CN115070057B - 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 80
- 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 42
- KSEBMYQBYZTDHS-UHFFFAOYSA-N ferulic acid Natural products COC1=CC(C=CC(O)=O)=CC=C1O KSEBMYQBYZTDHS-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229940114124 ferulic acid Drugs 0.000 title claims abstract description 42
- 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 41
- 235000001785 ferulic acid Nutrition 0.000 title claims abstract description 41
- 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 41
- 238000001308 synthesis method Methods 0.000 title claims abstract description 13
- 239000000419 plant extract Substances 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 43
- 239000002244 precipitate Substances 0.000 claims abstract description 37
- 239000006228 supernatant Substances 0.000 claims abstract description 37
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 27
- 239000012498 ultrapure water Substances 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 239000000126 substance Substances 0.000 claims abstract description 19
- 229910001923 silver oxide Inorganic materials 0.000 claims abstract description 18
- 239000006185 dispersion Substances 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 238000005119 centrifugation Methods 0.000 claims description 16
- 238000002604 ultrasonography Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 abstract description 18
- 230000008901 benefit Effects 0.000 abstract description 12
- 238000009210 therapy by ultrasound Methods 0.000 abstract description 9
- 239000002086 nanomaterial Substances 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 description 14
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 12
- 239000002105 nanoparticle Substances 0.000 description 11
- 239000003638 chemical reducing agent Substances 0.000 description 10
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 9
- 239000002904 solvent Substances 0.000 description 9
- 238000000862 absorption spectrum Methods 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- 230000031700 light absorption Effects 0.000 description 7
- 230000001376 precipitating effect Effects 0.000 description 7
- 229910052709 silver Inorganic materials 0.000 description 7
- 230000002194 synthesizing effect Effects 0.000 description 7
- 238000005303 weighing Methods 0.000 description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000004332 silver Substances 0.000 description 6
- 229910001961 silver nitrate Inorganic materials 0.000 description 6
- 241000282414 Homo sapiens Species 0.000 description 5
- 239000003381 stabilizer Substances 0.000 description 5
- 241000196324 Embryophyta Species 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 239000002028 Biomass Substances 0.000 description 3
- 229920001661 Chitosan Polymers 0.000 description 3
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000003078 antioxidant effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229920000191 poly(N-vinyl pyrrolidone) Polymers 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 238000006722 reduction reaction Methods 0.000 description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005580 one pot reaction Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 150000007530 organic bases Chemical class 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000012279 sodium borohydride Substances 0.000 description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 description 2
- 239000001509 sodium citrate Substances 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- 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
- 241000906579 Actaea cimicifuga Species 0.000 description 1
- 241000382455 Angelica sinensis Species 0.000 description 1
- 241000112528 Ligusticum striatum Species 0.000 description 1
- 241000819554 Mendis Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000001241 arc-discharge method Methods 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 235000013405 beer Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000007760 free radical scavenging Effects 0.000 description 1
- 239000003517 fume Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 235000008216 herbs Nutrition 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 239000012493 hydrazine sulfate Substances 0.000 description 1
- 229910000377 hydrazine sulfate Inorganic materials 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 229920001542 oligosaccharide Polymers 0.000 description 1
- 150000002482 oligosaccharides Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 235000017807 phytochemicals Nutrition 0.000 description 1
- 229930000223 plant secondary metabolite Natural products 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 238000004917 polyol method Methods 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 150000003254 radicals Chemical group 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 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
- 239000000243 solution Substances 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 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
- 229940038773 trisodium citrate Drugs 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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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
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
-
- 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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- 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
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- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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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 of silver oxide and ferulic acid (the mass ratio is 2:1-20:1) 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, centrifuging to precipitate unreacted substances after the reaction is finished, and collecting supernatant to obtain nano silver; dispersing the precipitate with fresh ultrapure water, ultrasonic crushing, centrifuging to obtain precipitate and supernatant, repeating the dispersion, ultrasonic treatment and centrifuging operations of the precipitate 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 ferulic acid extracted from plants.
Background
In recent years, metal nano particles have great attention because of small volume, large specific area and unique optical, electronic, sensing, catalytic, antibacterial and other properties. The nature of these nanomaterials depends on their size, shape, self-assembly. Silver nano has the characteristics of nano materials such as small-size effect, quantum size effect, interface effect and tunnel effect, and has the characteristics of silver metal materials such as good oxidation resistance and antibacterial property, and the silver nano materials are paid attention to due to obvious advantages. Although the current methods for synthesizing nano silver are numerous and the used raw materials are wide, it is still necessary to find the raw materials with simpler synthesis conditions, shorter reaction time and more environment protection. The synthesis method of silver nanometer is rich, and can be divided into two basic comprehensive methods from bottom to top and from top to bottom. The top-down method generally creates a nano-scale structure by cutting a bulk material to reduce its size to a desired value, i.e., a physical method, and the energy required for reducing the particle size includes mechanical energy (ball milling method), electric energy (arc discharge method), thermal energy (physical vapor deposition method), optical energy (laser ablation method). This method can produce nanoparticles having a uniform particle size and high purity, but requires complicated equipment and external energy. In 2008, tsuji et al laser ablate silver plates in polyvinylpyrrolidone (PVP) aqueous solution and secondarily laser irradiate the resulting colloid to prepare silver nanoparticles, but the preparation method uses more equipment and is expensive. The invention only needs an ultrasonic crusher and a centrifugal machine, has lower cost, can explore the influence on the nano silver yield in terms of required power, time and reactant concentration, and has simpler and controllable method operation. The bottom-up method is the most studied and widely applied method and mainly comprises the following steps: chemical methods (chemical reduction and photochemical methods) and biological methods. Chemical methods are currently the most commonly used method for synthesizing nano silver. This process involves Ag + Conversion to 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 is well controlled by controlling the reaction conditions. However, most chemical methods require the use of hydrazine hydrate, sodium borohydride, ascorbic acid, hydrogen peroxide, sodium citrate and the like as reducing agents to promote the synthesis of nano silver, and solvents used in the chemical reduction processMost are toxic, volatile, and potentially harmful 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 agents with the organic base triethylamine as a reaction promoter. However, the organic base triethylamine and formaldehyde have pungent odor, formaldehyde is also listed as a cancerogenic substance, and the used organic solvent is harmful to human beings, so that the invention does not need to use the dangerous chemical substance with high danger to human bodies, and the used solvent is ultrapure water, so that the nano silver can be synthesized by a one-pot method. The nano silver generated by the reaction of the ferulic acid and the silver oxide has good stability, simple synthetic route, economy, high efficiency, environmental protection and easy scale expansion, and can realize high-yield production.
In recent years, natural biomass materials are focused by researchers by virtue of the advantages of wide sources, low cost, reproducibility and the like, and the problems of biomass resource waste are effectively solved by functional development and high added value utilization of the natural biomass materials. Compared with other methods for synthesizing nano silver in the literature, the method for synthesizing nano silver by ferulic acid (FA, 4-hydroxy-3-methoxy cinnamic acid) has a plurality of advantages. Ferulic acid is widely present in vegetables, fruits, some beverages (such as coffee, beer, etc.) and some herbs such as angelica sinensis, cimicifuga foetida, ligusticum wallichii in reserves. And the price is low, and the water can be recycled in nature. It is a promising phytochemical with strong antioxidant activity, rarely exists in free form in plants, and forms a binding state with oligosaccharides, polyamines, lipids and polysaccharides. Structurally, ferulic acid contains phenolic hydroxyl groups and methoxy groups, so that the ferulic acid shows strong antioxidant activity, and the main effect is that the phenolic hydroxyl groups rapidly stop free radical chain reaction through a free radical scavenging mechanism. Second, the chemical structure of ferulic acid has highly conjugated unsaturation, and the molecule can be used as an effective ultraviolet absorber. The high ability of ferulic acid to absorb ultraviolet light may also contribute to its very effective antioxidant activity. Ferulic acid is a promising candidate material, and although the potential is huge, the advantages of ferulic acid are not fully utilized so far, so that the research of ferulic acid is significant. In addition, the nano silver also faces the problems of low yield, unsatisfied raw materials, environment protection, high raw material price, complex operation steps, harsh conditions and the like at present. Most of solvents used for synthesizing nano silver have the defects of harm to the environment or human body, non-recycling, unstable chemical property due to high oxidability, easy volatilization and the like.
In 2016, pramujitha Mendis et al, sodium borohydride is used as a main reducing agent, trisodium citrate and hydrazine sulfate are respectively used as a stabilizer and an auxiliary reducing agent, spherical silver nanoparticles are synthesized by using silver nitrate as a precursor, seven kinds of nano silver with different colors are developed, although the method reported in the document is simple and quick, no great breakthrough is made in selecting the reducing agent and the stabilizer, most of the silver nitrate is harmful to the environment, and the silver nitrate is a dangerous product which is easy to prepare and explode. In addition, for example, 2018, wong precha et al used one-pot method for preparing large-scale AgNPs-chitosan, although the method reported in this document is the same as the present invention, and all the methods are green synthesis methods, the reducing agent and stabilizer used in the document are chitosan, and the present invention uses ferulic acid. However, the equipment used in this report was an autoclave, and an experiment was required in which a chitosan stock solution and a silver nitrate solution were subjected to pressure application at 105 ℃, 110 ℃, 115 ℃ and 120 ℃ for 50 minutes. Then, experiments were performed at room temperature, 60 ℃, 90 ℃ and 120 ℃ for 8 hours without applying pressure. The equipment used in the report in the literature is dangerous, the reaction condition is also high temperature and high pressure, the reaction time is long, and the rapid production is not favored. 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 in a few minutes. In 2021, jharrimune et al synthesized Ag nanocubes by the polyol method, using hydrochloric acid, in which solvent (ethylene glycol) was considered as reducing agent, poly (N-vinyl pyrrolidone) (PVP) was shape-directing agent, and silver nitrate was the precursor. The ethylene glycol used in the method reported in the literature is a toxic organic solvent, the hydrochloric acid is a chemical which is corrosive and has great irritation to human skin, and more remarkable is that the method is used for synthesizing the Ag nanoThe rice process releases NO gas which, if exposed to air, may be further converted to NO 2 And (3) gas. Thus, the reaction must be carried out in a working, well ventilated fume hood, and protective clothing must be worn. In contrast, the reaction conditions used in the invention are simple and NO are produced 2 The solvent used is ultrapure water, is an excellent environment-friendly solvent and does not have danger to human bodies.
Therefore, the method for preparing the nano silver by green synthesis, which is simple to operate, environment-friendly in raw materials and quick in reaction, is a problem to be researched and solved.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the primary aim of the invention is to provide a green synthesis method for preparing nano silver by using plant extract ferulic acid; the method utilizes the ferulic acid to synthesize the nano silver for the first time, and can achieve the effect of synthesizing the nano silver stably without adding other stabilizing agents, and has simple process conditions, simple equipment and simple and convenient operation; the raw material ferulic acid used in the method is environment-friendly, has wide sources and high cost benefits, and is also convenient for large-scale production; the method also uses ultrapure water as a solvent system, so that the water is easy to obtain, has wide sources and can be recycled.
Another object of the present invention is to provide a nano silver synthesized by the above method, which has an average particle size of 35-80nm and excellent stability.
The aim of the invention is achieved 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, carrying out reaction under ultrasound, centrifuging to precipitate unreacted substances after the reaction is finished, and collecting supernatant to obtain nano silver; dispersing the precipitate with fresh ultrapure water, ultrasonic crushing, centrifuging to obtain precipitate and supernatant, repeating the dispersion, ultrasonic treatment and centrifuging operations of the precipitate 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 number 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 pole, the power ratio is 70%, and the time is 15min.
Preferably, the centrifugation condition is 2000 g-5000 g, and the time of each centrifugation is 8-12 min.
More preferably, the centrifugation conditions are 2000g and the time for each centrifugation is 10min.
A nano silver synthesized according to the above method, the average particle size of the nano silver being 35-80nm.
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 green, environmental protection, no toxicity, repeated use, wide source and low price.
(2) The reaction raw material used in the invention is a plant extract-ferulic acid, 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 ultra-pure water, so unreacted Ag 2 O can be easily removed by centrifugation, facilitating repeated sonication.
(3) The method only uses ferulic acid, ultrapure water and silver oxide as raw materials, and does not need to add any extra stabilizer or strong acid (HCL) or strong alkali (NaOH) to assist the synthesis of the ferulic acid, the ultrapure water and the silver oxide, and the method 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 accords with the concept 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 particles can stably exist at room temperature, and factors influencing the particle size of the nano silver and whether the nano silver particles can stably exist or not are well studied.
Drawings
Fig. 1 is a Transmission Electron Microscope (TEM) image of nano silver prepared in example 1.
FIG. 2 is an ultraviolet-visible absorption spectrum of silver nanoparticles in examples 1 to 7.
FIG. 3 is a graph showing the effect of days of standing on the UV absorbance of the synthesized nanosilver in examples 1 to 7.
Detailed Description
The present invention will be further described with reference to examples and drawings, but embodiments of the present invention are not limited thereto.
The reagents used in the examples are all commercially available. The examples include the ratios described in the figures, which are the mass ratios of silver oxide to ferulic acid. For example, "10:5" of FIG. 2 of the present invention is the mass of silver oxide of 10mg and ferulic acid of 5mg.
Example 1: weighing ferulic acid with absolute dry weight of 10mg and silver oxide with absolute dry weight of 5mg, placing into a 20mL sample bottle, adding 10mL of ultrapure water, performing ultrasonic treatment under the conditions of phi 6 rod and ultrasonic power ratio of 70% for 15min, precipitating unreacted substances by centrifugation (2000 g,10 min), and collecting supernatant as nano silver; dispersing the precipitate with fresh ultrapure water, then performing ultrasonic crushing on the precipitate for 15min under the conditions of a phi 6 rod and an ultrasonic power ratio of 70%, centrifuging to obtain the precipitate and supernatant, repeating the dispersion, ultrasonic and centrifugal operation of the precipitate for three times, and combining all the supernatants. The average particle diameter of the supernatant was 46.3nm as measured by a nanoparticle size and zeta potential analyzer and the zeta potential was-34.57 mV. The Transmission Electron Microscope (TEM) of the nano silver prepared in this example is shown in fig. 1, and it can be seen that the nano silver is spherical particles, and there is no aggregation between the nano particles, 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 431nm. Fig. 3 shows that the characteristic absorption peak value of the nano silver is increased to a certain value and is almost unchanged after the nano silver is stood for 7 days, which shows 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 into a 20mL sample bottle, adding 10mL of ultrapure water, performing ultrasonic treatment under the conditions of phi 6 rod and ultrasonic power ratio of 70% for 15min, precipitating unreacted substances by centrifugation (2000 g,10 min), and collecting supernatant as nano silver; dispersing the precipitate with fresh ultrapure water, then performing ultrasonic crushing on the precipitate for 15min under the conditions of a phi 6 rod and an ultrasonic power ratio of 70%, centrifuging to obtain the precipitate and supernatant, repeating the dispersion, ultrasonic and centrifugal operation of the precipitate for three times, and combining all the supernatants. The average particle diameter of the supernatant was 51.2nm as measured by a nanoparticle size and zeta potential analyzer and the zeta potential was-34.77 mV. The ultraviolet-visible light absorption spectrum of fig. 2 shows that the characteristic absorption peak of nano silver is 438nm. Fig. 3 shows that the characteristic absorption peak value of the nano silver is increased to a certain value and is almost unchanged after the nano silver is stood for 7 days, which shows that the nano silver has excellent stability.
Example 3: weighing 50mg of ferulic acid and 25mg of silver oxide with absolute dry weight, placing into a 20mL sample bottle, adding 10mL of ultrapure water, performing ultrasonic treatment under the conditions of a phi 6 rod and an ultrasonic power ratio of 70% for 15min, precipitating unreacted substances by centrifugation (2000 g,10 min), and collecting supernatant as nano silver; dispersing the precipitate with fresh ultrapure water, then performing ultrasonic crushing on the precipitate for 15min under the conditions of a phi 6 rod and an ultrasonic power ratio of 70%, centrifuging to obtain the precipitate and supernatant, repeating the dispersion, ultrasonic and centrifugal operation of the precipitate for three times, and combining all the supernatants. The average particle diameter of the supernatant was 77.1nm as measured by a nanoparticle size and zeta potential analyzer and the zeta potential was-25.03 mV. The ultraviolet-visible light absorption spectrum of fig. 2 shows that the characteristic absorption peak of nano silver is 444nm. Fig. 3 shows that the absorption peak of the nano silver is almost unchanged after standing for 7 days to increase to a certain extent, indicating that the nano silver has excellent stability.
Example 4: weighing ferulic acid with absolute dry weight of 10mg and silver oxide with absolute dry weight of 2.5mg, placing into a 20mL sample bottle, adding 10mL of ultrapure water, performing ultrasonic treatment under the conditions of phi 6 rod and ultrasonic power ratio of 70% for 15min, precipitating unreacted substances by centrifugation (2000 g,10 min), and collecting supernatant as nano silver; dispersing the precipitate with fresh ultrapure water, then performing ultrasonic crushing on the precipitate for 15min under the conditions of a phi 6 rod and an ultrasonic power ratio of 70%, centrifuging to obtain the precipitate and supernatant, repeating the dispersion, ultrasonic and centrifugal operation of the precipitate for three times, and combining all the supernatants. The average particle diameter of the supernatant was 43.8nm as measured by a nanoparticle size and zeta potential of-36.60 mV. The ultraviolet-visible light absorption spectrum of fig. 2 shows that the characteristic absorption peak of nano silver is 428nm. Fig. 3 shows that the characteristic absorption peak of nano-silver is almost unchanged after standing for 7 days, indicating that nano-silver has excellent stability.
Example 5: weighing ferulic acid with absolute dry weight of 5mg and silver oxide with absolute dry weight of 1mg, placing into a 20mL sample bottle, adding 10mL of ultrapure water, performing ultrasonic treatment under the conditions of phi 6 rod and ultrasonic power ratio of 70% for 15min, precipitating unreacted substances by centrifugation (2000 g,10 min), and collecting supernatant as nano silver; dispersing the precipitate with fresh ultrapure water, then performing ultrasonic crushing on the precipitate for 15min under the conditions of a phi 6 rod and an ultrasonic power ratio of 70%, centrifuging to obtain the precipitate and supernatant, repeating the dispersion, ultrasonic and centrifugal operation of the precipitate for three times, and combining all the supernatants. The average particle diameter of the supernatant was 35.4nm as measured by a nanoparticle size and zeta potential analyzer and the zeta potential was-40.33 mV. The ultraviolet-visible light absorption spectrum of fig. 2 shows a characteristic absorption peak of 419nm for nano silver. Fig. 3 shows that the characteristic absorption peak of nano-silver is almost unchanged after standing for 7 days, indicating that nano-silver has excellent stability.
Example 6: weighing ferulic acid with absolute dry weight of 10mg and silver oxide with absolute dry weight of 1mg, placing into a 20mL sample bottle, adding 10mL of ultrapure water, performing ultrasonic treatment under the conditions of phi 6 rod and ultrasonic power ratio of 70% for 15min, precipitating unreacted substances by centrifugation (2000 g,10 min), and collecting supernatant as nano silver; dispersing the precipitate with fresh ultrapure water, then performing ultrasonic crushing on the precipitate for 15min under the conditions of a phi 6 rod and an ultrasonic power ratio of 70%, centrifuging to obtain the precipitate and supernatant, repeating the dispersion, ultrasonic and centrifugal operation of the precipitate for three times, and combining all the supernatants. The average particle diameter of the supernatant was 35.8nm as measured by a nanoparticle size and zeta potential analyzer and the zeta potential was-40.6 mV. The ultraviolet-visible light absorption spectrum of fig. 2 shows that the characteristic absorption peak of nano silver is 410nm. Fig. 3 shows that the characteristic absorption peak of nano-silver is almost unchanged after standing for 7 days, indicating that 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 into a 20mL sample bottle, adding 10mL of ultrapure water, performing ultrasonic treatment under the conditions of phi 6 rod and ultrasonic power ratio of 70% for 15min, precipitating unreacted substances by centrifugation (2000 g,10 min), and collecting supernatant as nano silver; dispersing the precipitate with fresh ultrapure water, then performing ultrasonic crushing on the precipitate for 15min under the conditions of a phi 6 rod and an ultrasonic power ratio of 70%, centrifuging to obtain the precipitate and supernatant, repeating the dispersion, ultrasonic and centrifugal operation of the precipitate for three times, and combining all the supernatants. The average particle diameter of the supernatant was 37.4nm as measured by a nanoparticle size and zeta potential analyzer and the zeta potential was-42 mV. The ultraviolet-visible light absorption spectrum of fig. 2 shows that the characteristic absorption peak of nano silver is 412nm. Fig. 3 shows that the characteristic absorption peak of nano-silver is almost unchanged after standing for 7 days, indicating that nano-silver has excellent stability.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (5)
1. A green synthesis method for preparing nano silver by using ferulic acid of plant extract is characterized by comprising the following operation steps: the mass ratio of silver oxide to ferulic acid is 2: dissolving a mixture of silver oxide and ferulic acid in ultrapure water in a ratio of 1-20:1, performing reaction under ultrasound, centrifuging to precipitate unreacted substances after the reaction is finished, and collecting supernatant to obtain nano silver; dispersing the precipitate with fresh ultrapure water, then performing ultrasonic crushing, centrifuging to obtain precipitate and supernatant, repeating the dispersion, ultrasonic and centrifugal operations of the precipitate for three times, and combining all the supernatants; the conditions of the ultrasound are: the random amplitude transformer is a phi 2-15 number rod, the power ratio is 10-90%, and the time is 5-20 min.
2. The green synthesis method for preparing nano silver by using plant extract ferulic acid according to claim 1, wherein the method comprises the following steps: the conditions of the ultrasound are: the random amplitude transformer is a phi 6 pole, the power ratio is 70%, and the time is 15min.
3. The green synthesis method for preparing nano silver by using plant extract ferulic acid according to claim 1, wherein the method comprises the following steps: the centrifugation conditions are 2000 g-5000 g, and the centrifugation time is 8-12 min each time.
4. The green synthesis method for preparing nano silver by using plant extract ferulic acid according to claim 1, wherein the method comprises the following steps: the centrifugation condition is 2000g, and the time of each centrifugation is 10min.
5. A nano-silver synthesized according to the method of claim 1, characterized in that: the average grain diameter of the nano silver is 35-80nm.
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