CN110076349A - A kind of environment-friendly preparation method thereof of petal-shaped Nano silver piece - Google Patents
A kind of environment-friendly preparation method thereof of petal-shaped Nano silver piece Download PDFInfo
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- CN110076349A CN110076349A CN201910511275.4A CN201910511275A CN110076349A CN 110076349 A CN110076349 A CN 110076349A CN 201910511275 A CN201910511275 A CN 201910511275A CN 110076349 A CN110076349 A CN 110076349A
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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
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0551—Flake form nanoparticles
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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
- 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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Abstract
A kind of environment-friendly preparation method thereof of petal-shaped Nano silver piece, belongs to the preparation technical field of noble metal nanometer material.The preparation method of petal-shaped Nano silver piece of the present invention does not use the chemical reagent of toxicity from the point of view of Green Chemistry in preparation process.Using water as solvent, under normal temperature and pressure conditions, mixed solution reaction system is constructed using small molecular organic acid and polyethylene glycol, water soluble silver salt is silver-colored source, using tea extract small molecular polyphenol compound and its mixture to prepare for reducing agent green, appearance and size is controllable, the good petal-shaped Nano silver piece of homogeneity, its diameter has good antibiotic property less than 80 nm in 400~600 nm, thickness.Preparation method of the present invention is simple, easily operated, has many advantages, such as low cost, hypotoxicity, low energy consumption, high yield.
Description
Technical field
The invention belongs to the preparation technical fields of noble metal nanometer material.
Background technique
Nano silver piece belongs to one of noble metal (such as gold, silver and platinum) nano material.Due to its unique size with
Pattern, electric conductivity, optical, antibiotic property, chemical stability and in terms of show excellent performance, answer extensively
For fields such as chemical catalysis, inorganic ions detection, surface Raman enhancement, printing, opto-electronic device and bioengineering.
Polyphenol compound rich in the tealeaves such as green tea, white tea and black tea such as catechin, epicatechin, is not eaten
Sub- catechin, Epigallo-catechin gallate (EGCG) and gallic acid etc., substance of this kind have good antioxidant activity, also
It is good green reducing agent, and is applied and then rarely have document report in terms of the preparation of Nano silver piece.
Currently, the preparation method of Nano silver piece reported in the literature mainly has, photoinduction chemical reduction method, quickly reduction is heavy
Shallow lake method, soft template method, heat sink area method and ultrasonic radiation method etc..The soft template synthetic method of nano material be using micella, microemulsion,
The soft substance that a series of amphipathic molecules such as vesica or large biological molecule aggregation are formed is the controllable synthesis of template with certain
The method of the nano material of appearance and size.However, preparing majority in the method for Nano silver piece by means of soft template method uses poly- second
Alkene pyrrolidone (PVP) is surfactant and protective agent, needs to be added sodium borohydride (NaBH in reaction system4), hydrogen peroxide
(H2O2) etc. chemical reagent, prepare Nano silver piece, reagent used in such method under the conditions of high temperature (be greater than 100 DEG C reflux)
It is more toxic, and preparation process is complicated, energy consumption is higher.
In recent years, as environmental problem becomes increasingly conspicuous, Green Development theory has been rooted in the hearts of the people, and uses low energy consumption, green ring
Material needed for the preparation method of the starting material of guarantor obtains has become the hot spot that everybody studies.
Summary of the invention
It is easily operated the purpose of the present invention is to provide a kind of preparation method is simple, and there is low cost, hypotoxicity, low
The environment-friendly preparation method thereof of the petal-shaped Nano silver piece of the advantages that energy consumption, high yield, to be suitble to industrialization large-scale production.
The present invention the following steps are included:
1) by polyethylene glycol, small molecular organic acid and water mixed dissolution, the mixed solution that pH value is 3~6 is obtained；
Silver salt is dissolved in deionized water, the silver salt solution that concentration is 0.001~1.0 mol/L is obtained；
It takes infusion of tea in deionized water, 60~80 DEG C is heated to, and extract 20~40 min, using micro- after natural cooling
Hole filter membrane is filtered under diminished pressure the solution of immersion, obtains tea extract；
2) silver salt solution and tea extract are mixed under stirring condition with mixed solution, is then reacted under static conditions；
3) it to after reaction, obtain solid phase product, is dried in vacuo after washed, obtains petal-shaped Nano silver piece.
The acid system for being 3~6 in pH value by the compound soft template that polyethylene glycol and small molecular organic acid are constructed, is conducive to silver
Salt can be restored slowly in the solution.If silver nitrate is easily formed the precipitating of silver hydroxide or silver oxide under alkaline system,
Then it is unfavorable for formation and the structure regulating of silver nano material.
The preparation method of petal-shaped Nano silver piece of the present invention is from the point of view of Green Chemistry, in preparation process not
Use the chemical reagent of toxicity.Using water as solvent, under normal temperature and pressure conditions, small molecular organic acid and polyethylene glycol structure are utilized
Mixed solution reaction system is built, water soluble silver salt is silver-colored source, using tea extract small molecular polyphenol compound and its is mixed
Closing object is that reducing agent green prepares that appearance and size is controllable, the good petal-shaped Nano silver piece of homogeneity, diameter 400~
600 nm, thickness have good antibiotic property less than 80 nm.
Preparation method of the present invention is simple, easily operated, has many advantages, such as low cost, hypotoxicity, low energy consumption, high yield, special
It Shi He not industrialization large-scale production.
Further, the molecular weight of polyethylene glycol of the present invention is 400~4000.Chinese Pharmacopoeia (2015 editions) auxiliary material directory name
It is non-ionic water-soluble polymer that the polyethylene glycol that molecular weight is 400~4000 is described in list, and the present invention selects this point
The polyethylene glycol of son amount can construct compound soft template reaction system with small molecular organic acid, can be with by means of compound soft template method
Prepare required silver nano material.
The mixing mass ratio of the polyethylene glycol, small molecular organic acid and silver salt is 1: 3.84: 0.57.Small molecular organic acid
It is easily soluble in water, and it is soft template reaction system that compounding can be carried out with high molecular surfactant.This soft template reaction system
The silver nano material for synthesizing certain pattern, size can effectively be controlled.Such as change the proportion between substance, gained silver nano material
Morphology and size can have greatly changed, and be unfavorable for the formation of petal-shaped Nano silver piece.
The small molecular organic acid is glycine, alanine, serine, cysteine, asparagine, glutamine, Soviet Union
In propylhomoserin, aspartic acid or glutamic acid at least any one.Functional group amino or carboxylic in above each small molecular organic acid
Base is easily achieved the structure regulating of silver nano material to the enrichment of silver ion and fixed function.The solvent that the present invention uses be from
Sub- water, reducing agent are tea extracts, and polyethylene glycol is stabilizer, not only have and protect and be passivated nanoparticle surface, prevent
The effect of particle buildup is alternatively arranged as template and plays the size and pattern of Nano silver grain important induction and control action.
Mentioned reagent is innocuous agents, meets the principle of Green Chemistry.
In the step 1), with the aqueous solution of the aqueous solution of ammonium hydroxide, the aqueous solution of nitric acid or sodium hydroxide to the pH of mixed solution
Value is adjusted.The concentration of above each aqueous solution is relatively low, suitable for the adjustment to small range of pH value is changed.
Material of the present invention is to restore Ag using tea polyphenols substance in aqueous systems+Petal-like Nano silver piece is obtained, if adopting
With water-insoluble silver salt (such as AgCl, Ag2CO3Deng), then required silver can not be obtained by means of laboratory facilities of the present invention
Nano material.Therefore, silver salt of the present invention is one of silver nitrate, silver acetate or silver fluoride, this three kinds are all solubility
Silver salt.
The mixing ratio of the tealeaves and deionized water is 1 g: 10~50 mL.Preparation of the concentration of tealeaves to nano silver slice
Have an impact, if tea liquor body is low, reduction reaction rate is low, and yield is lower, it is possible to incomplete reaction (part Ag+It does not restore
For Ag).If tea liquor body is excessively high, the amount of reducing agent (tea polyphenols) is superfluous, wastes raw material, and be unfavorable for the acquisition of result.
The temperature condition for standing reaction is 0~60 DEG C, and the reaction time is 2~4 days.In this soft template system, temperature strip
Part is 0~60 DEG C, and if reaction temperature is too low, then reaction rate is too low；And such as reaction temperature is excessively high, then is unfavorable for forming silver nanoparticle
Piece.Reaction time is such as less than 2 days, and product is mainly the small particles of 2~50nm, and the ratio for generating petal shaped nano silver strip is less.
The vacuum drying temperature condition is 50~70 DEG C, and the time is 12~14 hours.Such as drying temperature less than 50 DEG C or more
Low, then drying time is long, needs 24 hours or longer time.If drying temperature is greater than 70 DEG C, then rate of drying is too fast
It is easy to reunite, petal-shaped Nano silver piece can be not easy by redisperse.
Detailed description of the invention
Fig. 1 is the TEM photo of the obtained sample of the present invention.
Fig. 2 is the FE-SEM photo of the obtained sample of the present invention.
Fig. 3 is that the X-ray diffraction (XRD) figure of petal-shaped Nano silver piece produced by the present invention is composed.
Fig. 4 is antibiogram of the petal-shaped Nano silver piece hydrosol produced by the present invention to different strains.
Specific embodiment
One, petal-shaped Nano silver piece is prepared:
It takes the alanine of 11.5 g to be dissolved in 1000 mL water, the polyethylene glycol that 3.0 g molecular weight are 2000 is then added, stirs
After mixing dissolution, dilute ammonium hydroxide, dilute HNO are used3Or the aqueous solution of sodium hydroxide adjusts its pH value to 5.5, i.e. acquisition mixed solution
A。
1.699 g silver nitrates (or silver acetate, silver fluoride) are taken to be dissolved in 100 mL deionized waters, being configured to concentration is
The silver nitrate stock solution B of 0.1 mol/L.
Taking the commercially available tealeaves of 30.0 g (can be green tea, yellow tea, white tea, green tea, black tea and dark green tea and their mixing
Object) it is soaked in 500 mL deionized waters, 80 DEG C are heated to, and extract 30 min, are subtracted after natural cooling using micropore filtering film
The solution that press filtration impregnates, obtains limpid tea extract C.
Under normal temperature and pressure conditions, speed of agitator is 500 rpm, and 100 mL silver salt solution B are successively added in mixed solution A
With the tea extract C of 300 mL, and it is kept stirring state 30 minutes.It is placed it in after stirring at 30 DEG C after standing reaction 4 days
Solid D is obtained through centrifugal sedimentation, then after drying 12 hours, obtains the solid D after washing in 50~70 DEG C of vacuum ovens
To petal-shaped Nano silver piece.
The above small molecular organic acid --- alanine can use glycine, serine, cysteine, asparagine, paddy
Glutamine, threonine, aspartic acid, in glutamic acid at least any one replace.
Two, Product Validation:
1, the TEM photo of petal-shaped Nano silver piece as shown in Figure 1 is as it can be seen that Nano silver piece of the present invention shows petal-shaped
The pattern of feature, monodispersity is preferable, and diameter is in 400~600 nm.
The FE-SEM photo of petal-shaped Nano silver piece as shown in Figure 2 is as it can be seen that Nano silver piece thickness < of the present invention
Within the scope of 80 nm.
By Fig. 3 petal-shaped Nano silver piece X-ray diffraction (XRD) figure spectrum as it can be seen that 2 θ value of the angle of diffraction be 38.24 °,
44.39 °, 64.60 °, 77.45 ° and 81.60 ° there is stronger diffraction maximum, correspond respectively to silver-colored face-centered cubic lattice (FCC) silver
(111), (200), (220), (311) and (222) crystal face of nanostructure (JCPDS file No. 04-0783), it is miscellaneous without other
The diffraction maximum of phase occurs, and shows that product is elemental silver.In addition, silver nanostructured the spreading out in (111) and (200) crystal face of experiment gained
Intensity is penetrated than about 6.4, this is consistent with silver nanostructured pattern in sample SEM and TEM photo, illustrates to be implicitly present in system
A large amount of Nano silver piece.
By the petal-shaped Nano silver piece hydrosol of Fig. 4 to the antibiogram (inhibition zone method) of different strains as it can be seen that Nano silver piece
To gram-positive bacteria (plate graduation: staphylococcus aureus (area a) and enterococcus faecalis (area d)), Gram-negative bacteria (verdigris
Pseudomonas alba (area b) and escherichia coli (area c)) show good antibacterial effect.
Claims (9)
1. a kind of environment-friendly preparation method thereof of petal-shaped Nano silver piece, it is characterised in that the following steps are included:
1) by polyethylene glycol, small molecular organic acid and water mixed dissolution, the mixed solution that pH value is 3~6 is obtained；
Silver salt is dissolved in deionized water, the silver salt solution that concentration is 0.001~1.0 mol/L is obtained；
It takes infusion of tea in deionized water, 60~80 DEG C is heated to, and extract 20~40min, using micro- after natural cooling
Hole filter membrane is filtered under diminished pressure the solution of immersion, obtains tea extract；
2) silver salt solution and tea extract are mixed under stirring condition with mixed solution, is then reacted under static conditions；
3) it to after reaction, obtain solid phase product, is dried in vacuo after washed, obtains petal-shaped Nano silver piece.
2. the environment-friendly preparation method thereof of petal-shaped Nano silver piece according to claim 1, it is characterised in that the polyethylene glycol
Molecular weight is 400~4000.
3. the environment-friendly preparation method thereof of petal-shaped Nano silver piece according to claim 2, it is characterised in that the polyethylene glycol, small
The mixing mass ratio of molecular organic acids and silver salt is 1: 3.84: 0.57.
4. the environment-friendly preparation method thereof of petal-shaped Nano silver piece according to claim 1, it is characterised in that the small molecule is organic
Acid is in glycine, alanine, serine, cysteine, asparagine, glutamine, threonine, aspartic acid or glutamic acid
At least any one.
5. the environment-friendly preparation method thereof of petal-shaped Nano silver piece according to claim 1, it is characterised in that in the step 1), with
Ammonium hydroxide, nitric acid or sodium hydrate aqueous solution are adjusted the pH value of mixed solution.
6. the environment-friendly preparation method thereof of petal-shaped Nano silver piece according to claim 1, it is characterised in that the silver salt is nitric acid
One of silver, silver acetate or silver fluoride.
7. the environment-friendly preparation method thereof of petal-shaped Nano silver piece according to claim 1, it is characterised in that the tealeaves and go from
The mixing ratio of sub- water is 1 g: 10~50 mL.
8. the environment-friendly preparation method thereof of petal-shaped Nano silver piece according to claim 1, it is characterised in that the standing reaction
Temperature condition is 0~60 DEG C, and the reaction time is 2~4 days.
9. the environment-friendly preparation method thereof of petal-shaped Nano silver piece according to claim 1, it is characterised in that described vacuum drying
Temperature condition is 50~70 DEG C, and the time is 12~14 hours.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113427015A (en) * | 2021-06-18 | 2021-09-24 | 上海交通大学 | Preparation method and application of novel silver nano material AgNFs |
| CN114808034A (en) * | 2022-05-09 | 2022-07-29 | 西安交通大学 | Laminar flower-like nano silver and preparation method and application thereof |
| CN114888299A (en) * | 2022-05-20 | 2022-08-12 | 苏州大学 | Preparation method and application of broccoli-shaped micro-nano silver |
| CN115365493A (en) * | 2022-08-01 | 2022-11-22 | 武汉纺织大学 | Preparation method and application of Au @ Ag nano composite particles at room temperature |
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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 |
| CN114888299A (en) * | 2022-05-20 | 2022-08-12 | 苏州大学 | Preparation method and application of broccoli-shaped micro-nano silver |
| CN115365493A (en) * | 2022-08-01 | 2022-11-22 | 武汉纺织大学 | Preparation method and application of Au @ Ag nano composite particles at room temperature |
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