CN109570526A - A kind of ultrafine spherical nano-Ag particles and preparation method thereof - Google Patents
A kind of ultrafine spherical nano-Ag particles and preparation method thereof Download PDFInfo
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- CN109570526A CN109570526A CN201811621576.4A CN201811621576A CN109570526A CN 109570526 A CN109570526 A CN 109570526A CN 201811621576 A CN201811621576 A CN 201811621576A CN 109570526 A CN109570526 A CN 109570526A
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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
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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
Abstract
The present invention relates to a kind of ultrafine spherical nano-Ag particles and preparation method thereof, it disperses in silver-colored source in ethylene glycol, it is uniformly mixing to obtain mixed solution, tungstates is dissolved in ethylene glycol, is then added in mixed solution, is reacted at room temperature, product is washed after reaction, is dried to obtain the spherical superfine nano Argent grain of black, Nano silver grain is spherical in shape, monodispersed and do not reunite significantly, and particle is smaller and is evenly distributed, and the partial size of Nano silver grain is 6-6.5nm.The present invention prepares nano-Ag particles by a step solvent method, it is easy to operate, using ethylene glycol as reducing agent and solvent, it is environmentally protective, reaction carries out at room temperature, energy saving, the ultrafine spherical nano-Ag particles being prepared, have excellent catalytic properties, organic synthesis field with good application prospect.
Description
Technical field
The present invention relates to technical field of nano material, and in particular to a kind of ultrafine spherical nano-Ag particles and its preparation side
Method.
Background technique
Silver is that the important precious metal material of one kind causes very big concern due to its unique catalysis characteristics in recent years.It is many
Well known, catalytic performance is related with the morphology and size of material.Nano silver material has the spies such as large specific surface area, easily prepared
Point has wide practical use catalyzing and synthesizing the fields such as organic matter.Such as nanoscale silver is to the organic matters table such as paranitrophenol
Reveal higher catalytic action, can be used for the intermediate of pharmaceutical synthesis using the para-aminophenol that this characteristic synthesizes, be such as used for
Produce drug acetaminophen, azo dyes, sulfur dye, acid dyes etc..But the catalytic performance of silver is lower at present, uses silver content
It is more, it would therefore be desirable to prepare the lesser nano silver of particle, improve its catalytic capability.
The nano-Ag particles common reducing agent reported in the literature for preparing includes boron hydride, hydrazine hydrate, dimethylformamide
Deng reducing power is strong, and reaction rate is fast, generally yields spherical or spherical nano particle；Other reducing agents include grape
Sugar, ascorbic acid, alcohol compound, aldehyde compound, aminated compounds etc., reaction usually require under heating conditions into
Row.In order to preferably control size, size distribution, stability and the dissolubility of nano particle, it usually needs addition protective agent, this
So that there is the Coulomb force repelled each other between particle and can be stabilized.But above-mentioned preparation method has the following deficiencies: 1, uses
Reducing agent toxicity is relatively strong, reaction temperature is higher, the reaction time is long；2, operating procedure is more complex, is easily introduced impurity；3, what is formed receives
Rice Argent grain is larger, causes the catalytic capability of catalyzed nano silver relatively low.Given this we are reducing agent using ethylene glycol
And solvent, sodium tungstate are catalyst, quickly prepare nano-Ag particles at room temperature.
Summary of the invention
The purpose of the present invention is deficiency to solve above-mentioned technical problem, provide a kind of ultrafine spherical nano-Ag particles and its
Preparation method.
The deficiency of the present invention to solve above-mentioned technical problem, used technical solution is: a kind of ultrafine spherical nano silver
The preparation method of particle, disperses in silver-colored source in ethylene glycol, is uniformly mixing to obtain mixed solution, and tungstates is dissolved in ethylene glycol
In, it is then added in mixed solution, reacts at room temperature, product is washed after reaction, is dried to obtain the spherical super of black
Thin nano-Ag particles.
As a kind of advanced optimizing for preparation method of ultrafine spherical nano-Ag particles of the invention: the silver source is acetic acid
Silver or silver nitrate, tungstates are sodium tungstate or potassium tungstate.
As a kind of advanced optimizing for preparation method of ultrafine spherical nano-Ag particles of the invention: the silver source is acetic acid
Silver, tungstates are sodium tungstate.
As a kind of advanced optimizing for preparation method of ultrafine spherical nano-Ag particles of the invention: silver acetate in reaction solution
Molar ratio with sodium tungstate is 1:1.
As a kind of advanced optimizing for preparation method of ultrafine spherical nano-Ag particles of the invention: the reaction is continuing
Stirring is lower to be carried out.
As a kind of advanced optimizing for preparation method of ultrafine spherical nano-Ag particles of the invention: the reaction time is
20-50min。
A kind of ultrafine spherical nano-Ag particles, are made by above-mentioned preparation method, and Nano silver grain is spherical in shape, monodispersed
And do not reunite significantly, particle is smaller and is evenly distributed, and the partial size of Nano silver grain is 6-6.5nm.
Beneficial effect
One, the present invention prepares nano-Ag particles by a step solvent method, easy to operate；
Two, the present invention uses ethylene glycol as reducing agent and solvent, environmentally protective；
Three, reaction of the invention carries out at room temperature, energy saving；
Four, the ultrafine spherical nano-Ag particles that the present invention is prepared, have excellent catalytic properties, and have in organic synthesis field
There is preferable application prospect.
Detailed description of the invention
Fig. 1 is the flow diagram of the preparation method of ultrafine spherical nano-Ag particles of the present invention；
Fig. 2 is the x-ray diffraction pattern that ultrafine spherical nano-Ag particles are made in embodiment 1；
Fig. 3 is the transmission electron microscope figure that ultrafine spherical nano-Ag particles are made in embodiment 1；
Fig. 4 is that ultrafine spherical nano-Ag particles are made as catalyst in embodiment 1, is catalyzed sodium borohydride reduction p-nitrophenol
The UV-visible spectrum of timing tracking test reaction progress degree；
Fig. 5 is the transmission electron microscope figure I that spherical nano-Ag particles are made in embodiment 2.
Fig. 6 is the transmission electron microscope figure II that spherical nano-Ag particles are made in embodiment 2.
Fig. 7 is the transmission electron microscope figure I that spherical nano-Ag particles are made in embodiment 3；
Fig. 8 is the transmission electron microscope figure II that spherical nano-Ag particles are made in embodiment 3；
Fig. 9 is the x-ray diffraction pattern that spherical nano-Ag particles are made in embodiment 3.
Specific embodiment
Further technical solution of the present invention is illustrated below in conjunction with specific embodiment.
Embodiment 1
A kind of preparation method of ultrafine spherical nano-Ag particles:
One, by 1mmolC2H3AgO2It is dissolved in 20ml ethylene glycol, is then stirred, mixing time 30min is obtained
Uniform solution；
Two, by 1mmolNa2WO4•2H2O is dissolved in 20ml ethylene glycol, is stirred, and mixing time 30min is obtained
Uniform solution；
Three, the mixed solution of whipping step one and step 2, mixing time 30min, product is washed, dry after reaction
Obtain the spherical superfine nano Argent grain of black.
The process flow of preparation is as shown in Figure 1, the oxidizing potential of ethylene glycol at room temperature is 1.65V, with the increasing of temperature
Adding and reduces, ethylene glycol is a kind of preferable reducing agent at high temperature, but silver ion is difficult by reduction of ethylene glycol at room temperature,
Na2WO4•2H2Sexavalence tungsten in O has oxidisability, can Oxidation of Glycol be at room temperature aldehyde, to be silver ion reduction
Silver-colored simple substance.
The object of prepared product is mutually characterized, as shown in Fig. 2, all diffraction maximums all can refer to be designated as face-centered cubic phase
Crystal silver (JCPDSNo.36-1451).It is retouched electron microscope thoroughly to characterize the pattern of prepared nano silver sample, such as
Shown in Fig. 3, obtained Nano silver grain is spherical, monodispersed and does not reunite significantly that particle is smaller and is evenly distributed,
The partial size of Nano silver grain is 6-6.5nm.Display is catalyzed sodium borohydride reduction pair using Nano silver grain as catalyst in Fig. 4
Nitrophenol synthesizes para-aminophenol, passes through the result of the every 30 seconds tracking and testings catalysis reaction of ultraviolet-visible spectrum.Work as silver nanoparticle
Particle is added in reaction system, and the peak intensity of the absorption peak at 400nm gradually lowers, meanwhile, occur at 300nm
New absorption peak, and with the extension of time, the intensity of this new absorption peak gradually increases, illustrate more and more to nitro
Phenol is because of the presence of catalyst, and by sodium borohydride reduction at para-aminophenol, reaction is completed within 7min, illustrates prepared
Ultrafine spherical nano-Ag particles catalytic performance with higher.
Embodiment 2
A kind of preparation method of ultrafine spherical nano-Ag particles, comprising the following steps:
Step 1: by 1mmolC2H3AgO2It is dissolved in 20ml ethylene glycol, is then stirred, mixing time 30min,
Obtain uniform solution；
Step 2: by 0.5mmolNa2WO4•2H2O is dissolved in 20ml ethylene glycol, is stirred, and mixing time is
30min obtains uniform solution；
Step 3: the mixed solution of whipping step one and step 2, mixing time 30min, after reaction product it is washed,
It is dried to obtain the spherical superfine nano Argent grain of black.
It is retouched electron microscope thoroughly to characterize the pattern of prepared nano silver sample, as it can be seen in figures 5 and 6, obtaining
Nano silver grain be it is spherical, reunite, particle size distribution is uneven.
Embodiment 3:
A kind of preparation method of ultrafine spherical nano-Ag particles, comprising the following steps:
Step 1: by 1mmolC2H3AgO2It is dissolved in 20ml ethylene glycol, is then stirred, mixing time 30min,
Obtain uniform solution；
Step 2: by 0.2mmolNa2WO4•2H2O is dissolved in 20ml ethylene glycol, is stirred, and mixing time is
30min obtains uniform solution；
Step 3: the mixed solution of whipping step one and step 2, mixing time 30min, after reaction product it is washed,
It is dried to obtain brown material.
Electron microscope is retouched thoroughly to characterize the pattern of prepared nano silver sample, as shown in FIG. 7 and 8, is obtained
Nano silver grain be it is spherical, reunite, particle size distribution is uneven.Table is mutually carried out to the object of prepared product
Sign, as shown in figure 9, all diffraction maximums all can refer to be designated as tetragonal phase wolframic acid silver (JCPDSNo.70-179).
Embodiment 4:
A kind of preparation method of ultrafine spherical nano-Ag particles, comprising the following steps:
Step 1: by 1mmolAgNO3It is dissolved in 20ml ethylene glycol, is then stirred, mixing time 30min is obtained
To uniform solution；
Step 2: by 1mmolK2WO4It is dissolved in 20ml ethylene glycol, is stirred, mixing time 30min is obtained
Even solution；
Step 3: the mixed solution of whipping step one and step 2, mixing time 40min, after reaction product it is washed,
It is dried to obtain nano-Ag particles.
Embodiment 5:
A kind of preparation method of ultrafine spherical nano-Ag particles, comprising the following steps:
Step 1: by 1mmolC2H3AgO2It is dissolved in 20 ethylene glycol, is then stirred, mixing time 30min is obtained
To uniform solution；
Step 2: by 0.5mmolK2WO4It is dissolved in 20ml ethylene glycol, is stirred, mixing time 30min is obtained
Uniform solution；
Step 3: the mixed solution of whipping step one and step 2, mixing time 30min, after reaction product it is washed,
It is dried to obtain nano-Ag particles.
Embodiment 6:
A kind of preparation method of ultrafine spherical nano-Ag particles, comprising the following steps:
Step 1: by 1mmolAgNO3It is dissolved in 20 ethylene glycol, is then stirred, mixing time 30min is obtained
Uniform solution；
Step 2: by 0.5mmolNa2WO4•2H2O is dissolved in 20ml ethylene glycol, is stirred, and mixing time is
30min obtains uniform solution；
Step 3: the mixed solution of whipping step one and step 2, mixing time 30min, after reaction product it is washed,
It is dried to obtain nano-Ag particles.
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, though
So the present invention has been disclosed as a preferred embodiment, and however, it is not intended to limit the invention, any technology people for being familiar with this profession
Member, without departing from the scope of the present invention, when the technology contents using the disclosure above make out a little change or repair
Decorations are the equivalent embodiment of equivalent variations, but without departing from the technical solutions of the present invention, according to the technical essence of the invention
Any simple modification, equivalent change and modification to the above embodiments, all of which are still within the scope of the technical scheme of the invention.
Claims (7)
1. a kind of preparation method of ultrafine spherical nano-Ag particles, it is characterised in that: disperse in silver-colored source in ethylene glycol, stirring is equal
It is even to obtain mixed solution, tungstates is dissolved in ethylene glycol, is then added in mixed solution, is reacted at room temperature, reaction knot
Product is washed after beam, is dried to obtain the spherical superfine nano Argent grain of black.
2. a kind of preparation method of ultrafine spherical nano-Ag particles as described in claim 1, it is characterised in that: the silver source is vinegar
Sour silver or silver nitrate, tungstates are sodium tungstate or potassium tungstate.
3. a kind of preparation method of ultrafine spherical nano-Ag particles as claimed in claim 2, it is characterised in that: the silver source is vinegar
Sour silver, tungstates is sodium tungstate.
4. a kind of preparation method of ultrafine spherical nano-Ag particles as claimed in claim 3, it is characterised in that: acetic acid in reaction solution
The molar ratio of silver and sodium tungstate is 1:1.
5. a kind of preparation method of ultrafine spherical nano-Ag particles as described in claim 1, it is characterised in that: the reaction is being held
Continuous stirring is lower to be carried out.
6. a kind of preparation method of ultrafine spherical nano-Ag particles as described in claim 1, it is characterised in that: the reaction time
For 20-50min.
7. a kind of ultrafine spherical nano-Ag particles, it is characterised in that: nano-Ag particles are by the arbitrarily described nano silver of claim 1-6
The preparation method of particle is made, and Nano silver grain is spherical in shape, monodispersed and do not reunite significantly, and particle is smaller and is distributed
Uniformly, the partial size of Nano silver grain is 6-6.5nm.
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Application publication date: 20190405 |