CN104550995A - Gold-silver composite nano chain antibacterial agent synthesizing method - Google Patents
Gold-silver composite nano chain antibacterial agent synthesizing method Download PDFInfo
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Abstract
The invention relates to a cold-silver composite nano chain antibacterial agent synthesizing method. The method includes the steps: (1) adding a template agent into AgNO3 solution, adjusting system pH value to be 10, dripping a reducing agent into the reaction solution under the condition of stirring, and subjecting the reaction solution to ageing for 1-5h at the room temperature to obtain a Ag nano-particle chain; (2) adding the Ag nano-particle chain into a reactor, using a dispersing agent for dispersing in deionized water, placing a HAuC14 solution filled test tube with a semipermeable membrane seal and a hydrazine hydrate solution filled test tube with a semipermeable membrane seal in the Ag nano-particle chain contained reactor upside down, placing the whole system in an ultrasonic disperser for ultrasonic treatment for 5-10min, subjecting the obtained solution to centrifugal separation, washing for several times, and naturally drying to obtain a Au/Ag composite nano chain. Compared with the prior art, the cold-silver composite nano chain antibacterial agent synthesizing method has the advantages of low preparation cost, technical simplicity, avoidance of pollution, high dispersibility and regular structure of products and the like.
Description
Technical field
The invention belongs to environmental science, be specifically related to a kind of synthetic method of gold and silver composite Nano chain antibacterial agent.
Background technology
Nano Silver is a kind of emerging functional material, has very high specific surface area and surface-active, is widely used as catalyst material, antistatic material, low temperature superconducting material, electric slurry and biology sensor material etc.In addition, Nano Silver also has antibacterial, the function such as deodorizing and absorption portion ultraviolet, thus can be applicable to pharmaceuticals industry and cosmetic industry.In chemical fibre, add a small amount of Nano Silver, some performance of chemical fabrics can be changed, and give very strong sterilizing ability.The metallic element used in existing inorganic fungicide is mainly to silver, copper, zinc etc. that human body is safer, 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, because silver compound or silver metal particle are after touching microorganism, following several respects effect occurring: the combination of the breathing of suppression microorganism, the synthesis hindering enzyme, destruction protein, damaging cells film, interference DNA.Nano silver particles has than common silver compound or the more excellent bactericidal activity of silver metal particle, by a large amount of for fields such as all kinds of washing, health products.
And after Precious Metals-Gold and Nano Silver compound, more excellent physicochemical property can be brought, therefore, receive the extensive attention of researcher.Current reported nanometer gold silver composite Nano bactericide preparation method has cold-maceration (T.Som, B.Karmakar.Core Shell Au Ag Nanoparticles in Dielectric Nanocomposites with Plasmon-Enhanced Fluorescence:A New Paradigmu in Antimony Glasses [J] .Nano Res., 2009, 2:607-616), organic hot solvent method (C.Wang, S.Peng, R.Chan, S.H.Sun, Synthesis of AuAg Alloy Nanoparticles from Core/Shell Structured Ag/Au [J] .small., 2009, 5:567-570), bioanalysis (A.Rai, M.Chaudhary, A.Ahmad, S.Bhargava, M.Sastry.Synthesis of triangular Au core-Ag shell nanoparticles [J] .Materials Research Bulletin, 2007.42:1212-1220), sol-gel process (Y.Okuno, K.Nishioka, A.Kiya, N.Nakashima, A.Ishibashi.Y.Niidome.Uniform and controllable preparation of Au-Ag core-shell nanorods using anisotropic silver shell formation on gold nanorods [J], Nanoscale, 2010, 2:1489-1493), two-step synthesis method .Y Okuno, K.Nishioka, A.Kiya, N.Nakashima, A.Ishibashi, Y.Niidome.Uniform and controllable preparation of Au-Ag core-shell nanorods using anisotropic silver shell formation on gold nanorods [J], Nanoscale, 2010, 2:1489-1493), phonochemistry method (Salkar, R.A., Jeevanandam, P., Aruna, S.T., Koltypin, Y.Gedanken, A.The Sonochemical Preparation of Amorphous Silver Nanoparticles [J] .J.Mater:Chem.1999,9:1333-1335) etc. method.In above-mentioned synthesis, the product of acquisition is mostly nano particle or nano bar-shape composite construction, not yet has the report of the nano combined chain material of gold and silver.According to pertinent literature, we can infer, chain structure nano composite material, when environmental area is applied, due to its structural advantage, has features such as being easier to recovery, the better excellence of bactericidal effect.Therefore, about the preparation of the nano combined chain antibacterial agent of gold and silver, there is important researching value.
Summary of the invention
Object of the present invention is exactly the synthetic method in order to overcome defect that above-mentioned prior art exists and the gold and silver composite Nano chain antibacterial agent that provides a kind of bactericidal effect good.
Object of the present invention can be achieved through the following technical solutions: a kind of synthetic method of gold and silver composite Nano chain antibacterial agent, and it is characterized in that, the method comprises the following steps:
(1) get template and join AgNO
3in solution, the pH value of regulation system is 10, under agitation, instilling reductant to no longer producing precipitation in reaction solution, after reaction solution at room temperature ageing 1-5h, obtaining Ag gold nanochains;
(2) above-mentioned Ag nano chain is added in reactor, with dispersant in deionized water, two fill HAuCl respectively
4the test tube of the band semipermeable membrane sealing of solution and hydrazine hydrate solution, be inverted in the reactor filling Ag nano chain, whole system is placed in ultrasonic disperser ultrasonic process 5-10 minute, obtain the solution of dark red in the reactor, by this solution centrifugation, and with deionized water and absolute ethanol washing for several times, namely natural seasoning obtains Au/Ag composite Nano chain.
Template described in step (1) comprises polyacrylamide, poly-methylcellulose, Sodium Polyacrylate, polyacrylamide, the addition of template and AgNO
3mass ratio be 1:1.7.
The pH value of the regulation system described in step (1) adopt ammoniacal liquor,
Reductant described in step (1) comprises vitamin c solution.
Dispersant described in step (2) is volume ratio is the TGA of 1:20 and the mixture of absolute ethyl alcohol, and 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) adopts comprises collodion membrane, egg film or air bladder.
HAuCl described in step (2)
4be 5 ~ 8:20 with the mol ratio of Ag, the consumption of hydrazine hydrate is excessive.
Compared with prior art, advantage of the present invention is as follows:
(1) the present invention's gold and silver nano combined chain bactericide structure neatly unification of preparing, has antibacterial effect more better than gold and silver nano-complex particle.
(2) transmitting procedure controlling reactive ion with semipermeable membrane is proposed, thus the thickness of the nucleation of control product, crystalline rate and silver particles surface gold, and the dispersion of ion is promoted by the mode of ultrasonic disperse.
(3) adopt vitamin C or glucose as reductant, produce without waste water, waste gas and waste liquid, belong to green syt category.
(4) method technique is simple, and without the need to complex device, whole production process is without any pollution simultaneously, meets sustainable development requirement.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1:
0.02g polyacrylamide is joined 20mL0.01mol/L AgNO
3in solution, being 10 with the pH of ammoniacal liquor regulation system, in mechanical agitation downhill reaction solution, instilling vitamin c solution as reductant to no longer producing precipitation, solution at room temperature ageing 1 hour, high speed centrifugation is separated, washing, obtains elemental silver gold nanochains.
Join in beaker by the silver nanochains of preparation together with 0.05mL TGA and 10mL absolute ethyl alcohol, ultrasonic process is after 5 minutes, and high speed centrifugation is separated, and obtains the silver nanochains of surface TGA process.Surface-treated Ag gold nanochains is joined in beaker, adds the dispersion of 20mL deionized water.7mL0.01mol/L HAuCl will be added respectively
4solution and 5mL hydrazine hydrate (N
2h
4h
2o, 30wt%) two test tubes with collodion membrane sealing after, be inverted be to fill in the beaker of silver nanochains.Ultrasonic 10 minutes of whole system, finally obtains the solution of dark red in beaker.High speed centrifugation is separated, and with deionized water and each 3 times of absolute ethanol washing, natural seasoning, obtain silver-colored golden composite Nano chain antibacterial agent, its length is about 2 microns, and the diameter of Au/Ag composite nanoparticle is about 35 nanometers.
Embodiment 2:
0.02g is gathered methylcellulose and join 20mL0.01mol/L AgNO
3in solution, be 10 with the pH of ammoniacal liquor regulation system, in mechanical agitation downhill reaction solution, instill vitamin c solution as reductant to no longer producing precipitation, solution at room temperature ageing 1 hour, high speed centrifugation is separated, and washing obtains elemental silver nano chain.
Join in beaker by the silver nanochains of preparation together with 0.5mL TGA and 10mL absolute ethyl alcohol, ultrasonic process is after 5 minutes, and high speed centrifugation is separated, and obtains the silver nanochains of surface TGA process.Surface-treated Ag nano chain is joined in beaker, adds the dispersion of 20mL deionized water.8mL0.01mol/L HAuCl will be added respectively
4solution and 6mL hydrazine hydrate (N
2h
4h
2o, 30wt%) two test tubes with egg film sealing after, be inverted be to fill in the beaker of silver nanochains.Ultrasonic 10 minutes of whole system, finally obtains the solution of dark red in beaker.High speed centrifugation is separated, and with deionized water and each 3 times of absolute ethanol washing, natural seasoning, acquisition gold and silver composite Nano chain antibacterial agent, 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/L AgNO
3in solution, be 10 with the pH of ammoniacal liquor regulation system, in mechanical agitation downhill reaction solution, instill vitamin c solution as reductant to no longer producing precipitation, solution at room temperature ageing 1 hour, high speed centrifugation is separated, and washing obtains elemental silver nano chain.
Join in beaker by the silver nanochains of preparation together with 0.5mL TGA and 10mL absolute ethyl alcohol, ultrasonic process is after 5 minutes, and high speed centrifugation is separated, and obtains the silver nanochains of surface TGA process.Surface-treated Ag nano chain is joined in beaker, adds the dispersion of 20mL deionized water.6mL0.01mol/L HAuCl will be added respectively
4solution and 5mL hydrazine hydrate (N
2h
4h
2o, 30wt%) two test tubes with air bladder sealing after, be inverted be to fill in the beaker of silver nanochains.Ultrasonic 10 minutes of whole system, finally obtains the solution of dark red in beaker.High speed centrifugation is separated, and with deionized water and each 3 times of absolute ethanol washing, natural seasoning, acquisition gold and silver composite Nano chain antibacterial agent, 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/L AgNO
3in solution, be 10 with the pH of ammoniacal liquor regulation system, in mechanical agitation downhill reaction solution, instill vitamin c solution as reductant to no longer producing precipitation, solution at room temperature ageing 5 hours, high speed centrifugation is separated, and washing obtains elemental silver nano chain.
Join in beaker by the silver nanochains of preparation together with 0.5mL TGA and 10mL absolute ethyl alcohol, ultrasonic process is after 5 minutes, and high speed centrifugation is separated, and obtains the silver nanochains of surface TGA process.Surface-treated Ag nano chain is joined in beaker, adds the dispersion of 20mL deionized water.5mL0.01mol/L HAuCl will be added respectively
4solution and 5mL hydrazine hydrate (N
2h
4h
2o, 30wt%) two test tubes with egg film sealing after, be inverted be to fill in the beaker of silver nanochains.Ultrasonic 10 minutes of whole system, finally obtains the solution of dark red in beaker.High speed centrifugation is separated, and with deionized water and each 3 times of absolute ethanol washing, natural seasoning, acquisition gold and silver composite Nano chain antibacterial agent, its length is about 3.5 microns, and the diameter of particle is about 28 nanometers.
Claims (7)
1. a synthetic method for gold and silver composite Nano chain antibacterial agent, it is characterized in that, the method comprises the following steps:
(1) get template and join AgNO
3in solution, the pH value of regulation system is 10, under agitation, in reaction solution, instills reductant, after reaction solution at room temperature ageing 1-5h, obtains Ag gold nanochains;
(2) above-mentioned Ag nano chain is added in reactor, with dispersant in deionized water, two fill HAuCl respectively
4the test tube of the band semipermeable membrane sealing of solution and hydrazine hydrate solution, be inverted in the reactor filling Ag nano chain, whole system is placed in ultrasonic disperser ultrasonic process 5-10 minute, obtain the solution of dark red in the reactor, by this solution centrifugation, and with deionized water and absolute ethanol washing for several times, namely natural seasoning obtains Au/Ag composite Nano chain.
2. the synthetic method of a kind of gold and silver composite Nano chain antibacterial agent according to claim 1, it is characterized in that, template described in step (1) comprises polyacrylamide, poly-methylcellulose, Sodium Polyacrylate, polyacrylamide, the addition of template and AgNO
3mass ratio be 1:1.7.
3. the synthetic method of a kind of gold and silver composite Nano chain antibacterial agent according to claim 1, is characterized in that, the pH value of the regulation system described in step (1) adopts ammoniacal liquor.
4. the synthetic method of a kind of gold and silver composite Nano chain antibacterial agent according to claim 1, it is characterized in that, the reductant described in step (1) comprises vitamin c solution.
5. the synthetic method of a kind of gold and silver composite Nano chain antibacterial agent according to claim 1, it is characterized in that, dispersant described in step (2) is volume ratio is the TGA of 1:20 and the mixture of absolute ethyl alcohol, and the addition of dispersant is 50 ~ 60ml/molAg.
6. the synthetic method of a kind of gold and silver composite Nano chain antibacterial agent according to claim 1, is characterized in that, the semipermeable membrane that the test tube of the band semipermeable membrane sealing described in step (2) adopts comprises collodion membrane, egg film or air bladder.
7. the synthetic method of a kind of gold and silver composite Nano chain antibacterial agent according to claim 1, is characterized in that, the HAuCl described in step (2)
4be 5 ~ 8:20 with the mol ratio of Ag.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108941608A (en) * | 2018-08-23 | 2018-12-07 | 安徽中科赛飞尔科技有限公司 | A kind of regulatable silver-colored/golden cavity nanometer rods construction method of shell thickness and its application |
| CN111590085A (en) * | 2020-06-01 | 2020-08-28 | 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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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108941608A (en) * | 2018-08-23 | 2018-12-07 | 安徽中科赛飞尔科技有限公司 | A kind of regulatable silver-colored/golden cavity nanometer rods construction method of shell thickness and its application |
| CN111590085A (en) * | 2020-06-01 | 2020-08-28 | 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 |
| 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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