CN106112008B - The method for preparing nano silver using sweet osmanthus blade - Google Patents
The method for preparing nano silver using sweet osmanthus blade Download PDFInfo
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- CN106112008B CN106112008B CN201610684109.0A CN201610684109A CN106112008B CN 106112008 B CN106112008 B CN 106112008B CN 201610684109 A CN201610684109 A CN 201610684109A CN 106112008 B CN106112008 B CN 106112008B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The method for preparing nano silver using sweet osmanthus blade, comprising the following steps: sweet osmanthus blade is cleaned into drying removing petiole with sterile water and main lobe arteries and veins is cut into about 1cm2Fragment；1-20g fragment is taken 30min is heated and stirred in the water-bath for being placed in 90 DEG C to obtain mixture in mixing with 100ml deionized water；Mixture filters while hot in the funnel for being lined with aseptic filter paper, and filtrate is cooled to room temperature spare；The ratio of 1:9 mixes filtrate with deionized water by volume, and HCl solution and NaOH solution are added in mixed liquor, and adjusting pH of mixed is 9；AgNO is added in above-mentioned mixed liquor3Powder makes AgNO in mixed liquor3Concentration is 1-8mmol/L；Above-mentioned mixed liquor, which is placed in reaction 15min in 60-80 DEG C of water-bath, can be obtained nano silver.This method has easy to operate, inexpensive, low energy consumption, hypotoxicity, while also having high yield and high stability.
Description
Technical field
The present invention relates to nano material and field of nanometer technology, specifically a kind of side that nano silver is prepared using sweet osmanthus blade
Method.
Background technique
Nano particle, also known as nano-powder refer to size at least in one dimension in nanometer scale (1-100nm)
Ultrafine dust.Special small-size effect, skin effect, quantum size effect and macro quanta tunnel effect etc., make it
Show the property different from macroscopic material.Nano silver is a kind of important metal nanoparticle, in ion detection, chemistry
Substance detection, fluorescence signal enhancing, Surface enhanced Raman scattering, anti-microbial property research and medical treatment etc. all have high
Application value.With science and technology fast development, nano silver just gradually penetrating into we life every nook and cranny, as antibacterial toothbrush,
Antibacterial towel, medical antibacterial gauze and household electrical appliance etc..Nano silver is as a kind of new antibacterial agent, with broad spectrum activity, efficiently
Property and the features such as persistence, be widely used to the inhibition research of the pathogenic microorganisms such as bacterium, fungi and virus at present.
Traditional nano silver preparation method mainly includes physical method and chemical method.The nano silver purity of physical method preparation
It is higher, active relatively strong, but low output, equipment cost are expensive, energy consumption is high and stability is poor.The nanometer of chemical method preparation
Silver-colored yield is high, equipment investment is few, speed is fast, but be easily mixed into impurity, highly toxic reagent biology is caused with environment it is potentially hazardous.
As environmental protection is increasingly rooted in the hearts of the people, low power consuming, low cost and environmentally friendly biological synthesis method more meet
" Green Chemistry " theory.This method avoid complicated mechanically actuated and the use of high poison chemical reagent, abundant raw materials, energy
Enough large-scale productions and low in cost, have become one of the hot spot of field of nanometer material technology research at present.
The raw material of biosynthesis nano silver mainly have microorganism (bacterium, actinomyces, fungi) and higher plant.2000
Year, Joerger etc. is using pseudomonas stanieri (Pseudomonas stutzeri) synthesis partial size between the three of 20-200nm
Angular or spherical nano-silver, subsequent bacillus, Escherichia coli, saccharomycete and sickle-like bacteria etc. are used to prepare nano silver one after another.
Since Torresde in 2002 etc. is reported for the first time using silver nano-grain of the clover synthesis partial size less than 10nm, more and more
Plant is used for such research, such as onion, persimmon, STEVIA REBAUDIANA, banyan and Afghan pine.
Summary of the invention
The technical problem to be solved in the present invention is to provide the method for preparing nano silver using sweet osmanthus blade, this method has easy
Operation, low cost, low energy consumption, hypotoxicity, while also there is high yield and high stability.
The method for preparing nano silver using sweet osmanthus blade, comprising the following steps:
(1) the sweet osmanthus blade of acquisition is cleaned with sterile water and is dried up in aseptic operating platform, remove petiole and main lobe
Arteries and veins is simultaneously cut into about 1cm2Fragment；
(2) it takes 1-20g fragment that 100ml deionized water is added in beaker to be uniformly mixed, is subsequently placed in 90 DEG C of water-bath
Middle heating 30min obtains mixture with stirring in heating process；
(3) mixture filters while hot in the funnel for being lined with aseptic filter paper, and filtrate is cooled to room temperature spare；
(4) filtrate and deionized water are mixed to get mixed liquor by the ratio of 1:9 by volume, are then added in mixed liquor
HCl solution and NaOH solution, the pH for adjusting mixed liquor is 9；
(5) AgNO is added in step (4) described mixed liquor3Powder makes AgNO in mixed liquor3Concentration is 1-8mmol/
L；
(6) above-mentioned mixed liquor is placed in reaction 15min in 60-80 DEG C of water-bath can be obtained nano silver.
Preferably, using 5g fragment in the step (2), solution ph is 9 in step (4), step (5) mixing
AgNO in liquid3Concentration is 1 mmol/L, and water bath temperature is 60 DEG C in step (6).
Raw material has drawn from the blade of the sweet osmanthus under Oleaceae in the present invention, and filtrate is served as also in nano silver synthesis process
Former agent, by the Ag in solution+It is reduced to Ag simple substance.Ag in solution+It serves as in reaction and is reduced substance.
By taking preferred embodiment as an example, by above-mentioned steps, solution becomes faint yellow from colourless, indicates the formation of nano silver.
Its absorbance is surveyed using ultraviolet-uisible spectrophotometer, there is strong absworption peak at 460nm in obtained absorption spectrum,
Its plasma resonance for corresponding to nanometer silver surface, further determined the formation of nano silver.
Product is further analyzed with transmission electron microscope (TEM), the nano silver that TEM is synthesized as the result is shown is ball
Shape is subsphaeroidal, favorable dispersibility, partial size 10-35nm, according to TEM image, randomly selects 200 nano-Ag particles, utilizes
Image J software is measured and is analyzed, and 105 nano-Ag particles are distributed within the scope of 10-20nm, and 85 are distributed in 20-30nm；
10 are distributed in 30-40nm.
According to Nano silver solution prepared by above-mentioned preferred embodiment, now its bacteriostatic activity is measured by experiment, this reality
It tests and nano silver and existing Pesticide Tebuconazole compares the fungistatic effect of southern corn leaf blight.
One, experimental procedure:
A, prepared by Nano silver solution
(1) the sweet osmanthus blade of acquisition is cleaned with sterile water and is dried up in aseptic operating platform, remove petiole and main lobe
Arteries and veins is simultaneously cut into about 1cm2Fragment；
(2) it takes 5g fragment that 100ml deionized water is added in beaker to be uniformly mixed, is subsequently placed in 90 DEG C of water-bath and adds
Hot 30min obtains mixture with stirring in heating process；
(3) mixture filters while hot in the funnel for being lined with aseptic filter paper, and filtrate is cooled to room temperature spare；
(4) filtrate and deionized water are mixed to get mixed liquor by the ratio of 1:9 by volume, are then added in mixed liquor
HCl solution and NaOH solution adjust the pH to 9 of mixed liquor；
(5) AgNO is added in step (4) described mixed liquor3Powder makes AgNO in mixed liquor3Concentration is 1mmol/L；
(6) above-mentioned mixed liquor is placed in reaction 15min in 60 DEG C of water-bath can be obtained nano silver.
B, comparative test
(1) southern corn leaf blight is cultivated 5-7 days in constant incubator, then prepares bacterium with aseptic water washing mycelium
Suspension, and adjusting spore concentration under the microscope is 106A/ml(blood cell plate counts), and each section spore concentration is made to keep one
It causes；
(2) 100 μ l bacteria suspensions are drawn respectively with liquid-transfering gun to drop on 6 identical PDA plate culture mediums, are applied using sterilizing
Cloth stick is coated with uniformly；
(3) aseptic filter paper piece that diameter is 5mm is clamped respectively with sterilizing tweezers to be placed on above-mentioned 6 PDA plate culture mediums,
Each PDA plate culture medium is equipped with 3 aseptic filter paper pieces, 3 aseptic filter paper on pieces on each PDA plate culture medium point
10 μ l Nano silver solutions, 10 μ l Tebuconazoles (20 μ g/ml) and 10 μ l blade filtrates are not added dropwise, stand 5-10min；
(4) 6 groups of PDA plate culture mediums are placed in constant incubator, dark condition culture 2-3 days at 30 DEG C, are observed
Dropwise addition object on each filter paper is to the inhibitory effect of southern corn leaf blight and measures antibacterial circle diameter.
Two, experimental result and analysis
It is general in order to have more experimental result, in comparative test, use 6 groups of parallel tests, nano silver in every group
Solution is experimental group, and tebuconazole solution is comparison, and blade filtrate is blank control.Result is as follows after processing for experimental data:
Nano silver solution average diameter of inhibition zone is 11.3 ± 0.24mm, and tebuconazole solution average diameter of inhibition zone is 7.3
± 0.85mm, blade filtrate do not have bacteriostasis property.
It can thus be seen that a kind of being prepared prepared by the method for nano silver using sweet osmanthus blade through provided by the present invention
Nano silver, fungistatic effect is better than existing Tebuconazole, and stability is also more preferable.
Advantages of the present invention: sweet osmanthus blade is evergreen all the year round, it can be ensured that raw material are sufficient, and it is raw to be conducive to industrial mass
It produces.This method is easy to operate, time-consuming is short, not using toxic chemicals in raw material, does not also have in the preparation process of nano silver
There is the ingredient for generating and having pollution to environment.The nano silver prepared is with high purity, stability is good, the strong uniform particle sizes of sterilizing ability, fits
For inhibiting in pathogen, the reverse of pathogen drug resistance, environment detection of heavy metal ion, toxic compounds detection etc. many necks
Domain.
Specific embodiment
Embodiment one:
(1) the sweet osmanthus blade of acquisition is cleaned with sterile water and is dried up in aseptic operating platform, remove petiole and main lobe
Arteries and veins is simultaneously cut into about 1cm2Fragment；
(2) it takes 1g fragment that 100ml deionized water is added in beaker to be uniformly mixed, is subsequently placed in 90 DEG C of water-bath and adds
Hot 30min obtains mixture with stirring in heating process；
(3) mixture filters while hot in the funnel for being lined with aseptic filter paper, and filtrate is cooled to room temperature spare；
(4) filtrate and deionized water are mixed to get mixed liquor by the ratio of 1:9 by volume, are then added in mixed liquor
HCl solution and NaOH solution adjust the pH to 11 of mixed liquor；
(5) AgNO is added in step (4) described mixed liquor3Powder makes AgNO in mixed liquor3Concentration is 4mmol/L；
(6) above-mentioned mixed liquor is placed in reaction 15min in 80 DEG C of water-bath can be obtained nano silver.
Taking spore concentration is 106A/ml(blood cell plate counts) southern corn leaf blight bacteria suspension, it is flat to be spread evenly across PDA
On plate culture medium, taking diameter is that the aseptic filter paper piece of 5mm is placed on above-mentioned PDA plate culture medium, is added dropwise in above-described embodiment and makes
10 μ l of Nano silver solution, stand dark condition culture 2-3 days at 30 DEG C again after 10min, measuring its antibacterial circle diameter is
10.2±0.62mm。
Embodiment two:
(1) the sweet osmanthus blade of acquisition is cleaned with sterile water and is dried up in aseptic operating platform, remove petiole and main lobe
Arteries and veins is simultaneously cut into about 1cm2Fragment；
(2) it takes 2g fragment that 100ml deionized water is added in beaker to be uniformly mixed, is subsequently placed in 90 DEG C of water-bath and adds
Hot 30min obtains mixture with stirring in heating process；
(3) mixture filters while hot in the funnel for being lined with aseptic filter paper, and filtrate is cooled to room temperature spare；
(4) filtrate and deionized water are mixed to get mixed liquor by the ratio of 1:9 by volume, are then added in mixed liquor
HCl solution and NaOH solution adjust the pH to 11 of mixed liquor；
(5) AgNO is added in step (4) described mixed liquor3Powder makes AgNO in mixed liquor3Concentration is 1mmol/L；
(6) above-mentioned mixed liquor is placed in reaction 15min in 80 DEG C of water-bath can be obtained nano silver.
Taking spore concentration is 106A/ml(blood cell plate counts) southern corn leaf blight bacteria suspension, it is flat to be spread evenly across PDA
On plate culture medium, taking diameter is that the aseptic filter paper piece of 5mm is placed on above-mentioned PDA plate culture medium, is added dropwise in above-described embodiment and makes
10 μ l of Nano silver solution, stand dark condition culture 2-3 days at 30 DEG C again after 10min, measuring its antibacterial circle diameter is
7.5±0.41mm。
Embodiment three:
(1) the sweet osmanthus blade of acquisition is cleaned with sterile water and is dried up in aseptic operating platform, remove petiole and main lobe
Arteries and veins is simultaneously cut into about 1cm2Fragment；
(2) it takes 5g fragment that 100ml deionized water is added in beaker to be uniformly mixed, is subsequently placed in 90 DEG C of water-bath and adds
Hot 30min obtains mixture with stirring in heating process；
(3) mixture filters while hot in the funnel for being lined with aseptic filter paper, and filtrate is cooled to room temperature spare；
(4) filtrate and deionized water are mixed to get mixed liquor by the ratio of 1:9 by volume, are then added in mixed liquor
HCl solution and NaOH solution adjust the pH to 9 of mixed liquor；
(5) AgNO is added in step (4) described mixed liquor3Powder makes AgNO in mixed liquor3Concentration is 1mmol/L；
(6) above-mentioned mixed liquor is placed in reaction 15min in 60 DEG C of water-bath can be obtained nano silver.
Taking spore concentration is 106A/ml(blood cell plate counts) southern corn leaf blight bacteria suspension, it is flat to be spread evenly across PDA
On plate culture medium, taking diameter is that the aseptic filter paper piece of 5mm is placed on above-mentioned PDA plate culture medium, is added dropwise in above-described embodiment and makes
10 μ l of Nano silver solution, stand dark condition culture 2-3 days at 30 DEG C again after 10min, measuring its antibacterial circle diameter is
11.3±0.24mm。
Example IV:
(1) the sweet osmanthus blade of acquisition is cleaned with sterile water and is dried up in aseptic operating platform, remove petiole and main lobe
Arteries and veins is simultaneously cut into about 1cm2Fragment；
(2) it takes 10g fragment that 100ml deionized water is added in beaker to be uniformly mixed, be subsequently placed in 90 DEG C of water-bath
30min is heated, adjoint stirring in heating process obtains mixture；
(3) mixture filters while hot in the funnel for being lined with aseptic filter paper, and filtrate is cooled to room temperature spare；
(4) filtrate and deionized water are mixed to get mixed liquor by the ratio of 1:9 by volume, are then added in mixed liquor
HCl solution and NaOH solution adjust the pH to 9 of mixed liquor；
(5) AgNO is added in step (4) described mixed liquor3Powder makes AgNO in mixed liquor3Concentration is 4mmol/L；
(6) above-mentioned mixed liquor is placed in reaction 15min in 60 DEG C of water-bath can be obtained nano silver.
Taking spore concentration is 106A/ml(blood cell plate counts) southern corn leaf blight bacteria suspension, it is flat to be spread evenly across PDA
On plate culture medium, taking diameter is that the aseptic filter paper piece of 5mm is placed on above-mentioned PDA plate culture medium, is added dropwise in above-described embodiment and makes
10 μ l of Nano silver solution, stand dark condition culture 2-3 days at 30 DEG C again after 10min, measuring its antibacterial circle diameter is
9.2±0.62mm。
Embodiment five:
(1) the sweet osmanthus blade of acquisition is cleaned with sterile water and is dried up in aseptic operating platform, remove petiole and main lobe
Arteries and veins is simultaneously cut into about 1cm2Fragment；
(2) it takes 15g fragment that 100ml deionized water is added in beaker to be uniformly mixed, be subsequently placed in 90 DEG C of water-bath
30min is heated, adjoint stirring in heating process obtains mixture；
(3) mixture filters while hot in the funnel for being lined with aseptic filter paper, and filtrate is cooled to room temperature spare；
(4) filtrate and deionized water are mixed to get mixed liquor by the ratio of 1:9 by volume, are then added in mixed liquor
HCl solution and NaOH solution adjust the pH of mixed liquor to 9；
(5) AgNO is added in step (4) described mixed liquor3Powder makes AgNO in mixed liquor3Concentration is 2mmol/L；
(6) above-mentioned mixed liquor is placed in reaction 15min in 60 DEG C of water-bath can be obtained nano silver.
Taking spore concentration is 106A/ml(blood cell plate counts) southern corn leaf blight bacteria suspension, it is flat to be spread evenly across PDA
On plate culture medium, taking diameter is that the aseptic filter paper piece of 5mm is placed on above-mentioned PDA plate culture medium, is added dropwise in above-described embodiment and makes
10 μ l of Nano silver solution, stand dark condition culture 2-3 days at 30 DEG C again after 10min, measuring its antibacterial circle diameter is
6.8±0.62mm。
Embodiment six:
(1) the sweet osmanthus blade of acquisition is cleaned with sterile water and is dried up in aseptic operating platform, remove petiole and main lobe
Arteries and veins is simultaneously cut into about 1cm2Fragment；
(2) it takes 20g fragment that 100ml deionized water is added in beaker to be uniformly mixed, be subsequently placed in 90 DEG C of water-bath
30min is heated, adjoint stirring in heating process obtains mixture；
(3) mixture filters while hot in the funnel for being lined with aseptic filter paper, and filtrate is cooled to room temperature spare；
(4) filtrate and deionized water are mixed to get mixed liquor by the ratio of 1:9 by volume, are then added in mixed liquor
HCl solution and NaOH solution adjust the pH of mixed liquor to 9；
(5) AgNO is added in step (4) described mixed liquor3Powder makes AgNO in mixed liquor3Concentration is 2mmol/L；
(6) above-mentioned mixed liquor is placed in reaction 15min in 80 DEG C of water-bath can be obtained nano silver.
Taking spore concentration is 106A/ml(blood cell plate counts) southern corn leaf blight bacteria suspension, it is flat to be spread evenly across PDA
On plate culture medium, taking diameter is that the aseptic filter paper piece of 5mm is placed on above-mentioned PDA plate culture medium, is added dropwise in above-described embodiment and makes
10 μ l of Nano silver solution, stand dark condition culture 2-3 days at 30 DEG C again after 10min, measuring its antibacterial circle diameter is
9.3±0.47mm。
Claims (2)
1. the method for preparing nano silver using sweet osmanthus blade, comprising the following steps:
(1) the sweet osmanthus blade of acquisition is cleaned with sterile water and is dried up in aseptic operating platform, remove petiole and main lobe arteries and veins simultaneously
It is cut into about 1cm2Fragment；
(2) it takes 1-20g fragment that 100ml deionized water is added in beaker to be uniformly mixed, is subsequently placed in 90 DEG C of water-bath and adds
Hot 30min obtains mixture with stirring in heating process；
(3) mixture filters while hot in the funnel for being lined with aseptic filter paper, and filtrate is cooled to room temperature spare；
(4) filtrate and deionized water are mixed to get mixed liquor by the ratio of 1:9 by volume, and HCl is then added in mixed liquor
Solution and NaOH solution, the pH for adjusting mixed liquor is 9；
(5) AgNO is added in step (4) described mixed liquor3Powder makes AgNO in mixed liquor3Concentration is 1-8mmol/L；
(6) above-mentioned mixed liquor is placed in reaction 15min in 60-80 DEG C of water-bath can be obtained nano silver.
2. a kind of method for preparing nano silver using sweet osmanthus blade according to claim 1, it is characterised in that: the step
Suddenly 5g fragment, AgNO in step (5) mixed liquor are used in (2)3Concentration is 1 mmol/L, and water bath temperature is 60 in step (6)
℃。
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| CN107282137A (en) * | 2016-04-12 | 2017-10-24 | 中国石油化工股份有限公司 | The method for preparing catalyst of vinyl acetate |
| CN108124903A (en) * | 2017-12-30 | 2018-06-08 | 安徽科技学院 | A kind of preparation method of the bactericidal nano-silver agent of inhibition southern corn leaf blight |
| CN109277582A (en) * | 2018-10-18 | 2019-01-29 | 楚雄师范学院 | A kind of production method of biological nano silver |
| CN111203544A (en) * | 2018-11-21 | 2020-05-29 | 南开大学 | Metal nano silver material and synthetic method and application thereof |
| CN110116219A (en) * | 2019-04-28 | 2019-08-13 | 尹跃超 | A kind of method that green quickly prepares gold-silver alloy nano particle |
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