CN115070057A - Green synthesis method for preparing nano-silver by using plant extract ferulic acid - Google Patents
Green synthesis method for preparing nano-silver by using plant extract ferulic acid Download PDFInfo
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 81
- KSEBMYQBYZTDHS-HWKANZROSA-N ferulic acid Chemical compound COC1=CC(\C=C\C(O)=O)=CC=C1O KSEBMYQBYZTDHS-HWKANZROSA-N 0.000 title claims abstract description 43
- KSEBMYQBYZTDHS-UHFFFAOYSA-N ferulic acid Natural products COC1=CC(C=CC(O)=O)=CC=C1O KSEBMYQBYZTDHS-UHFFFAOYSA-N 0.000 title claims abstract description 43
- KSEBMYQBYZTDHS-HWKANZROSA-M (E)-Ferulic acid Natural products COC1=CC(\C=C\C([O-])=O)=CC=C1O KSEBMYQBYZTDHS-HWKANZROSA-M 0.000 title claims abstract description 42
- 229940114124 ferulic acid Drugs 0.000 title claims abstract description 42
- 235000001785 ferulic acid Nutrition 0.000 title claims abstract description 42
- QURCVMIEKCOAJU-UHFFFAOYSA-N trans-isoferulic acid Natural products COC1=CC=C(C=CC(O)=O)C=C1O QURCVMIEKCOAJU-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000000419 plant extract Substances 0.000 title claims abstract description 14
- 238000001308 synthesis method Methods 0.000 title claims abstract description 14
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- 238000000034 method Methods 0.000 claims abstract description 33
- 239000002244 precipitate Substances 0.000 claims abstract description 30
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- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 4
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- FUSNOPLQVRUIIM-UHFFFAOYSA-N 4-amino-2-(4,4-dimethyl-2-oxoimidazolidin-1-yl)-n-[3-(trifluoromethyl)phenyl]pyrimidine-5-carboxamide Chemical compound O=C1NC(C)(C)CN1C(N=C1N)=NC=C1C(=O)NC1=CC=CC(C(F)(F)F)=C1 FUSNOPLQVRUIIM-UHFFFAOYSA-N 0.000 description 1
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- 241000411851 herbal medicine Species 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
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- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
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- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- 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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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The invention belongs to the technical field of nano material preparation, and discloses a green synthesis method for preparing nano silver by using plant extract ferulic acid. The method comprises the following operation steps: dissolving a mixture (mass ratio is 2: 1-20: 1) of silver oxide and ferulic acid in ultrapure water, reacting under the ultrasonic conditions of a certain random amplitude transformer, a certain ultrasonic crushing power ratio and a certain ultrasonic crushing time, precipitating unreacted substances through centrifugation after the reaction is finished, and collecting supernatant to obtain nano silver; dispersing the precipitate with fresh ultrapure water, then carrying out ultrasonic disruption, centrifuging to obtain a precipitate and a supernatant, repeating the dispersing, ultrasonic and centrifuging operations of the precipitate for three times, and combining all the supernatants. The method has the advantages of simple process conditions, simple equipment, simple and convenient operation and quick reaction, and the prepared nano silver particles have higher stability.
Description
Technical Field
The invention belongs to the technical field of nano material preparation, and particularly relates to a green synthesis method for preparing nano silver by using plant extract ferulic acid.
Background
In recent years, metal nanoparticles have attracted much attention because of their small size, large specific area, and unique optical, electronic, sensing, catalytic, and antibacterial properties. The properties of these nanomaterials depend on their size, shape, self-assembly. The silver nano has the characteristics of nano materials such as small-size effect, quantum size effect, interface effect and tunnel effect, and also has the characteristics of silver metal materials such as good oxidation resistance and antibacterial property, and is paid much attention due to the obvious advantages of the silver nano materials. Although the existing methods for synthesizing nano silver are numerous and the used raw materials are wide, the search for simpler synthesis conditions, shorter reaction time and more environment-friendly raw materials is still necessary. The synthesis method of the silver nano-particles is rich and can be divided into two basic comprehensive methods from bottom to top and from top to bottom. Top-down methods typically create nano-scale structures by cutting large pieces of material to reduce their size to a desired value, i.e., physical methods, and the energy required to reduce the particle size includes mechanical energy (ball milling), electrical energy (arc discharge), thermal energy (physical vapor deposition), optical energy (laser ablation). This method can produce nanoparticles of uniform particle size and high purity, but requires complicated equipment and external energy. In 2008, Tsuji et al laser-ablated a silver plate in a polyvinylpyrrolidone (PVP) aqueous solution and secondarily irradiated the colloid to prepare silver nanoparticles, but the preparation method uses a large amount of equipment and is expensive. The method only needs an ultrasonic crusher and a centrifugal machine, has low cost, and can explore the influence on the yield of the nano-silver from the aspects of required power, time and reactant concentrationThe operation is simple and controllable. The bottom-up method is the most studied and widely applied method, and mainly comprises the following steps: chemical (chemical reduction and photochemical) and biological. Chemical method is the most common method for synthesizing nano silver at present. This process involves Ag + Converting into Ag by electron transfer under certain conditions 0 . The chemical method has the advantages that a large amount of nano particles can be obtained in a short time, and the size distribution of the silver particles can be well controlled by controlling reaction conditions. However, most of chemical methods need hydrazine hydrate, sodium borohydride, ascorbic acid, hydrogen peroxide, sodium citrate and the like as reducing agents to promote the synthesis of nano silver, and most of solvents used in the chemical reduction process are toxic and volatile and have potential hazard to the environment and organisms. For example, in 2008 Wu et al synthesized highly concentrated and stable silver nanoparticle suspensions by chemical reduction of silver nitrate in formaldehyde reducing agent with the organic base triethylamine as a reaction promoter. However, the organic bases triethylamine and formaldehyde have pungent odor, formaldehyde is also listed as carcinogen, the used organic solvent is harmful to human beings, the invention does not need to use dangerous chemicals which have high danger to human bodies, and the used solvent is ultrapure water and can synthesize nano silver by a one-pot method. The nano silver generated by the reaction of the ferulic acid and the silver oxide has good stability, the synthetic route is simple, economic and efficient, the environment is protected, and the scale is easy to expand to realize high-yield production.
In recent years, natural biomass materials are paid attention to by researchers by virtue of the advantages of wide sources, low cost, renewability and the like, and the problem of biomass resource waste is effectively solved by functional development and high-added-value utilization of the natural biomass materials. Compared with the method for synthesizing nano silver in other documents, the method for synthesizing nano silver by ferulic acid (FA, 4-hydroxy-3-methoxycinnamic acid) has many advantages. In terms of reserves, ferulic acid is widely found in vegetables, fruits, some beverages (such as coffee, beer, etc.) and some Chinese herbal medicines, such as angelica, cimicifuga foetida, ligusticum wallichii. And the price is low, and the regeneration can be recycled in nature. It is a promising phytochemical substance, has strong antioxidant activity, rarely exists in free state in plant body, and mainly forms combined state with oligosaccharide, polyamine, lipid and polysaccharide. Structurally, ferulic acid contains a phenolic hydroxyl group and a methoxy group, so that the ferulic acid shows strong antioxidant activity and has the main effect of rapidly stopping a free radical chain reaction through a free radical scavenging mechanism by the phenolic hydroxyl group. Secondly, the chemical structure of ferulic acid has highly conjugated unsaturation, which can act as an effective uv absorber. The high ability of ferulic acid to absorb ultraviolet light may also contribute to its very potent antioxidant activity. Ferulic acid is a promising candidate material, and despite its great potential, the advantages of ferulic acid have not been fully exploited to date, thus making it of great interest to accelerate its research. In addition, the nano silver also has the problems of low yield, unsatisfied green and environment-friendly raw materials, high raw material price, complex operation steps, harsh conditions and the like. And most of solvents used for synthesizing the nano silver have the defects of harmfulness to the environment or human body, non-recyclability, unstable chemical property due to high oxidizability, volatility and the like.
In 2016, Pramujitha Mendis et al take sodium borohydride as a main reducing agent, trisodium citrate and hydrazine sulfate as a stabilizer and an auxiliary reducing agent respectively, synthesize spherical silver nanoparticles by using silver nitrate as a precursor, and develop seven kinds of nano-silver with different colors. In addition to this, for example, in 2018, Wongpreecha et al prepared large-scale AgNPs-chitosan by one-pot method, although the method reported in this document is the same as the present invention and is a green synthetic method, the reducing agent and stabilizer used in the document are chitosan, and the present invention uses ferulic acid. However, the apparatus used in this report is a high-pressure autoclave, and it is necessary to perform an experiment in which a chitosan stock solution and a silver nitrate solution are subjected to pressure application for 50 minutes at 105 ℃, 110 ℃, 115 ℃ and 120 ℃. Then, the experiment was carried out at room temperature, 60 ℃, 90 ℃ and 120 ℃ for 8 hours without applying pressure. The equipment used in the literature is dangerous, reaction stripThe parts are also high temperature and high pressure, the reaction time is very long, and the rapid production is not facilitated. The reaction equipment used in the invention is an ultrasonic crusher, and the preparation process conditions and equipment are simple, the reaction is rapid, and the nano silver can be successfully prepared within minutes. In 2021, Jharimune et al synthesized Ag nanocubes by the polyol method using hydrochloric acid as a catalyst, where solvent (ethylene glycol) was considered as the reducing agent, poly (N-vinyl pyrrolidone) (PVP) was the shape directing agent, and silver nitrate was the precursor. The method reported in the literature uses ethylene glycol as a toxic organic solvent, hydrochloric acid as a corrosive chemical with greater irritation to human skin, and it is further noted that NO gas is released during the synthesis of Ag nanoparticles by this method, and may be further converted into NO if exposed to air 2 A gas. Therefore, the reaction must be carried out in a fume hood with good working and ventilation, and protective clothing must be worn. In contrast, the reaction conditions used in the present invention are simple and do not generate NO or NO 2 And the used solvent is ultrapure water, is an excellent environment-friendly solvent and has no danger to human bodies.
Therefore, the problem to be researched and solved is to find a green synthesis method for preparing nano silver, which is simple to operate, environment-friendly in used raw materials and rapid in reaction.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention mainly aims to provide a green synthetic method for preparing nano-silver by using ferulic acid which is a plant extract; the method utilizes ferulic acid to stably synthesize nano-silver for the first time, does not need to add other stabilizers, can also achieve the effect of stably synthesizing nano-silver, and has the advantages of simple process conditions, simple equipment and simple and convenient operation; the method has the advantages that the used raw material ferulic acid is environment-friendly, wide in source and high in cost benefit, and is convenient for large-scale production; the method also uses ultrapure water as a solvent system, and the water is easy to obtain, has wide source and can be recycled.
Another object of the present invention is to provide nano silver synthesized by the above method, which has an average particle diameter of 35 to 80nm and excellent stability.
The purpose of the invention is realized by the following technical scheme:
a green synthesis method for preparing nano-silver by using plant extract ferulic acid comprises the following operation steps: dissolving a mixture of silver oxide and ferulic acid in ultrapure water, reacting under ultrasound, centrifuging and precipitating unreacted substances after the reaction is finished, and collecting supernatant to obtain nano-silver; dispersing the precipitate with fresh ultrapure water, then carrying out ultrasonic disruption, centrifuging to obtain a precipitate and a supernatant, repeating the dispersing, ultrasonic and centrifuging operations of the precipitate for three times, and combining all the supernatants.
Preferably, in the mixture of silver oxide and ferulic acid, the mass ratio of silver oxide to ferulic acid is 2: 1-20: 1.
Preferably, the conditions of the ultrasound are: the random amplitude transformer is a phi 2-15 rod, the power ratio is 10-90%, and the time is 5-20 min.
More preferably, the conditions of the ultrasound are: the random amplitude transformer is a phi 6 rod, the power ratio is 70%, and the time is 15 min.
Preferably, the centrifugation condition is 2000 g-5000 g, and the time of each centrifugation is 8-12 min.
More preferably, the centrifugation is performed at 2000g for 10min per centrifugation.
The nano silver synthesized by the method has the average particle size of 35-80 nm.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the solvent of the invention utilizes ultrapure water, and has the advantages of environmental protection, no toxicity, reutilization, wide source and low cost.
(2) The reaction raw material utilized by the invention is a plant extract, namely ferulic acid, which can be found in various natural plants, has low price, can be recycled in nature and has certain economic benefit; the precursor of the invention is Ag 2 O，Ag 2 O exhibits very low solubility in solvent ultrapure water, and thus unreacted Ag 2 O can be easily removed by centrifugation to facilitate repeated sonication.
(3) The method only uses ferulic acid, ultrapure water and silver oxide as raw materials, does not need to add any additional stabilizer or strong acid (HCL) or strong base (NaOH) to assist the synthesis compared with other existing methods, has the advantages of simple process conditions, simple equipment, simple and convenient operation and quick reaction, is high-valued utilization of plant extracts, has certain economic benefit, and conforms to the concepts of green chemistry and sustainable development.
(4) The nano silver particles prepared by the green synthesis method have higher stability, and the poly ferulic acid is coated on the surface of the nano silver so that the nano silver can stably exist at room temperature, thereby well researching the factors influencing the particle size of the nano silver and whether the nano silver can stably exist.
Drawings
Fig. 1 is a Transmission Electron Microscope (TEM) of nano silver prepared in example 1.
FIG. 2 is a graph showing UV-VIS absorption spectra of silver nanoparticles of examples 1 to 7.
FIG. 3 is a graph showing the effect of the number of days of standing on the maximum UV absorbance of the synthesized nanosilver in examples 1 to 7.
Detailed Description
The present invention will be further described with reference to the following examples and drawings, but the embodiments of the present invention are not limited thereto.
The reagents used in the examples are all conventionally available from the market. The ratios reported in the examples, including the figures, are mass ratios of silver oxide to ferulic acid. For example, the ratio of "10: 5" in FIG. 2 of the present invention is 10mg of the silver oxide and 5mg of ferulic acid.
Example 1: weighing 10mg of ferulic acid and 5mg of silver oxide in absolute dry weight, placing the ferulic acid and the 5mg of silver oxide in a 20mL sample bottle, adding 10mL of ultrapure water, carrying out ultrasonic treatment for 15min under the conditions of a No. 6 rod and an ultrasonic power ratio of 70%, precipitating unreacted substances by centrifugation (2000g, 10min), and collecting supernate which is nano-silver; dispersing the precipitate with fresh ultrapure water, ultrasonic crushing for 15min under the conditions of a phi 6 rod and an ultrasonic power ratio of 70%, centrifuging to obtain precipitate and supernatant, repeating the dispersing, ultrasonic and centrifuging operations of the precipitate for three times, and combining all supernatants. The supernatant was analyzed by a nanometer particle size and zeta potential analyzer to determine an average particle size of 46.3nm and a zeta potential of-34.57 mV. As shown in fig. 1, a Transmission Electron Microscope (TEM) of the nano silver prepared in this example shows that the nano silver is in the form of spherical particles, and the nano particles are not aggregated, indicating that the stability of the particles is good. The ultraviolet-visible light absorption spectrum of fig. 2 shows that the characteristic absorption peak of nano-silver is 431 nm. Fig. 3 shows that the characteristic absorption peak value of the nano-silver is increased to a certain value and is almost kept unchanged after the nano-silver is stood for 7 days, which indicates that the nano-silver has excellent stability.
Example 2: weighing ferulic acid with absolute dry weight of 20mg and silver oxide with absolute dry weight of 10mg, placing in a 20mL sample bottle, adding ultrapure water with 10mL, performing ultrasonic treatment for 15min under the condition of a No. 6 rod and an ultrasonic power ratio of 70%, precipitating unreacted substances through centrifugation (2000g, 10min), and collecting supernate which is nano-silver; dispersing the precipitate with fresh ultrapure water, ultrasonic crushing for 15min under the conditions of a phi 6 rod and an ultrasonic power ratio of 70%, centrifuging to obtain precipitate and supernatant, repeating the dispersing, ultrasonic and centrifuging operations of the precipitate for three times, and combining all supernatants. The supernatant was measured to have an average particle size of 51.2nm and a zeta potential of-34.77 mV using a nanometer particle size and zeta potential analyzer. The UV-visible absorption spectrum of FIG. 2 shows that the characteristic absorption peak of nano-silver is 438 nm. Fig. 3 shows that the characteristic absorption peak value of the nano-silver is increased to a certain value and is almost kept unchanged after the nano-silver is stood for 7 days, which indicates that the nano-silver has excellent stability.
Example 3: weighing ferulic acid with absolute dry weight of 50mg and silver oxide with absolute dry weight of 25mg, placing in a 20mL sample bottle, adding 10mL ultrapure water, performing ultrasonic treatment for 15min under the conditions of a No. 6 rod and an ultrasonic power ratio of 70%, precipitating unreacted substances through centrifugation (2000g, 10min), and collecting supernate as nano-silver; dispersing the precipitate with fresh ultrapure water, ultrasonic crushing for 15min under the conditions of a phi 6 rod and an ultrasonic power ratio of 70%, centrifuging to obtain precipitate and supernatant, repeating the dispersing, ultrasonic and centrifuging operations of the precipitate for three times, and combining all supernatants. The supernatant was measured to have an average particle size of 77.1nm and a zeta potential of-25.03 mV using a nanometer particle size and zeta potential analyzer. The ultraviolet-visible light absorption spectrum of fig. 2 shows that the characteristic absorption peak of nano-silver is 444 nm. Fig. 3 shows that the absorption peak value of the nano-silver is almost unchanged after the nano-silver is stood for 7 days to a certain extent, which indicates that the nano-silver has excellent stability.
Example 4: weighing 10mg of ferulic acid and 2.5mg of silver oxide in absolute dry weight, placing the ferulic acid and the silver oxide in a 20mL sample bottle, adding 10mL of ultrapure water, carrying out ultrasonic treatment for 15min under the conditions of a No. 6 rod and an ultrasonic power ratio of 70%, precipitating unreacted substances by centrifugation (2000g, 10min), and collecting supernate which is nano-silver; dispersing the precipitate with fresh ultrapure water, ultrasonic crushing for 15min under the conditions of a phi 6 rod and an ultrasonic power ratio of 70%, centrifuging to obtain precipitate and supernatant, repeating the dispersing, ultrasonic and centrifuging operations of the precipitate for three times, and combining all supernatants. The supernatant was measured to have an average particle size of 43.8nm and a zeta potential of-36.60 mV using a nanometer particle size and zeta potential analyzer. The UV-visible absorption spectrum of FIG. 2 shows that the characteristic absorption peak of nano-silver is 428 nm. Fig. 3 shows that the characteristic absorption peak of the nano-silver after standing for 7 days is almost kept unchanged, indicating that the nano-silver has excellent stability.
Example 5: weighing 5mg of ferulic acid and 1mg of silver oxide in absolute dry weight, placing the ferulic acid and the silver oxide in a 20mL sample bottle, adding 10mL of ultrapure water, carrying out ultrasonic treatment for 15min under the conditions of a No. 6 rod and an ultrasonic power ratio of 70%, precipitating unreacted substances by centrifugation (2000g, 10min), and collecting supernate which is nano-silver; dispersing the precipitate with fresh ultrapure water, ultrasonic crushing for 15min under the conditions of a phi 6 rod and an ultrasonic power ratio of 70%, centrifuging to obtain precipitate and supernatant, repeating the dispersing, ultrasonic and centrifuging operations of the precipitate for three times, and combining all supernatants. The supernatant was measured to have an average particle size of 35.4nm and a zeta potential of-40.33 mV using a nanometer particle size and zeta potential analyzer. The UV-visible absorption spectrum of FIG. 2 shows that the characteristic absorption peak of nano-silver is 419 nm. Fig. 3 shows that the characteristic absorption peak of the nano-silver after standing for 7 days is almost kept unchanged, indicating that the nano-silver has excellent stability.
Example 6: weighing 10mg of ferulic acid and 1mg of silver oxide in absolute dry weight, placing the ferulic acid and the silver oxide in a 20mL sample bottle, adding 10mL of ultrapure water, carrying out ultrasonic treatment for 15min under the conditions of a No. 6 rod and an ultrasonic power ratio of 70%, precipitating unreacted substances by centrifugation (2000g, 10min), and collecting supernate which is nano-silver; dispersing the precipitate with fresh ultrapure water, ultrasonic crushing for 15min under the conditions of a phi 6 rod and an ultrasonic power ratio of 70%, centrifuging to obtain precipitate and supernatant, repeating the dispersing, ultrasonic and centrifuging operations of the precipitate for three times, and combining all supernatants. The supernatant was measured to have an average particle size of 35.8nm and a zeta potential of-40.6 mV using a nanometer particle size and zeta potential analyzer. The UV-visible absorption spectrum of FIG. 2 shows that the characteristic absorption peak of nano-silver is 410 nm. Fig. 3 shows that the characteristic absorption peak of the nano-silver remained almost unchanged after standing for 7 days, indicating that the nano-silver has excellent stability.
Example 7: weighing ferulic acid with absolute dry weight of 20mg and silver oxide with absolute dry weight of 1mg, placing in a 20mL sample bottle, adding ultrapure water with 10mL, performing ultrasonic treatment for 15min under the condition of a No. 6 rod and an ultrasonic power ratio of 70%, precipitating unreacted substances through centrifugation (2000g, 10min), and collecting supernate which is nano-silver; dispersing the precipitate with fresh ultrapure water, ultrasonic crushing for 15min under the conditions of a phi 6 rod and an ultrasonic power ratio of 70%, centrifuging to obtain precipitate and supernatant, repeating the dispersing, ultrasonic and centrifuging operations of the precipitate for three times, and combining all supernatants. The supernatant was measured to have an average particle diameter of 37.4nm and a zeta potential of-42 mV using a nanometer particle size and zeta potential analyzer. The UV-visible absorption spectrum of FIG. 2 shows that the characteristic absorption peak of nano-silver is 412 nm. Fig. 3 shows that the characteristic absorption peak of the nano-silver after standing for 7 days is almost kept unchanged, indicating that the nano-silver has excellent stability.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (7)
1. A green synthesis method for preparing nano-silver by using plant extract ferulic acid is characterized by comprising the following operation steps: dissolving a mixture of silver oxide and ferulic acid in ultrapure water, reacting under ultrasound, centrifuging and precipitating unreacted substances after the reaction is finished, and collecting supernatant to obtain nano-silver; dispersing the precipitate with fresh ultrapure water, then carrying out ultrasonic disruption, centrifuging to obtain a precipitate and a supernatant, repeating the dispersing, ultrasonic and centrifuging operations of the precipitate for three times, and combining all the supernatants.
2. The green synthesis method for preparing nano silver by using plant extracts as claimed in claim 1, wherein: in the mixture of the silver oxide and the ferulic acid, the mass ratio of the silver oxide to the ferulic acid is 2: 1-20: 1.
3. The green synthesis method for preparing nano silver by using plant extracts as claimed in claim 1, wherein: the ultrasonic conditions are as follows: the random amplitude transformer is a phi 2-15 rod, the power ratio is 10-90%, and the time is 5-20 min.
4. The green synthesis method for preparing nano silver by using plant extracts as claimed in claim 1, wherein: the ultrasonic conditions are as follows: the random amplitude transformer is a phi 6 pole, the power ratio is 70%, and the time is 15 min.
5. The green synthesis method for preparing nano silver by using plant extracts as claimed in claim 1, wherein: the centrifugation condition is 2000 g-5000 g, and the time of each centrifugation is 8-12 min.
6. The green synthesis method for preparing nano silver by using plant extracts as claimed in claim 1, wherein: the centrifugation condition is 2000g, and the time of each centrifugation is 10 min.
7. Nano-silver synthesized according to the method of claim 1, characterized in that: the average grain diameter of the nano silver is 35-80 nm.
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| JP2011032509A (en) * | 2009-07-30 | 2011-02-17 | Dowa Electronics Materials Co Ltd | Metal nanoparticle-dispersed solution |
| CN102202815A (en) * | 2008-05-16 | 2011-09-28 | 维鲁泰克技术股份有限公司 | Green synthesis of nanometals using plant extracts and use thereof |
| CN105396149A (en) * | 2015-07-07 | 2016-03-16 | 宋玉军 | Nanometer alloy anti-cancer drug with functions of independent targeting and imaging, and preparation method thereof |
| US20210070629A1 (en) * | 2019-09-05 | 2021-03-11 | Imam Abdulrahman Bin Faisal University | Green synthesis of noble metal/transition metal oxide nanocomposite |
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| CN102202815A (en) * | 2008-05-16 | 2011-09-28 | 维鲁泰克技术股份有限公司 | Green synthesis of nanometals using plant extracts and use thereof |
| JP2011032509A (en) * | 2009-07-30 | 2011-02-17 | Dowa Electronics Materials Co Ltd | Metal nanoparticle-dispersed solution |
| CN105396149A (en) * | 2015-07-07 | 2016-03-16 | 宋玉军 | Nanometer alloy anti-cancer drug with functions of independent targeting and imaging, and preparation method thereof |
| US20210070629A1 (en) * | 2019-09-05 | 2021-03-11 | Imam Abdulrahman Bin Faisal University | Green synthesis of noble metal/transition metal oxide nanocomposite |
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