CN105665737A - Biosynthesis method of nano Ag - Google Patents

Biosynthesis method of nano Ag Download PDF

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Publication number
CN105665737A
CN105665737A CN201610054965.8A CN201610054965A CN105665737A CN 105665737 A CN105665737 A CN 105665737A CN 201610054965 A CN201610054965 A CN 201610054965A CN 105665737 A CN105665737 A CN 105665737A
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green tea
solution
ultra
nanometer
nano
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杨辉
任雁宇
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05Metallic powder characterised by the size or surface area of the particles
    • B22F1/054Nanosized particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Composite Materials (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Colloid Chemistry (AREA)

Abstract

A biosynthesis method of nano Ag comprises the following steps: adding green tea in ultra-pure water, heating in water bath and then filtering, and cooling to obtain a green tea extracting solution; adding AgNO3 crystals in the ultra-pure water to obtain an AgNO3 solution, mixing the green tea extracting solution and the AgNO3 solution, and magnetically stirring at room temperature to obtain a nano Ag colloidal solution; and washing precipitate obtained after centrifuging of the nano Ag colloidal solution by using the ultra-pure water, and then drying to obtain nano Ag particles with particle sizes of 5-20 nm. The green tea extracting solution is used as a reducing agent and a dispersing agent, the nano Ag particles are reduced and prepared from a silver nitrate (AgNO3) solution, in order to improve quality of products, the ultra-pure water is used as a solvent, any chemical reagents are not required, conditions are simple and mild, raw materials are easy to obtain, the method is easy and convenient to operate, sizes of the obtained products are uniform, and dispersity is good.

Description

A kind of biological synthesis method of nanometer Ag
Technical field
The invention belongs to field of nanometer technology, relate to the biological synthesis method of a kind of nanometer Ag.
Background technology
Nanometer Ag is owing to having specific surface area effect, small size effect, quantum effect, physicochemical property that catalytic performance and anti-microbial property etc. are special and be subject to concern (ReutherR.TheNanoSustainandNanoValidProject-TwoNewEUFP7Re searchInitiativestoAssesstheUniquePhysical-ChemicalandTo xicologicalPropertiesofEngineeredNanomaterials [J] .JBiomedNanotechnol widely, 2011,7 (1): 8-10.). in recent years, along with going deep into of Study of synthesis method, obtained nanometer Ag material is widely used (AnjumS in the industry such as food, medical treatment gradually, SharmaA, TummalapalliM, etal.ANovelRouteforthePreparationofSilverLoadedPolyvinyl AlcoholNanogelsforWoundCareSystems [J] .IntJPolymMaterPo, 2015,64 (17): 894-905.). so the synthetic method of green non-hazardous just becomes the focus of research. the method of synthesis nanometer Ag includes physics, chemistry and bioanalysis. Physical is high to equipment requirements, and condition is harsh, it is difficult to expand scale, chemical method is not fee from and uses poisonous chemical reagent, and this not only pollutes the environment and also can bring potentially hazardous to the industry of applying nano materials, so, by contrast, bioanalysis has bigger advantage. at present, biological synthesis process mainly uses microorganism (SatyavniK, GurudeebanS, RamanthanT, etal.Biomedicalpotentialofsilvernanoparticlessynthesized fromcallicellsofCitrulluscolocynthis (L.) Schrad [J] .Journalofnanobiotechnology, 2011, 9 (43) and containing abundant flavone, polyphenol and protein compound plant stem-leaf extracting solution (ArunachalamR, DhanasinghS, KalmuthuB, etal.PhytosynthesisofsilvernanoparticlesusingCocciniagra ndisleafextractanditsapplicationinthephotocatalyticdegra dation [J] .ColloidsandsurfacesB, Biointerfaces, 2012, 94 (226-30.), (JAcobSJ, FinubJS, NarayananA.SynthesisofsilvernanoparticlesusingPiperlongu mleafextractsanditscytotoxicactivityagainstHep-2cellline [J] .ColloidsandsurfacesB, Biointerfaces, 2012, 91 (212-4.) are from Ag+In solution, reduction prepares nano Ag particles.
(the PhilipD such as DaizyPhilip, UnniC, AromalLSA, etal.MurrayaKoenigiileaf-assistedrapidgreensynthesisofsi lverandgoldnanoparticles [J] .SpectrochimicaactaPartA, Molecularandbiomolecularspectroscopy, 2011,78 (2): 899-904.) prepared the nano Ag particles of about 20nm as reducing agent with MurrayaKoenigii leaf extract, but containing substantial amounts of impurity; (the AshokkumarS such as S.Ashokkumar, RaviS, KathiravanV, etal.Synthesis, characterizationandcatalyticactivityofsilvernanoparticle susingTribulusterrestrisleafextract [J] .SpectrochimicaactaPartA, Molecularandbiomolecularspectroscopy, 2014,121 (88-93.) utilize Tribulusterrestris leaf extract at room temperature respectively with variable concentrations Ag+Solution reaction, obtains 15~40nm, and nanometer Ag particle size distribution is wider, and ratio of reuniting is more serious, Chinese invention patent CN201410540835.6 is with commercial beverage for reducing agent, it is blended in ultrasonic 1~10h under the temperature conditions of 20 DEG C~60 DEG C with the volume ratio of 100:1~1:1 with the silver ammino solution of mass fraction 0.01~100g/L, obtain nano-class silver colloidal solution, repeatedly clean with ethanol and deionized water, centrifugal, obtain nanometer silver after dried. the method complicated condition, and the nano Ag particles obtained contains the organic compound being difficult to eluting in a large number, can affect purity and the range of application of nanometer Ag. in addition, green tea extractive liquor is also used to preparation nanometer Ag (SunQ, CaiX, LIJ, etal.Greensynthesisofsilvernanoparticlesusingtealeafextr actandevaluationoftheirstabilityandantibacterialactivity [J] .ColloidsandSurfacesA:PhysicochemicalandEngineeringAspec ts, 2014, 444 (226-31.), (BabuS, ClavilleMO, GhebreyessusK.Rapidsynthesisofhighlystablesilvernanopart iclesanditsapplicationforcolourimetricsensingofcysteine [J] .JournalofExperimentalNanoscience, 2015, 10 (16): 1242-55.), (NadagoudaMN, VarmaRS.Greensynthesisofsilverandpalladiumnanoparticlesa troomtemperatureusingcoffeeandteaextract [J] .GreenChemistry, 2008, 10 (8): 859.), (LooYY, ChiengBW, NishibuchiIM, etal.Synthesisofsilvernanoparticlesbyusingtealeafextract fromCamelliasinensis [J] .Internationaljournalofnanomedicine, 2012, 7 (4263-7.), but it is impure all to there is product in these synthetic methods, particle diameter is bigger and uneven, the shortcomings such as degree of crystallinity difference.
Summary of the invention
Present invention aims to the deficiency of above synthetic method, a kind of raw material is provided to be easy to get, condition is simple, workable, it is suitable for the biological synthesis method of the nanometer Ag of large-scale industrial production, the nanometer Ag material prepared is pure, without any chemical substance, it is possible to stable dispersion as additive.
For reaching above-mentioned purpose, the technical solution used in the present invention is:
1) take green tea and by the mass ratio of 1:40~100, green tea is added to the water 80~100 DEG C of water-bath 10~40min with water, filter, cooling, obtain green tea extractive liquor;
2) AgNO is taken3It is the AgNO of 0.02~0.08mol/L that crystal is added to the water preparation concentration3Solution, is placed in lucifuge place stand-by;
3) by green tea extractive liquor and AgNO3Solution presses the volume ratio mixing of 1:20~40, and under room temperature, magnetic agitation obtains nanometer Ag colloid solution;
4) by the nanometer Ag colloid solution centrifuge at 5000~10000r/min, gained precipitation use water cyclic washing 3~4 times, dry within 6~12 hours, obtain the nano Ag particles that particle diameter is 5~20nm at 80~150 DEG C.
In order to improve the quality of product, the present invention is using ultra-pure water as solvent.
The present invention is with green tea extractive liquor for reducing agent and dispersant, from silver nitrate (AgNO3) in solution reduction prepare nano Ag particles, it is not necessary to adding any chemical reagent, condition is simply gentle, and raw material is easy to get, easy and simple to handle feasible, and products therefrom size is uniform, good dispersion.
The present invention is with AgNO3For raw material, with green tea extractive liquor for reducing agent, wide material sources are easy to get, environmental protection, and containing compounds such as abundant polyphenol, flavone and protides in green tea extractive liquor. These compounds contain substantial amounts of polar group, can with positively charged Ag+Coordination is occurred to cause Ag+Activeness reduce, thus simultaneously work as reduction and peptizaiton so that the nanometer Ag uniform particle sizes obtained and good stability. The present invention eliminates the incubation that microorganism is loaded down with trivial details, it is to avoid using the large amount of organic that fruit juice peel brings, and condition is simply gentle, product is easy. The nanometer silver particle diameter that this technology obtains is 5~20nm.
Accompanying drawing explanation
Fig. 1 is the XRD diffracting spectrum of the nanometer Ag of embodiment 1 preparation;
Fig. 2 a is the TEM photo of embodiment 1;
Fig. 2 b is the TEM high-resolution photo of embodiment 1.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Embodiment 1:
1) take green tea and by the mass ratio of 1:80, green tea is added 90 DEG C of water-bath 30min in ultra-pure water with ultra-pure water, filter, cooling, obtain green tea extractive liquor;
2) AgNO is taken3It is the AgNO of 0.02mol/L that crystal adds preparation concentration in ultra-pure water3Solution, is placed in lucifuge place stand-by;
3) by green tea extractive liquor and AgNO3Solution presses the volume ratio mixing of 1:30, and under room temperature, magnetic agitation obtains nanometer Ag colloid solution;
4) by the nanometer Ag colloid solution centrifuge at 10000r/min, gained precipitation ultra-pure water cyclic washing 3~4 times, dry within 6 hours, obtain nano Ag particles at 150 DEG C.
Fig. 1 is the XRD diffracting spectrum of nanometer Ag prepared by the present embodiment, as seen from the figure in 2 θ=38.118,44.304,64.450, (111) at 77.407,81.550 five places, (200), (220), (311) and (222) these five crystal faces have very strong absworption peak, and this shows that synthesized nanometer Ag crystallinity is fine.
Fig. 2 a and Fig. 2 b is the SEM figure of nanometer Ag prepared by the present embodiment, it can be seen that nanometer Ag is spherical in shape, and is evenly distributed, and mean diameter is at 5~20nm.
Embodiment 2:
1) take green tea and by the mass ratio of 1:60, green tea is added 100 DEG C of water-bath 10min in ultra-pure water with ultra-pure water, filter, cooling, obtain green tea extractive liquor;
2) AgNO is taken3It is the AgNO of 0.06mol/L that crystal adds preparation concentration in ultra-pure water3Solution, is placed in lucifuge place stand-by;
3) by green tea extractive liquor and AgNO3Solution presses the volume ratio mixing of 1:20, and under room temperature, magnetic agitation obtains nanometer Ag colloid solution;
4) by the nanometer Ag colloid solution centrifuge at 8000r/min, gained precipitation ultra-pure water cyclic washing 3~4 times, dry within 12 hours, obtain nano Ag particles at 80 DEG C.
Embodiment 3:
1) take green tea and by the mass ratio of 1:40, green tea is added 80 DEG C of water-bath 40min in ultra-pure water with ultra-pure water, filter, cooling, obtain green tea extractive liquor;
2) AgNO is taken3It is the AgNO of 0.08mol/L that crystal adds preparation concentration in ultra-pure water3Solution, is placed in lucifuge place stand-by;
3) by green tea extractive liquor and AgNO3Solution presses the volume ratio mixing of 1:40, and under room temperature, magnetic agitation obtains nanometer Ag colloid solution;
4) by the nanometer Ag colloid solution centrifuge at 5000r/min, gained precipitation ultra-pure water cyclic washing 3~4 times, dry within 8 hours, obtain nano Ag particles at 100 DEG C.
Embodiment 4:
1) take green tea and by the mass ratio of 1:100, green tea is added 95 DEG C of water-bath 15min in ultra-pure water with ultra-pure water, filter, cooling, obtain green tea extractive liquor;
2) AgNO is taken3It is the AgNO of 0.05mol/L that crystal adds preparation concentration in ultra-pure water3Solution, is placed in lucifuge place stand-by;
3) by green tea extractive liquor and AgNO3Solution presses the volume ratio mixing of 1:25, and under room temperature, magnetic agitation obtains nanometer Ag colloid solution;
4) by the nanometer Ag colloid solution centrifuge at 7000r/min, gained precipitation ultra-pure water cyclic washing 3~4 times, dry within 10 hours, obtain nano Ag particles at 130 DEG C.
Embodiment 5:
1) take green tea and by the mass ratio of 1:50, green tea is added 85 DEG C of water-bath 35min in ultra-pure water with ultra-pure water, filter, cooling, obtain green tea extractive liquor;
2) AgNO is taken3It is the AgNO of 0.07mol/L that crystal adds preparation concentration in ultra-pure water3Solution, is placed in lucifuge place stand-by;
3) by green tea extractive liquor and AgNO3Solution presses the volume ratio mixing of 1:35, and under room temperature, magnetic agitation obtains nanometer Ag colloid solution;
4) by the nanometer Ag colloid solution centrifuge at 9000r/min, gained precipitation ultra-pure water cyclic washing 3~4 times, dry within 7 hours, obtain nano Ag particles at 90 DEG C.
Embodiment 6:
1) take green tea and by the mass ratio of 1:90, green tea is added 90 DEG C of water-bath 40min in ultra-pure water with ultra-pure water, filter, cooling, obtain green tea extractive liquor;
2) AgNO is taken3It is the AgNO of 0.03mol/L that crystal adds preparation concentration in ultra-pure water3Solution, is placed in lucifuge place stand-by;
3) by green tea extractive liquor and AgNO3Solution presses the volume ratio mixing of 1:28, and under room temperature, magnetic agitation obtains nanometer Ag colloid solution;
4) by the nanometer Ag colloid solution centrifuge at 6000r/min, gained precipitation ultra-pure water cyclic washing 3~4 times, dry within 11 hours, obtain nano Ag particles at 120 DEG C.
Embodiment 7:
1) take green tea and by the mass ratio of 1:70, green tea is added 100 DEG C of water-bath 20min in ultra-pure water with ultra-pure water, filter, cooling, obtain green tea extractive liquor;
2) AgNO is taken3It is the AgNO of 0.04mol/L that crystal adds preparation concentration in ultra-pure water3Solution, is placed in lucifuge place stand-by;
3) by green tea extractive liquor and AgNO3Solution presses the volume ratio mixing of 1:32, and under room temperature, magnetic agitation obtains nanometer Ag colloid solution;
4) by the nanometer Ag colloid solution centrifuge at 10000r/min, gained precipitation ultra-pure water cyclic washing 3~4 times, dry within 9 hours, obtain nano Ag particles at 110 DEG C.

Claims (2)

1. the biological synthesis method of a nanometer Ag, it is characterised in that:
1) take green tea and by the mass ratio of 1:40~100, green tea is added to the water 80~100 DEG C of water-bath 10~40min with water, filter, cooling, obtain green tea extractive liquor;
2) AgNO is taken3It is the AgNO of 0.02~0.08mol/L that crystal is added to the water preparation concentration3Solution, is placed in lucifuge place stand-by;
3) by green tea extractive liquor and AgNO3Solution presses the volume ratio mixing of 1:20~40, and under room temperature, magnetic agitation obtains nanometer Ag colloid solution;
4) by the nanometer Ag colloid solution centrifuge at 5000~10000r/min, gained precipitation use water cyclic washing 3~4 times, dry within 6~12 hours, obtain the nano Ag particles that particle diameter is 5~20nm at 80~150 DEG C.
2. the biological synthesis method of nanometer Ag according to claim 1, it is characterised in that: described water is ultra-pure water.
CN201610054965.8A 2016-01-27 2016-01-27 Biosynthesis method of nano Ag Pending CN105665737A (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106538625A (en) * 2016-10-26 2017-03-29 广西大学 A kind of biosynthesis Nano Silver fishery disinfectant
CN107758628A (en) * 2017-08-31 2018-03-06 华南农业大学 A kind of nanometer selenium for preparing the method for nanometer selenium using camellia plant water extract and being prepared
CN107893038A (en) * 2017-11-17 2018-04-10 中山大学 A kind of termite bacterium and its method for synthesizing nano-silver
CN109909513A (en) * 2019-04-26 2019-06-21 中国科学院西双版纳热带植物园 A kind of method and purposes with comospore Glochidion puberum biosynthesis nano silver particles
CN110026550A (en) * 2018-11-07 2019-07-19 扬州工业职业技术学院 A kind of nano zero-valence copper and preparation method and application
CN110076349A (en) * 2019-06-13 2019-08-02 江苏汇诚医疗科技有限公司 A kind of environment-friendly preparation method thereof of petal-shaped Nano silver piece
CN110810445A (en) * 2019-11-19 2020-02-21 西北民族大学 Method for biologically synthesizing nano-silver bacteriostatic agent by utilizing Tibetan medicine willow tea extract
CN113084182A (en) * 2021-03-04 2021-07-09 福建农林大学 Method for preparing nano-silver by using tea leaching solution as raw material

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106538625A (en) * 2016-10-26 2017-03-29 广西大学 A kind of biosynthesis Nano Silver fishery disinfectant
CN107758628A (en) * 2017-08-31 2018-03-06 华南农业大学 A kind of nanometer selenium for preparing the method for nanometer selenium using camellia plant water extract and being prepared
CN107758628B (en) * 2017-08-31 2020-10-09 华南农业大学 Method for preparing nano-selenium by using camellia plant water extract and nano-selenium prepared by method
CN107893038A (en) * 2017-11-17 2018-04-10 中山大学 A kind of termite bacterium and its method for synthesizing nano-silver
CN110026550A (en) * 2018-11-07 2019-07-19 扬州工业职业技术学院 A kind of nano zero-valence copper and preparation method and application
CN109909513A (en) * 2019-04-26 2019-06-21 中国科学院西双版纳热带植物园 A kind of method and purposes with comospore Glochidion puberum biosynthesis nano silver particles
CN109909513B (en) * 2019-04-26 2022-03-04 中国科学院西双版纳热带植物园 Method for biologically synthesizing nano silver particles by using glochidion pubescens and application
CN110076349A (en) * 2019-06-13 2019-08-02 江苏汇诚医疗科技有限公司 A kind of environment-friendly preparation method thereof of petal-shaped Nano silver piece
CN110076349B (en) * 2019-06-13 2022-02-18 江苏汇诚医疗科技有限公司 Green preparation method of petal-shaped silver nanosheets
CN110810445A (en) * 2019-11-19 2020-02-21 西北民族大学 Method for biologically synthesizing nano-silver bacteriostatic agent by utilizing Tibetan medicine willow tea extract
CN110810445B (en) * 2019-11-19 2021-06-01 西北民族大学 Method for biologically synthesizing nano-silver bacteriostatic agent by utilizing Tibetan medicine willow tea extract
CN113084182A (en) * 2021-03-04 2021-07-09 福建农林大学 Method for preparing nano-silver by using tea leaching solution as raw material

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