Method for preparing noble metal alloy nano material with three-dimensional porous network structure |
| CN102851877A (en) * | 2012-09-11 | 2013-01-02 | 中国科学技术大学 | Method for assembling gold and silver one-dimensional nano-material by adopting electrostatic spinning technology and application thereof |
| CN103170646A (en) * | 2013-03-29 | 2013-06-26 | 太原理工大学 | Synthetic method of nanometer materials of cobalt fractal structure |
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