CN100450677C - Plant reduction method for preparing silver Nano granules and gold Nano granules - Google Patents

Plant reduction method for preparing silver Nano granules and gold Nano granules Download PDF

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Publication number
CN100450677C
CN100450677C CNB2006101352569A CN200610135256A CN100450677C CN 100450677 C CN100450677 C CN 100450677C CN B2006101352569 A CNB2006101352569 A CN B2006101352569A CN 200610135256 A CN200610135256 A CN 200610135256A CN 100450677 C CN100450677 C CN 100450677C
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grain
nano granules
gold nano
reduction method
gold
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CN1958198A (en
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李清彪
黄加乐
孙道华
何宁
邵文尧
苏远波
杨欣
王惠璇
王远鹏
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Xiamen University
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Xiamen University
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Abstract

A process for preparing Ag nanoparticles and Au nanoparticles by plant reducing method includes such steps as proportionally mixing the dried powder of camphor tree's leaf with the solution of silver nitrate (or chlorauric acid), and reacting at 15-60 deg.C to obtain Ag (or Au) nanoparticles.

Description

Plant reduction method for preparing silver Nano granules and gold nano grain
Technical field
The present invention relates to a kind of silver nano-grain and gold nano grain, especially relate to a kind of method that adopts plant reduction method for preparing silver Nano granules and gold nano grain.
Background technology
Silver nano-grain has a wide range of applications in industrial many fields because of its unique physical and chemical properties, is the main component of ethylene epoxidizing catalyst as silver always; Simple substance silver has very strong sterilizing ability, and after the silver of load was prepared into nano level particle, its bactericidal activity was greatly improved.Gold nano grain makes it show potential using value in fields such as biochemical immunity with its unique optics and electrical properties, good stable, small size and skin effect and unique biological compatibility.The preparation method of silver nano-grain and gold nano grain is always based on physics and chemical method, although comparatively abundant to the research of these two kinds of methods both at home and abroad, technology is also comparatively ripe, and they exist shortcomings such as the higher and easy contaminated environment of production cost.In addition, in recent years, along with some microorganisms are proved under temperate condition, have the ability of reducing metal ion, people recognize and can utilize the micro-reduction method to prepare metal nanoparticle.Shortcomings such as though the micro-reduction method can overcome the traditional chemical method and physics method production cost is higher, easy contaminated environment, but, utilizing the micro-reduction legal system to be equipped with in the process of silver nano-grain and gold nano grain, reduction rate is slower, be unfavorable for the exploitation of course of industrialization, sometimes need to add additives such as acids and bases, to accelerate the biological reducing reaction speed; In addition, the incubation of microorganism comparatively bothers, and causes microbiological contamination easily.In recent years, have report to utilize synthetic silver nano-grain of plant extracts and gold nano grain, as utilize alfalfa living plant or the synthetic gold of living beings or silver nano-grain (1, J.Nanopart.Res., 1999,1,397; 2, Nano Lett., 2002,2,397; 3, Langmuir, 2003,19,1357.) utilize fish pelargonium boil liquid reduction preparation gold or silver nano-grain (1, J.Mater.Chem., 2003,13,1822; 2, Biotechnol.Prog., 2003,9,1627.) utilize lemonweed to boil liquid synthetic triangle sheet gold nano grain (Nat.Mater., 2004,3,482.) utilize the tamarind leaf extract to synthesize triangle sheet gold nano grain (Synth.React.Inorg.Met.-Org.Nano-Metal Chem., that 2005,35,19.) utilizes aloe barbadensis Miller boils liquid reduction AuCl 4 -, the triangle sheet gold nano grain (Biotechnol.Prog., 2006,22,577.) of acquisition high yield.At normal temperatures, utilize plant leaf living beings or boil liquid can be with Ag +, Au 3+Be reduced into silver nano-grain and gold nano grain respectively, its reduction rate and prepared nano particle can compare favourably with the traditional preparation process method, thereby not only can overcome the shortcoming of above-mentioned traditional chemical method and physics method, can also overcome the shortcoming that the micro-reduction method exists.
Summary of the invention
The present invention aims to provide a kind of plant leaf that utilizes with Ag under temperate condition +, Au 3+Be reduced into the new method of silver nano-grain and gold nano grain respectively.
Silver nano-grain preparation method of the present invention the steps include: that Cinnamomum camphora leaves dry powder and the 100ml liquor argenti nitratis ophthalmicus of getting 0.01~10.0g mix, and reacts under 15~60 ℃ of temperature, promptly makes silver nano-grain.
The reaction time that described Cinnamomum camphora leaves dry powder and liquor argenti nitratis ophthalmicus mix is preferably 24~120h.The concentration of liquor argenti nitratis ophthalmicus is preferably 0.01mM~10M.
Gold nano grain preparation method of the present invention the steps include: that Cinnamomum camphora leaves dry powder and the 100ml chlorauric acid solution of getting 0.01~10.0g mix, and reacts under 15~60 ℃ of temperature, promptly makes gold nano grain.
The reaction time that described Cinnamomum camphora leaves dry powder and chlorauric acid solution mix is preferably 1~6h.The concentration of chlorauric acid solution is preferably 0.01mM~10M.
Its Ag of nano-Ag particles of the present invention and nanogold particle +And Au 3+Be that the particle diameter of gained silver nano-grain is at 10~100nm by the reduction of Cinnamomum camphora leaves dry powder, the length of side of triangle sheet gold nano grain is at 25~150nm, and the particle diameter of spherical gold nano grain is at 5~40nm.
Plant leaf of the present invention is that fragrant camphor tree leaf dried powder is different from existing report.The preparation utilization of virtue camphor tree leaf dried powder 40~100 ℃ with fresh fragrant camphor tree leaf oven dry, perhaps fresh fragrant camphor tree leaf is dried outdoor, perhaps under 10~40 ℃ of temperature, utilize cross-ventilation allow fresh fragrant camphor tree leaf natural air drying.Then utilize the method for hand lapping or mechanical lapping, will do fragrant camphor tree leaf and make the dried fine powder of fragrant camphor tree leaf.
Technology of the present invention is simple, does not need the additive except that silver nitrate or gold chloride, and prepared nano level silver-colored particle and gold grain have good dispersiveness and stability in the aqueous solution, form metal nanoparticle colloidal sol easily.
The specific embodiment
The invention will be further described below by embodiment.
Embodiment 1
Pulverize and cross 20 mesh sieves in Cinnamomum camphora leaves and get Cinnamomum camphora leaves dry powder.Take by weighing 5g virtue camphor tree leaf dried powder, with concentration be the AgNO of 10mM 3Solution 100ml reacts in the conical flask of 100ml, is reflected on 40 ℃, the shaking bath of 150r/min to carry out.Behind the reaction 118h, observation post gets silver sol with transmission electron microscope (TEM), and wherein the pattern of silver nano-grain is subsphaeroidal, and the particle diameter overwhelming majority is distributed in 50~80nm, and average grain diameter is 64.8nm.
Embodiment 2
Adopt the Cinnamomum camphora leaves dry powder among the embodiment 1, take by weighing 1g virtue camphor tree leaf dried powder, with concentration be the HAuCl of 10mM 4Solution 100ml reaction, reaction temperature is 30 ℃, other reaction condition is with embodiment 1.With transmission electron microscope sample is observed aurosol, can see a large amount of patterns triangle sheet gold nano grain clearly, the thickness of triangle sheet gold nano grain is in 20nm, and the length of side is at 20~150nm, and the average length of side is 80.0nm.
Embodiment 3
Adopt the Cinnamomum camphora leaves dry powder among the embodiment 1.Take by weighing 5g virtue camphor tree leaf dried powder, with concentration be the HAuCl of 10mM 4Solution 100ml reaction, reaction temperature is 30 ℃, other reaction condition is with embodiment 1.Observe aurosol with transmission electron microscope (TEM), can observe the gold nano grain pattern and be sphere, the particle diameter of gained gold nano grain is distributed in 10~40nm, and average grain diameter is 23.4nm.
Embodiment 4
Adopt the Cinnamomum camphora leaves dry powder among the embodiment 1.Take by weighing 10g virtue camphor tree leaf dried powder, with concentration be the HAuCl of 10mM 4Solution 100ml reaction, reaction temperature is 30 ℃, other reaction condition is with embodiment 1.Behind the reaction 1.5h, observe aurosol with transmission electron microscope (TEM), gained gold nano grain pattern is sphere, and particle diameter is distributed in 15~35nm, and average grain diameter is 21.5nm.

Claims (2)

1. plant reduction method for preparing silver Nano granules, it is characterized in that the steps include: that Cinnamomum camphora leaves dry powder and the 100ml liquor argenti nitratis ophthalmicus of getting 0.01~10.0g mix, the concentration of liquor argenti nitratis ophthalmicus is 0.01mM~10M, reacts 24~120h under 15~60 ℃ of temperature, promptly makes silver nano-grain.
2. plant reduction method prepares gold nano grain, it is characterized in that the steps include: that Cinnamomum camphora leaves dry powder and the 100ml chlorauric acid solution of getting 0.01~10.0g mix, the concentration of chlorauric acid solution is 0.01mM~10M, reacts 1~6h under 15~60 ℃ of temperature, promptly makes gold nano grain.
CNB2006101352569A 2006-11-28 2006-11-28 Plant reduction method for preparing silver Nano granules and gold Nano granules Expired - Fee Related CN100450677C (en)

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US8057682B2 (en) * 2008-05-16 2011-11-15 Verutek Technologies, Inc. Green synthesis of nanometals using plant extracts and use thereof
CN101498037B (en) * 2009-01-14 2011-04-27 厦门大学 Method for preparing single crystal silver nano-wire by plant biomass reduction
CN101905331B (en) * 2010-08-24 2012-02-22 厦门大学 Method for extracting nano-silver in aqueous phase by using ionic liquid
CN101912976A (en) * 2010-08-24 2010-12-15 厦门大学 Method for preparing silver nano granules by reducing plant extract
CN101934238B (en) * 2010-09-10 2011-11-30 厦门大学 Preparation method of ethylene epoxidized silver catalyst
CN102240815A (en) * 2011-06-16 2011-11-16 广东工业大学 Method for preparing nano silver particles by using plant extract for reduction, and application of method
JP2014525906A (en) * 2011-07-12 2014-10-02 ナラヤン バンデール、ヨゲシュ Novel nanogold and its preparation process
CN103464782A (en) * 2013-09-16 2013-12-25 江苏大学 Method utilizing shaddock ped extracting solution to synthesize silver nanoparticles in microwave
CN104889419B (en) * 2015-05-18 2017-01-04 王洁 Biological synthesis method of spherical nano silver particles
CN105127443A (en) * 2015-08-22 2015-12-09 钱景 Preparation of nano-silver particles and application of nano-silver particles
CN105478795B (en) * 2015-12-14 2017-11-28 上海理工大学 A kind of method that silver nano-grain is prepared using sugarcane extract
CN105642911B (en) * 2016-01-27 2018-05-04 陕西科技大学 A kind of synthetic method of nanometer Ag
CN105665737A (en) * 2016-01-27 2016-06-15 陕西科技大学 Biosynthesis method of nano Ag
CN106513701B (en) * 2016-11-10 2018-07-10 江苏省农业科学院 It is a kind of to prepare the ecological method for collecting nano silver
CN106513707B (en) * 2016-12-07 2018-06-08 鲁东大学 A kind of nano silver antibacterial agent and its preparation process using blueberry leaf extract biosynthesis
CN106862590B (en) * 2017-02-24 2018-09-25 华中农业大学 A method of utilizing Guangxi Du's chaste tree blade extract biosynthesis nano silver
CN107265505B (en) * 2017-06-23 2019-04-16 黄山学院 A kind of preparation method of manganese dioxide
CN109909512A (en) * 2017-12-12 2019-06-21 中国科学院深圳先进技术研究院 A kind of silver nanowires and its green magnanimity preparation method
CN110976904B (en) * 2019-11-21 2022-09-06 延安大学 Method for preparing nano silver by using reed extract and application of method in preparation of silver-containing hydrogel fiber cloth
CN111230135B (en) * 2020-03-17 2021-08-24 江南大学 Method for preparing gold nanoparticles
CN113506648B (en) * 2021-09-10 2021-12-21 西安宏星电子浆料科技股份有限公司 Inner-layer gold conductor paste for Ca-B-Si system LTCC
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CN114918422B (en) * 2022-04-27 2024-03-19 南开大学 Mechanochemical preparation method of nano material and nano composite material

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