CN110076349B - Green preparation method of petal-shaped silver nanosheets - Google Patents
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Abstract
A green preparation method of petal-shaped silver nanosheets belongs to the technical field of precious metal nanometer material preparation. The preparation method of the petal-shaped silver nanosheet is in view of green chemistry, and toxic chemical reagents are not used in the preparation process. The method comprises the steps of taking water as a solvent, constructing a mixed solution reaction system by utilizing micromolecular organic acid and polyethylene glycol under the conditions of normal temperature and normal pressure, taking a water-soluble silver salt as a silver source, and taking micromolecular polyphenol compounds in tea extract and a mixture thereof as a reducing agent to prepare the petal-shaped silver nanosheet which is controllable in shape and size and good in uniformity in a green mode, wherein the diameter of the petal-shaped silver nanosheet is 400-600 nm, the thickness of the petal-shaped silver nanosheet is less than 80 nm, and the petal-shaped silver nanosheet has good antibacterial property. The preparation method is simple and easy to operate, and has the advantages of low cost, low toxicity, low energy consumption, high yield and the like.
Description
Technical Field
The invention belongs to the technical field of preparation of precious metal nano materials.
Background
The silver nano-sheet belongs to one of noble metal (such as gold, silver, platinum and the like) nano-materials. Due to the unique size and shape, the material has excellent performances in the aspects of conductivity, optical property, antibacterial property, chemical stability, plasticity and the like, and is widely applied to the fields of chemical catalysis, inorganic ion detection, surface Raman enhancement, printing, photoelectronic devices, biological engineering and the like.
The green tea, the white tea, the black tea and other tea contain rich polyphenol compounds such as catechin, epicatechin, gallocatechin, epigallocatechin gallate, gallic acid and the like, the polyphenol compounds have good antioxidant activity and are also good green reducing agents, and the application of the polyphenol compounds in the preparation of silver nanosheets is reported in the literature.
At present, the preparation methods of silver nanosheets reported in the literature mainly include a light-induced chemical reduction method, a rapid reduction precipitation method, a soft template method, a thermal deposition method, an ultrasonic radiation method and the like. The soft template synthesis method of nano material is a method for controllably synthesizing nano material with a certain morphology and size by using soft matter formed by a series of amphiphilic molecules such as micelle, microemulsion, vesicle or biological macromolecular aggregate as a template. However, in most methods for preparing silver nano-sheets by means of the soft template method, polyvinylpyrrolidone (PVP) is used as a surfactant and a protective agent, and sodium borohydride (NaBH) needs to be added into a reaction system4) Hydrogen peroxide (H)2O2) The silver nano-sheet is prepared by chemical reagents under the condition of high temperature (more than 100 ℃ of reflux), and the reagents used in the method have higher toxicity, complex preparation process and higher energy consumption.
In recent years, with the increasingly prominent environmental problems, the concept of green development is keen, and the preparation method of using low-energy-consumption green and environment-friendly starting materials to obtain the required materials becomes a hot point of research.
Disclosure of Invention
The invention aims to provide a green preparation method of petal-shaped silver nanosheets, which is simple in preparation method, easy to operate, low in cost, low in toxicity, low in energy consumption, high in yield and the like, and is suitable for industrial large-scale production.
The invention comprises the following steps:
1) mixing and dissolving polyethylene glycol, a small molecular organic acid and water to obtain a mixed solution with a pH value of 3-6;
dissolving silver salt in deionized water to obtain silver salt water solution with the concentration of 0.001-1.0 mol/L;
soaking tea leaves in deionized water, heating to 60-80 ℃, leaching for 20-40 min, naturally cooling, and filtering the soaked solution under reduced pressure by using a microporous filtering membrane to obtain a tea leaf extracting solution;
2) mixing the silver salt aqueous solution and the tea extract with the mixed solution under the stirring condition, and then reacting under the standing condition;
3) and after the reaction is finished, obtaining a solid-phase product, washing and then drying in vacuum to obtain the petal-shaped silver nanosheets.
The composite soft template constructed by polyethylene glycol and micromolecular organic acid is an acidic system with the pH value of 3-6, and is beneficial to slowly reducing silver salt in solution. If silver nitrate is easy to form silver hydroxide or silver oxide precipitate in an alkaline system, the formation and the structural regulation of the silver nano material are not facilitated.
The preparation method of the petal-shaped silver nanosheet is in view of green chemistry, and toxic chemical reagents are not used in the preparation process. The method comprises the steps of taking water as a solvent, constructing a mixed solution reaction system by utilizing micromolecular organic acid and polyethylene glycol under the conditions of normal temperature and normal pressure, taking a water-soluble silver salt as a silver source, and taking micromolecular polyphenol compounds in tea extract and a mixture thereof as a reducing agent to prepare the petal-shaped silver nanosheet which is controllable in shape and size and good in uniformity in a green mode, wherein the diameter of the petal-shaped silver nanosheet is 400-600 nm, the thickness of the petal-shaped silver nanosheet is less than 80 nm, and the petal-shaped silver nanosheet has good antibacterial property.
The preparation method is simple, easy to operate, low in cost, low in toxicity, low in energy consumption, high in yield and the like, and is particularly suitable for industrial large-scale production.
Furthermore, the molecular weight of the polyethylene glycol is 400-4000. Polyethylene glycol with the molecular weight of 400-4000 is recorded in an auxiliary material catalogue list of Chinese pharmacopoeia (2015 edition) as a nonionic water-soluble polymer, the polyethylene glycol with the molecular weight can be selected to construct a composite soft template reaction system with small molecular organic acid, and the required silver nano material can be prepared by means of a composite soft template method.
The mixing mass ratio of the polyethylene glycol, the micromolecular organic acid and the silver salt is 1: 3.84: 0.57. The small molecular organic acid is easy to dissolve in water and can be compounded with a high molecular surfactant to form a soft template reaction system. The soft template reaction system can effectively control and synthesize the silver nano material with certain shape and size. If the proportion of the substances is changed, the shape and the size of the obtained silver nano material can be greatly changed, and the formation of the petal-shaped silver nano sheet is not facilitated.
The small molecular organic acid is at least one of glycine, alanine, serine, cysteine, asparagine, glutamine, threonine, aspartic acid or glutamic acid. The functional groups of amino or carboxyl in the micromolecular organic acid have enrichment and fixation effects on silver ions, and the structure regulation of the silver nano material is easy to realize. The solvent adopted by the invention is deionized water, the reducing agent is tea extract, and the polyethylene glycol is a stabilizer, so that the silver nanoparticle protective agent not only has the functions of protecting and passivating the surfaces of the nanoparticles and preventing the particles from aggregating, but also can be used as a template to play an important role in inducing and controlling the size and the shape of the silver nanoparticles. The reagents are nontoxic and accord with the principle of green chemistry.
In the step 1), the pH value of the mixed solution is adjusted by using an aqueous solution of ammonia water, an aqueous solution of nitric acid or an aqueous solution of sodium hydroxide. The concentrations of the above aqueous solutions are relatively low, and are suitable for adjusting the pH value within a relatively small range.
The material of the invention utilizes tea polyphenol substances to reduce Ag in a water system+Obtaining petal-shaped silver nanosheet, if water-insoluble silver salt (such as AgCl, Ag) is used2CO3Etc.), the desired silver nanomaterial cannot be obtained by means of the experimental means described in the present invention. Therefore, the silver salt of the present invention is one of silver nitrate, silver acetate or silver fluoride, and the three are soluble silver salts.
The mixing ratio of the tea leaves to the deionized water is 1 g: 10-50 mL. The concentration of tea has influence on the preparation of the nano-silver tablets, such as low concentration of tea, low reduction reaction rate, low yield and possibility of incomplete reaction (partial Ag)+Not reduced to Ag). If the concentration of tea leaves is too high, the amount of reducing agent (tea polyphenol) is excessive, raw materials are wasted, and the result is not obtained easily.
The temperature condition of the standing reaction is 0-60 ℃, and the reaction time is 2-4 days. In the soft template system, the temperature condition is 0-60 ℃, and if the reaction temperature is too low, the reaction rate is too low; if the reaction temperature is too high, the silver nanosheet is not formed favorably. If the reaction time is less than 2 days, the product is mainly small particles of 2-50 nm, and the proportion of the generated petal-shaped nano silver sheets is less.
The temperature condition of the vacuum drying is 50-70 ℃, and the time is 12-14 hours. If the drying temperature is less than 50 ℃ or less, the drying time is long, and it takes 24 hours or more. If the drying temperature is higher than 70 ℃, the drying speed is too fast and easy to agglomerate, and the petal-shaped silver nano-sheets are difficult to redisperse.
Drawings
FIG. 1 is a TEM image of a sample prepared by the present invention.
FIG. 2 is an FE-SEM photograph of a sample prepared by the present invention.
Fig. 3 is an X-ray diffraction (XRD) pattern of the petal-shaped silver nanosheet prepared by the present invention.
FIG. 4 is an antibacterial diagram of the petal-shaped silver nanosheet hydrosol prepared by the method disclosed by the invention on different strains.
Detailed Description
Firstly, preparing petal-shaped silver nanosheets:
dissolving 11.5 g alanine in 1000 mL water, adding 3.0 g polyethylene glycol with molecular weight of 2000, stirring to dissolve, and adding dilute ammonia water and dilute HNO3Or adjusting the pH value of the mixed solution to 5.5 by using an aqueous solution of sodium hydroxide to obtain a mixed solution A.
1.699 g of silver nitrate (or silver acetate and silver fluoride) is dissolved in 100 mL of deionized water to prepare silver nitrate stock solution B with the concentration of 0.1 mol/L.
Soaking commercially available tea (green tea, yellow tea, white tea, oolong tea, black tea, and their mixture) 30.0 g in 500 mL of deionized water, heating to 80 deg.C, extracting for 30 min, naturally cooling, and filtering the soaked solution under reduced pressure with microporous membrane to obtain clear tea extractive solution C.
Under the conditions of normal temperature and normal pressure, the stirring speed is 500 rpm, 100 mL of silver salt solution B and 300 mL of tea extract C are added into the mixed solution A in sequence, and the stirring state is kept for 30 minutes. And after stirring, standing the mixture at 30 ℃ for reaction for 4 days, carrying out centrifugal sedimentation to obtain a solid D, and then drying the washed solid D in a vacuum drying oven at 50-70 ℃ for 12 hours to obtain the petal-shaped silver nanosheet.
The small molecular organic acid-alanine can be replaced by at least any one of glycine, serine, cysteine, asparagine, glutamine, threonine, aspartic acid and glutamic acid.
Secondly, product verification:
1. as can be seen from the TEM picture of the petal-shaped silver nanosheet shown in FIG. 1, the silver nanosheet disclosed by the invention has the petal-shaped characteristic appearance, good monodispersity and a diameter of 400-600 nm.
As can be seen from the FE-SEM picture of the petal-shaped silver nanosheets shown in figure 2, the silver nanosheets of the present invention have a thickness of less than 80 nm.
As can be seen from the X-ray diffraction (XRD) pattern of the petal-shaped silver nanosheet of fig. 3, strong diffraction peaks appear at diffraction angle 2 θ values of 38.24 °, 44.39 °, 64.60 °, 77.45 ° and 81.60 °, respectively correspond to (111), (200), (220), (311) and (222) crystal planes of a silver face-centered cubic lattice (FCC) silver nanostructure (JCPDS file number 04-0783), no diffraction peaks of other hetero phases appear, and the product is elemental silver. In addition, the diffraction intensity ratio of the (111) crystal face to the (200) crystal face of the silver nanostructure obtained through the experiment is about 6.4, which is consistent with the morphology of the silver nanostructure in SEM and TEM pictures of samples, and shows that a large amount of silver nanosheets are actually present in the system.
As can be seen from the antibacterial map (bacteriostasis circle method) of the petal-shaped silver nanosheet hydrosol shown in FIG. 4 on different strains, the silver nanosheets all show good antibacterial effects on gram-positive bacteria (plate division: Staphylococcus aureus (region a) and enterococcus faecalis (region d)), and gram-negative bacteria (Pseudomonas aeruginosa (region b) and Escherichia coli (region c)).
Claims (8)
1. A green preparation method of petal-shaped silver nanosheets is characterized by comprising the following steps:
1) mixing and dissolving polyethylene glycol, a small molecular organic acid and water to obtain a mixed solution with a pH value of 3-6; the small molecular organic acid is at least any one of glycine, alanine, serine, cysteine, asparagine, glutamine, threonine, aspartic acid or glutamic acid;
dissolving silver salt in deionized water to obtain silver salt water solution with the concentration of 0.001-1.0 mol/L;
soaking tea leaves in deionized water, heating to 60-80 ℃, leaching for 20-40 min, naturally cooling, and filtering the soaked solution under reduced pressure by using a microporous filtering membrane to obtain a tea leaf extracting solution;
2) mixing the silver salt aqueous solution and the tea extract with the mixed solution under the stirring condition, and then reacting under the standing condition;
3) and after the reaction is finished, obtaining a solid-phase product, washing and then drying in vacuum to obtain the petal-shaped silver nanosheets.
2. A green preparation method of petal-shaped silver nano-sheets according to claim 1, wherein the molecular weight of the polyethylene glycol is 400-4000.
3. The green preparation method of petaloid silver nanoplates as claimed in claim 2, wherein the mixing mass ratio of the polyethylene glycol, the small molecule organic acid and the silver salt is 1: 3.84: 0.57.
4. A green production method of petal-shaped silver nanosheets according to claim 1, characterized in that in step 1), the pH of the mixed solution is adjusted with an aqueous solution of ammonia, nitric acid, or sodium hydroxide.
5. A green preparation method of petaloid silver nanoplates according to claim 1, characterized in that the silver salt is one of silver nitrate, silver acetate or silver fluoride.
6. A green preparation method of petal-shaped silver nano-sheets according to claim 1, wherein the mixing ratio of the tea leaves to the deionized water is 1 g: 10-50 mL.
7. The green preparation method of petal-shaped silver nanosheets according to claim 1, wherein the standing reaction is carried out at a temperature of 0 to 60 ℃ for 2 to 4 days.
8. A green preparation method of petal-shaped silver nanosheets according to claim 1, wherein the vacuum drying is carried out at a temperature of 50 to 70 ℃ for 12 to 14 hours.
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| CN114808034B (en) * | 2022-05-09 | 2024-05-24 | 西安交通大学 | Lamellar flower-like nano silver and preparation method and application thereof |
| CN114888299B (en) * | 2022-05-20 | 2023-04-18 | 苏州大学 | Preparation method and application of broccoli-shaped micro-nano silver |
| CN115365493B (en) * | 2022-08-01 | 2024-03-26 | 武汉纺织大学 | Preparation method and application of Au@Ag nano composite particles under room temperature condition |
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