CN105127442A - Method for synthesizing nano-silver colloid with green coffee bean extract as reducing agent - Google Patents
Method for synthesizing nano-silver colloid with green coffee bean extract as reducing agent Download PDFInfo
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Abstract
The invention relates to a method for synthesizing nano-silver colloid with a green coffee bean extract as a reducing agent. The method comprises the following steps that an oxidizing agent for a reaction is prepared; silver salt is dissolved in deionized water and stirred till the silver salt is completely dissolved, and the prepared oxidizing agent is used in a standby manner; the reducing agent for the reaction is prepared; a plant extract is dissolved in deionized water and stirred till the plant extract is completely dissolved, and the prepared reducing agent is used in a standby manner; the nano silver colloid with the small particle size is synthesized; and the prepared reducing agent is dripped in the oxidizing agent, dripping and stirring are carried out at the same time, stirring is continuously carried out for ten minutes after dripping is finished, and the complete reaction can be ensured. The method for synthesizing the nano-silver colloid with the green coffee bean extract as the reducing agent is low in cost, easy to operate and environment-friendly. Compared with nano-silver prepared through a traditional method, the prepared nano-silver is smaller in size and better in antibacterial effect.
Description
Technical field
The present invention relates to and a kind ofly utilize green coffee bean extract as the method for reducing agent synthesis of nano elargol, belong to the preparing technical field of nano-silver colloid.
Background technology
Anti-biotic material refers within a certain period of time, has the powerful class new function material killed or suppress microorganism (bacterium, fungi, saccharomycete, algae and virus etc.) function.Anti-biotic material has now been widely used among daily life and industrial and agricultural development.Particularly in recent years, environment extreme degradation, people are also increasing to the demand of powerful anti-biotic material.Current anti-biotic material to be referred to by adding certain antibacterial material, i.e. antiseptic, thus makes material have suppression or kill the ability being attached to himself surface or adjacent microorganism.Antiseptic is roughly divided into three classes: inorganic, organic and natural antibacterial agent.Along with the reinforcement of people's environmental consciousness, the use of natural antibacterial agent becomes first-selected.At the extract of some animals and plants of occurring in nature, mineral substance, himself just have good suppression or the ability of killing microorganisms, these materials are referred to as natural antibacterial material.
Nano Silver (NanoSilver) refers to the elemental silver particle of particle diameter between 1-100nm (SilverNanoparticles, AgNPs writes a Chinese character in simplified form in educational circles) prepared by certain chemistry route or physical means.Nano Silver all has broad application prospects in electronic material, catalysis material, optical material, medical material and heat exchange material etc., has become one of 21 century the most promising material.It is a kind of good natural antibacterial agent.Because it has skin effect, small-size effect and macro quanta tunnel effect, Nano Silver has strong suppression and killing action to tens of kinds of pathogenic microorganisms such as Escherichia coli, gonococcus, chlamydia trachomatises, and can not produce drug resistance.Nano Silver is incorporated among other material, a greater variety of carrying nano silver composite antibacterial material can be prepared.Nano Silver has that broad-spectrum antiseptic, strong bactericidal, permeability are strong, reparative regeneration, antibacterial lasting, the feature such as have no drug resistance, therefore silver ion antiseptic is of greatest concern in metal ion antibacterial agent research.Patent CN102218541A describes a kind of novel large-scale producing method of water-soluble nano silver.This preparation method be first just silver salt and protective agent, stabilizing agent at 30-70 DEG C stirring and dissolving in aqueous solvent; regulate pH value; when solution system clear is after 5-20 minute; add in reaction system by reducing agent again, the 5-30 minute of Keep agitation reaction afterwards, obtains the Nano Silver that size is less than 20nm; but its preparation process is loaded down with trivial details; reaction required time is longer, and if the protective agent used in preparation process, stabilizing agent except clean, the subsequent applications of Nano Silver may be had influence on.
Summary of the invention
The present invention is intended to invent the method that the green reducing process of a kind of use prepares the less Nano Silver of size; preparation time is short; this method overcomes protective agent, the sordid problem of stabilizer treatment used in Nano Silver preparation process in prior art, and obtained Nano Silver has better antibacterial effect.
Technical scheme provided by the invention is:
Utilize green coffee bean extract as a method for reducing agent synthesis of nano elargol, comprise the following steps:
1) oxidant in preparation feedback: be dissolved in by silver salt in deionized water, is stirred to it and dissolves completely, and obtained oxidant is for subsequent use;
2) reducing agent in preparation feedback: be dissolved in by plant extracts in deionized water, is stirred to it and dissolves completely, and obtained reducing agent is for subsequent use;
3) synthesize small particle diameter nano-silver colloid: drip in oxidant by obtained reducing agent, drip while stir, drip off continuation stirring and react completely with guarantee for ten minutes.
Step 1) in, described silver salt is soluble silver salt.
Step 1) in, described silver salt is nitrate.
Step 2) in, described plant extracts is water soluble plant extract.
Step 2) in, described plant extracts is green coffee bean water-soluble extractive.
Step 3) in reaction carry out at normal temperatures.
Step 3) in reaction carry out under continuous stirring, ensure reactant reaction complete.
Step 1) in silver salt concentrations between 0.2mM ~ 1mM; For subsequent use by masking foil parcel lucifuge after preparing oxidant.
Described step 1) and step 2) in, the usage ratio of silver nitrate and green coffee bean extract is, green coffee bean extract is excessive slightly after making silver nitrate complete reaction is advisable.
Step 3) in, a speed of being dripped by obtained reducing agent when oxidant is 1 drop/sec.
Beneficial effect:
The green coffee beans plant extracts of the present invention prepares Nano Silver as reducing agent, cost is low, simple to operate, green friendly to environment, and obtained Nano Silver has less size compared with Nano Silver obtained under conventional method, antibacterial effect is better, is more suitable for using as antiseptic.The present invention is that the silver nitrate that reduces in aqueous phase obtains the nano-silver colloid of variable concentrations with pure green plants extract for reducing agent.Synthetic method of the present invention has raw material sources cheapness, and laboratory facilities are simple and easy to the advantages such as realization, and the stability of the elargol sample simultaneously synthesized is also fine, Absorbable organic halogens two months under normal temperature lucifuge.
Accompanying drawing explanation
Fig. 1: embodiment 1 low power transmission electron microscope picture result.
Fig. 2: embodiment 2 low power transmission electron microscope picture result.
Fig. 3: embodiment 3 low power transmission electron microscope picture result.
Fig. 4: embodiment 1 high power transmission electron microscope picture.
Fig. 5: embodiment 1-3 UV, visible light extinction spectrum instrument figure result.
Fig. 6: the Oxford cup lab diagram of bacterium in water under different Nano Silver sample treatment.
Fig. 7: the Oxford cup lab diagram in agar plate medium.
Fig. 8: colibacillary growing way figure under variable concentrations Nano Silver sample treatment.
Fig. 9: the growing way figure of gold-coloured staphylococci under variable concentrations Nano Silver sample treatment.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described.
Case study on implementation 1
The silver nitrate taking 0.1275g is put in beaker, dissolves completely by the deionized water of 15ml.The solution masking foil prepared wraps up, and lucifuge is for subsequent use.
The green coffee bean extract taking 0.4030g is dissolved in 20ml deionized water as reducing agent.Abundant stirring is to ensure to dissolve completely.
Be added drop-wise in liquor argenti nitratis ophthalmicus by green coffee bean extract, reaction is carried out at normal temperatures, drips speed and remains on 1 drop/sec.Drip off rear continuation stirring 10 minutes to ensure that silver nitrate reacts completely.Obtain nano-silver colloid.
Scanned under low, high power transmission electron microscope by obtained nano-silver colloid Ag1, Fig. 1 is low power transmission electron microscope picture result, and Fig. 4 is high power transmission electron microscope picture.
Synthesize the nano-silver colloid Ag1 UV, visible light extinction spectrum instrument scanning obtained, Fig. 5 is UV, visible light extinction spectrum instrument figure result.
The antibacterial effect of the elargol sample of synthesis is by characterizing the inhibitory action of Escherichia coli and staphylococcus aureus growth.Result is shown in figs. 6-9.Fig. 6,7 is the Oxford cup lab diagram of bacterium in water and agar plate medium under different Nano Silver sample treatment.Fig. 8 is that under variable concentrations Nano Silver sample treatment, colibacillary growing way figure, Fig. 9 are the growing way figure of gold-coloured staphylococci under variable concentrations Nano Silver sample treatment.
Case study on implementation 2
The silver nitrate taking 0.2550g is put in beaker, dissolves completely by the deionized water of 15ml.The solution masking foil prepared wraps up, and lucifuge is for subsequent use.
The green coffee bean extract taking 0.8060g is dissolved in 20ml deionized water as reducing agent.Abundant stirring is to ensure to dissolve completely.
Be added drop-wise in liquor argenti nitratis ophthalmicus by green coffee bean extract, reaction is carried out at normal temperatures, drips speed and remains on 1 drop/sec.Drip off rear continuation stirring 10 minutes to ensure that silver nitrate reacts completely.Obtain nano-silver colloid.
Scanned under low power transmission electron microscope by obtained nano-silver colloid Ag2, Fig. 2 is exactly transmission electron microscope picture result.
Synthesize the nano-silver colloid Ag2 UV, visible light extinction spectrum instrument scanning obtained, Fig. 5 is UV, visible light extinction spectrum instrument figure result.
Case study on implementation 3
The silver nitrate taking 0.5100g is put in beaker, dissolves completely by the deionized water of 15ml.The solution masking foil prepared wraps up, and lucifuge is for subsequent use.
The green coffee bean extract taking 1.6120g is dissolved in 20ml deionized water as reducing agent.Abundant stirring is to ensure to dissolve completely.
Be added drop-wise in liquor argenti nitratis ophthalmicus by green coffee bean extract, reaction is carried out at normal temperatures, drips speed and remains on 1 drop/sec.Drip off rear continuation stirring 10 minutes to ensure that silver nitrate reacts completely.Obtain nano-silver colloid.
Scanned under low power transmission electron microscope by obtained nano-silver colloid Ag3, Fig. 3 is exactly transmission electron microscope picture result.
Synthesize the nano-silver colloid Ag3 UV, visible light extinction spectrum instrument scanning obtained, Fig. 5 is UV, visible light extinction spectrum instrument figure result.
As shown in Figures 1 to 3, the low power transmission electron microscope picture of the silver sol sample synthesized from three kinds of concentration can be found out, along with the rising of reactant concentration, the Argent grain of generation becomes large, and dispersed variation.
Fig. 4 is the crystal lattice pattern of Ag1 under high power transmission electron microscope.Can find out the lattice of Nano Silver clearly from figure, and spacing of lattice size is at about 0.230nm, corresponds to 111 crystal faces of silver.
Fig. 5 is the collection of illustrative plates that the nano silver colloidal sol of variable concentrations scans gained under ultraviolet-visual spectrometer.From figure, there is a peak at about 430nm in the uv-vis spectra of nano-silver colloid, this peak is the characteristic peak of nano-noble metal.The position at the peak of sample Ag1 the peak of 425nm, Ag2 position comparatively Ag1 there occurs obvious red shift, and the position at the peak of Ag3 comparatively Ag2 also there occurs obvious red shift.This is that the particle of the Nano Silver of generation also becomes large, and the peak position of ultraviolet-visible spectrogram there occurs red shift thereupon owing to raising along with reactant concentration.This is consistent with transmission electron microscope picture result in Fig. 1.
Fig. 6,7 shows the test result of Oxford cup experiment.We find, the antibacterial activity on agar plate is compared with not too obvious in water.When flat board adds the nano silver colloidal sol sample of 1 μm of ol/L, almost there is no inhibition zone.In addition, when dropping 5 μm of ol/L and 2 μm of ol/L nano silver colloidal sol samples, inhibition zone does not have obvious difference yet.This means the species influence of penetrating power by gel media of the Nano Silver that we prepare.
Fig. 8, Fig. 9 are the growing state figure of Escherichia coli and staphylococcus aureus under the silver sol sample effect of variable concentrations.As we know from the figure, along with the reduction of silver sol sample concentration, the inhibitory action of Escherichia coli and staphylococcus aureus is also diminished.Roughly can determine that the minimum inhibitory concentration of nano silver colloidal sol to Escherichia coli and staphylococcus aureus that we synthesize is respectively 0.04 μm of ol/L, 0.1 μm of ol/L.We have good bacteriostasis to Escherichia coli and staphylococcus aureus by the nano silver colloidal sol of synthesis.
This patent reactant used is cheap and easy to get, and the reaction time is short, and without the need to adding any protective agent in course of reaction, and the Nano Silver of synthesis has less size, has good inhibitory action to Escherichia coli and staphylococcus aureus.
The above; it is only preferred embodiment of the present invention; not any pro forma restriction is done to the present invention; any those skilled in the art; do not departing within the scope of technical solution of the present invention; according to technical spirit of the present invention, any simple amendment that above embodiment is done, equivalently replace and improve, within the protection domain all still belonging to technical solution of the present invention.
Claims (10)
1. utilize green coffee bean extract as a method for reducing agent synthesis of nano elargol, it is characterized in that: comprise the following steps:
1) oxidant in preparation feedback: be dissolved in by silver salt in deionized water, is stirred to it and dissolves completely, and obtained oxidant is for subsequent use;
2) reducing agent in preparation feedback: be dissolved in by plant extracts in deionized water, is stirred to it and dissolves completely, and obtained reducing agent is for subsequent use;
3) synthesize small particle diameter nano-silver colloid: drip in oxidant by obtained reducing agent, drip while stir, drip off continuation stirring and react completely with guarantee for ten minutes.
2. utilize green coffee bean extract as the method for reducing agent synthesis of nano elargol as claimed in claim 1, it is characterized in that: step 1) in, described silver salt is soluble silver salt.
3. utilize green coffee bean extract as the method for reducing agent synthesis of nano elargol as claimed in claim 1, it is characterized in that: step 1) in, described silver salt is nitrate.
4. utilize green coffee bean extract as the method for reducing agent synthesis of nano elargol as claimed in claim 1, it is characterized in that: step 2) in, described plant extracts is water soluble plant extract.
5. utilize green coffee bean extract as the method for reducing agent synthesis of nano elargol as claimed in claim 1, it is characterized in that: step 2) in, described plant extracts is green coffee bean water-soluble extractive.
6. utilize green coffee bean extract as the method for reducing agent synthesis of nano elargol as claimed in claim 1, it is characterized in that: step 3) in reaction carry out at normal temperatures.
7. utilize green coffee bean extract as the method for reducing agent synthesis of nano elargol as claimed in claim 1, it is characterized in that: step 3) in reaction carry out under continuous stirring, ensure reactant reaction complete.
8. utilize green coffee bean extract as the method for reducing agent synthesis of nano elargol as claimed in claim 1, it is characterized in that: step 1) in silver salt concentrations between 0.2mM ~ 1mM; For subsequent use by masking foil parcel lucifuge after preparing oxidant.
9. utilize green coffee bean extract as the method for reducing agent synthesis of nano elargol as claimed in claim 1, it is characterized in that: described step 1) and step 2) in, the usage ratio of silver nitrate and green coffee bean extract is, green coffee bean extract is excessive slightly after making silver nitrate complete reaction is advisable.
10. utilize green coffee bean extract as the method for reducing agent synthesis of nano elargol as claimed in claim 1, it is characterized in that: step 3) in, a speed of being dripped by obtained reducing agent when oxidant is 1 drop/sec.
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CN105755050A (en) * | 2016-05-06 | 2016-07-13 | 华中农业大学 | Method for biologically synthesizing nano silver through fatsia japonica leaf extract |
CN106607594A (en) * | 2016-11-30 | 2017-05-03 | 重庆文理学院 | Rapid low-cost preparation method of gold nanoparticles |
CN107309438A (en) * | 2017-07-14 | 2017-11-03 | 福建农林大学 | A kind of method that polysaccharide from Phyllanthus Emblica L prepares Nano Silver compound particle |
CN107876798A (en) * | 2017-12-12 | 2018-04-06 | 上海理工大学 | A kind of method that gold nano grain is prepared using Sargent gloryvine extract solution |
CN113070484A (en) * | 2021-03-10 | 2021-07-06 | 海南华创槟榔研究院 | Size-controllable spherical nano silver particles, preparation method and application |
US11186493B2 (en) | 2019-09-05 | 2021-11-30 | Imam Abdulrahman Bin Faisal University | Green synthesis of noble metal/transition metal oxide nanocomposite |
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CN102343440A (en) * | 2010-07-29 | 2012-02-08 | 同济大学 | Method for preparing water-soluble nano silver by using actinidia as template |
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Cited By (10)
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CN105755050A (en) * | 2016-05-06 | 2016-07-13 | 华中农业大学 | Method for biologically synthesizing nano silver through fatsia japonica leaf extract |
CN105755050B (en) * | 2016-05-06 | 2021-09-03 | 华中农业大学 | Method for biologically synthesizing nano silver by using illicium verum leaf extract |
CN106607594A (en) * | 2016-11-30 | 2017-05-03 | 重庆文理学院 | Rapid low-cost preparation method of gold nanoparticles |
CN106607594B (en) * | 2016-11-30 | 2018-07-10 | 重庆文理学院 | A kind of quick, low cost gold nanoparticle preparation method |
CN107309438A (en) * | 2017-07-14 | 2017-11-03 | 福建农林大学 | A kind of method that polysaccharide from Phyllanthus Emblica L prepares Nano Silver compound particle |
CN107876798A (en) * | 2017-12-12 | 2018-04-06 | 上海理工大学 | A kind of method that gold nano grain is prepared using Sargent gloryvine extract solution |
US11186493B2 (en) | 2019-09-05 | 2021-11-30 | Imam Abdulrahman Bin Faisal University | Green synthesis of noble metal/transition metal oxide nanocomposite |
US11661349B2 (en) | 2019-09-05 | 2023-05-30 | Imam Abdulrahman Bin Faisal University | Method for making coffee husk reducing agent |
CN113070484A (en) * | 2021-03-10 | 2021-07-06 | 海南华创槟榔研究院 | Size-controllable spherical nano silver particles, preparation method and application |
CN114469530A (en) * | 2022-03-10 | 2022-05-13 | 嫒赟(上海)生物科技股份有限公司 | Nano silver antibacterial sanitary towel |
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