CN103302306A - Method for reducing and preparing functionalized nano-silver based on polyphenol - Google Patents
Method for reducing and preparing functionalized nano-silver based on polyphenol Download PDFInfo
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- CN103302306A CN103302306A CN2013102420648A CN201310242064A CN103302306A CN 103302306 A CN103302306 A CN 103302306A CN 2013102420648 A CN2013102420648 A CN 2013102420648A CN 201310242064 A CN201310242064 A CN 201310242064A CN 103302306 A CN103302306 A CN 103302306A
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Abstract
The invention discloses a novel method for reducing and preparing functionalized nano-silver based on polyphenol. The preparation process is as follows: 1), stock solutions of all reaction liquids are prepared, and the stock solutions comprise a silver-bearing predecessor stock solution, a polyphenol compound stock solution and an alkaline stock solution; 2), a polyphenol compound solution is prepared: a certain amount of the polyphenol compound stock solution is taken and added into ultrapure water, and the stock solution and the ultrapure water are mixed uniformly; 3), the pH value and the temperature of the polyphenol compound solution are adjusted: a proper amount of the alkaline stock solution is taken and added into the polyphenol compound solution prepared in the step 2), the pH value of the mixed solution is adjusted, the mixed solution is placed and kept out of the sun, and the temperature of the mixed solution is adjusted; and 4), a nano-silver solution is generated: a certain amount of the silver-bearing predecessor stock solution is added into the mixed solution with adjusted pH value and temperature in the step 3) and is kept out of the sun, and reaction is performed for a certain time. The operation method is simple, the synthesis speed is high, the cost is low, the biocompatibility is high, the method is pollution-free, the sizes of the synthesized nano-silver particles are small, the monodispersity is good, and the nano-silver also has the performance of a polyphenol compound.
Description
Technical field
The present invention relates to the nano material preparing technical field, particularly relate to the method that a kind of polyphenol reduction prepares functionalized nano silver.
Background technology
Nano Silver has good broad-spectrum antibacterial action, is widely used in electronic product, household electrical appliance, cosmetics, textile and curable product, is one of the highest nano material of present commercialization.In addition, Nano Silver is at photoacoustic imaging, antiviral, antimycotic, antibiont tunicle, antithrombotic, antitumor and promote the aspect such as wound healing also to have potential using value.Therefore, the preparation of Nano Silver also receives researcher's very big concern always.
At present, the preparation method of Nano Silver comprises Physical, chemical method and bioanalysis.Physical comprises laser ablation method, electrochemical process, spark-discharge method etc., generally needs to use special instrument, and is expensive.Chemical method is the synthetic the most frequently used method of present Nano Silver, the shape that this method can fine regulation and control Nano Silver, distribution of sizes etc., but because it has introduced chemical reagent, may cause the harm to body health and environment.And the bioanalysis synthesizing nano-silver is the focus of studying at present, can utilize the preparation Nano Silvers such as bacterium, fungi, plant, and particularly receives people's concern based on the method for plant.Microorganism may be introduced the harmful substances such as endotoxin, and biology and the environmental safety of the Nano Silver that plant is synthetic are higher.The plant method mainly utilizes some bioactivators in the plant to come synthesizing nano-silver as reducing agent, such as polysaccharide, polyphenol etc.Because plant component is complicated, nanoscale silver and the distribution of sizes of being synthesized are relatively poor.
Summary of the invention
It is single and have the reducing agent of biological function that the technical problem that the present invention mainly solves provides a kind of composition, can solve with some bioactivators in the plant as reducing agent synthetic nanoscale silver and the poor difficult problem of distribution of sizes.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: provide that a kind of reduction prepares the method for functionalized nano silver based on polyphenol, preparation technology is as follows:
(1) prepares each reactant liquor stoste, comprising: argentiferous predecessor stoste, polyphenolic substance stoste and alkaline stoste;
(2) preparation polyphenolic substance solution: get a certain amount of polyphenolic substance stoste and add in the ultra-pure water, mix;
(3) pH value and the temperature of adjusting polyphenolic substance solution: get an amount of alkaline stoste and add in the prepared polyphenolic substance solution of step (2), the pH value of regulating mixed solution, lucifuge is placed, and regulates the temperature of mixed solution;
(4) generate Nano silver solution: get in the mixed solution of a certain amount of argentiferous predecessor stoste adding adjusted pH value of step (3) and temperature lucifuge reaction certain hour.
In a preferred embodiment of the present invention, the argentiferous predecessor in the described argentiferous predecessor stoste is at least a in silver nitrate, the silver acetate; The concentration of silver ion is 1～12mmol/L in the described argentiferous predecessor stoste.
In a preferred embodiment of the present invention, the polyphenolic substance in the described polyphenolic substance stoste is the compound with ortho position dihydroxy benzenes ring structure.
In a preferred embodiment of the present invention, the polyphenolic substance in the described polyphenolic substance stoste includes but not limited at least a in gallic acid, protocatechuic acid, caffeic acid, the chlorogenic acid; The concentration of the polyphenolic substance in the described polyphenolic substance stoste is 1～8mmol/L.
In a preferred embodiment of the present invention, described alkaline stoste is at least a in sodium hydroxide solution, potassium hydroxide solution, the ethanolamine solutions; The concentration of described alkaline stoste is 0.02～0.5mol/L.
In a preferred embodiment of the present invention, the pH value of mixed solution is 7.5～11.5 described in the step (3); The temperature of mixed solution is 10～50 ℃ described in the step (3), and preferred temperature is 20～30 ℃; The time of the reaction of lucifuge described in the step (4) is 10～60 minutes.
In a preferred embodiment of the present invention, the consumption of polyphenolic substance stoste is 200uL described in the step (2); The consumption of ultra-pure water is 10mL described in the step (2).
In a preferred embodiment of the present invention, the consumption of argentiferous predecessor stoste is 200～300uL described in the step (4).
The invention has the beneficial effects as follows: the present invention is based on the method that polyphenol reduction prepare functionalized nano silver, method of operating is simple, aggregate velocity is fast, with low cost, and the silver nano-grain size of synthesizing is little, and monodispersity is good; Not only composition is single for the used polyphenolic substance of the present invention, and has certain biological function, for example gallic acid has antibiotic, convergence, hemostasis, the effects such as antidiarrheal, protocatechuic acid has antibiotic, eliminate the phlegm, the effect of relievining asthma, caffeic acid has antibiotic, antiviral, the effect of increasing leukocyte and hemostasis, chlorogenic acid has antibiotic, antiviral, increase white blood cell, hepatic cholagogic, antitumor, hypotensive, reducing blood lipid, remove the effects such as free radical and stimulating central nervous system system, therefore, the present invention has also kept the biological synthesis process biocompatibility high, free of contamination characteristics, in addition, because polyphenolic substance is at the Nano Silver surface sorption, so that Nano Silver has again new function.
Description of drawings
Fig. 1 is transmission electron microscope (TEM) photo based on the nano-Ag particles of gallic acid reduction preparation;
Fig. 2 is transmission electron microscope (TEM) photo based on the nano-Ag particles of protocatechuic acid reduction preparation;
Fig. 3 is transmission electron microscope (TEM) photo based on the nano-Ag particles of caffeic acid reduction preparation;
Fig. 4 is transmission electron microscope (TEM) photo based on the nano-Ag particles of chlorogenic acid reduction preparation.
The specific embodiment
Below by specific embodiment method of the present invention is described, thereby so that advantages and features of the invention can be easier to be it will be appreciated by those skilled in the art that protection scope of the present invention is made more explicit defining.Method described in the following embodiment if no special instructions, is conventional method; Described reagent and material if no special instructions, all can obtain from commercial channels.
Embodiment 1
Under the room temperature, liquor argenti nitratis ophthalmicus, the gallic acid solution of 1mmol/L and the sodium hydroxide solution of 0.02mol/L of preparation 6mmol/L.Getting 200uL 1mmol/L gallic acid solution joins in the 10mL ultra-pure water, mix, then add the 0.02mol/L sodium hydroxide solution, the pH value of regulator solution is 9.5, again 200uL 6mmol/L liquor argenti nitratis ophthalmicus is added in the above-mentioned alkaline solution, mix, 10 ℃ of lucifuge reaction 30min can obtain Yellow nanometer silver solution.The TEM of sample characterizes as shown in Figure 1, average grain diameter 13nm.
Embodiment 2
Under the room temperature, silver acetate solution, the protocatechuic acid solution of 6mmol/L and the sodium hydroxide solution of 0.5mol/L of preparation 1mmol/L.Getting 200uL 6mmol/L protocatechuic acid liquid joins in the 10mL ultra-pure water, mix, then add the 0.5mol/L sodium hydroxide solution, the pH value of regulator solution is 10.5, again 300uL 1mmol/L silver acetate solution is added in the above-mentioned alkaline solution, mix, 50 ℃ of lucifuge reaction 10min can obtain Yellow nanometer silver solution.The TEM of sample characterizes as shown in Figure 2, average grain diameter 8.8nm.
Embodiment 3
Under the room temperature, liquor argenti nitratis ophthalmicus, the caffeic acid solution of 8mmol/L and the potassium hydroxide solution of 0.2mol/L of preparation 12mmol/L.Getting 200uL 8mmol/L caffeic acid solution joins in the 10mL ultra-pure water, mix, then add the 0.2mol/L potassium hydroxide solution, regulator solution pH value is 11.5, again 200uL 12mmol/L liquor argenti nitratis ophthalmicus is added in the above-mentioned alkaline solution, mix, 20 ℃ of lucifuge reaction 30min can obtain Yellow nanometer silver solution.The TEM of sample characterizes as shown in Figure 3, average grain diameter 6.8nm.
Embodiment 4
Under the room temperature, liquor argenti nitratis ophthalmicus, the solution of chlorogenic acid of 1mmol/L and the potassium hydroxide solution of 0.02mol/L of preparation 1mmol/L.Getting 100uL 1mmol/L solution of chlorogenic acid joins in the 10mL ultra-pure water, mix, then add the 0.02mol/L potassium hydroxide solution, regulator solution pH value is 7.5, again 200uL 1mmol/L liquor argenti nitratis ophthalmicus is added in the above-mentioned alkaline solution, mix, 50 ℃ of lucifuge reaction 60min can obtain Yellow nanometer silver solution.The sign of sample TEM as shown in Figure 4, average grain diameter 6.5nm.
Above-mentioned example only is explanation technical conceive of the present invention and characteristics, and its purpose is to allow the people who is familiar with technique can understand content of the present invention and according to this enforcement, can not limit protection scope of the present invention with this.All equivalent transformations that Spirit Essence is done according to the present invention or modification all should be encompassed within protection scope of the present invention.
Claims (8)
1. a method for preparing functionalized nano silver based on polyphenol reduction is characterized in that, concrete steps are as follows:
(1) prepare each reactant liquor stoste, described reactant liquor stoste comprises: argentiferous predecessor stoste, polyphenolic substance stoste and alkaline stoste;
(2) preparation polyphenolic substance solution: get a certain amount of polyphenolic substance stoste and add in the ultra-pure water, mix;
(3) pH value and the temperature of adjusting polyphenolic substance solution: get an amount of alkaline stoste and add in the prepared polyphenolic substance solution of step (2), the pH value of regulating mixed solution, lucifuge is placed, and regulates the temperature of mixed solution;
(4) generate Nano silver solution: get in the mixed solution of a certain amount of argentiferous predecessor stoste adding adjusted pH value of step (3) and temperature lucifuge reaction certain hour.
2. the method for preparing functionalized nano silver based on polyphenol reduction according to claim 1 is characterized in that, the argentiferous predecessor in the described argentiferous predecessor stoste is at least a in silver nitrate, the silver acetate; The concentration of silver ion is 1～12mmol/L in the described argentiferous predecessor stoste.
3. the method for preparing functionalized nano silver based on polyphenol reduction according to claim 1 is characterized in that, the polyphenolic substance in the described polyphenolic substance stoste is the compound with ortho position dihydroxy benzenes ring structure.
4. the method for preparing functionalized nano silver based on polyphenol reduction according to claim 3 is characterized in that, the polyphenolic substance in the described polyphenolic substance stoste includes but not limited at least a in gallic acid, protocatechuic acid, caffeic acid, the chlorogenic acid; The concentration of the polyphenolic substance in the described polyphenolic substance stoste is 1～8mmol/L.
5. the method for preparing functionalized nano silver based on polyphenol reduction according to claim 1 is characterized in that, described alkaline stoste is at least a in sodium hydroxide solution, potassium hydroxide solution, the ethanolamine solutions; The concentration of described alkaline stoste is 0.02～0.5mol/L.
6. the method for preparing functionalized nano silver based on polyphenol reduction according to claim 1 is characterized in that, the pH value of mixed solution is 7.5～11.5 described in the step (3); The temperature of mixed solution is 10～50 ℃ described in the step (3); The time of the reaction of lucifuge described in the step (4) is 10～60 minutes.
7. the method for preparing functionalized nano silver based on polyphenol reduction according to claim 6 is characterized in that, the temperature of mixed solution is 20～30 ℃ described in the step (3).
8. the method for preparing functionalized nano silver based on polyphenol reduction according to claim 1 is characterized in that, the consumption of polyphenolic substance stoste is 200uL described in the step (2); The consumption of ultra-pure water is 10mL described in the step (2);
The method for preparing functionalized nano silver based on polyphenol reduction according to claim 1 is characterized in that the consumption of argentiferous predecessor stoste is 200～300uL described in the step (4).
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| CN103706803A (en) * | 2013-10-21 | 2014-04-09 | 黄山学院 | Method for using grapefruit juice to restore silver ions in silver nitrate solution |
| CN103978223A (en) * | 2014-05-12 | 2014-08-13 | 武汉纺织大学 | Method for green synthesis of nano-gold by using water extract of eucommia ulmoides |
| CN103978222A (en) * | 2014-05-12 | 2014-08-13 | 武汉纺织大学 | Method for green synthesis of nano-palladium by using water extract of eucommia ulmoides |
| CN104338936A (en) * | 2014-10-29 | 2015-02-11 | 西南大学 | Synthetic method of stable silver nanoparticles |
| CN105234388A (en) * | 2015-09-29 | 2016-01-13 | 成都博岩科技有限公司 | Stability-enhanced nano-silver and preparation method and application thereof |
| CN106041352A (en) * | 2016-08-17 | 2016-10-26 | 武汉工程大学 | Silver nano-particle coated by organic acid silver, method for preparing silver nano-particle and application thereof |
| CN106392098A (en) * | 2016-10-10 | 2017-02-15 | 苏州经贸职业技术学院 | Preparation method of nanometer silver hydrosol and treatment method for dye wastewater |
| CN107088661A (en) * | 2017-05-11 | 2017-08-25 | 扬州大学 | A kind of synthetic method of Nano Silver |
| CN107363269A (en) * | 2017-09-23 | 2017-11-21 | 信阳师范学院 | A kind of preparation method of the Nano silver solution based on tea powder |
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