CN108339990A - A kind of preparation method of the silver-colored palladium core-shell nanospheres with catalytic activity - Google Patents
A kind of preparation method of the silver-colored palladium core-shell nanospheres with catalytic activity Download PDFInfo
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Abstract
A kind of preparation method of the galactic nucleus palladium shell nanosphere with catalytic activity, mainly by the acetic acid Vapreotide solution of a concentration of 0.1~0.3mM；According to acetic acid Vapreotide：Silver nitrate=1:Silver nitrate aqueous solution is added in 5~20 molar ratio, in 100~200rpm, 25 DEG C of 10~30h of incubation；By silver nitrate:Sodium borohydride=1:80~120 μ L sodium borohydride aqueous solutions are added in 5~10 molar ratio；The solution of acquisition distilled water is diluted 5~10 times, under stiring, by silver nitrate:Palladium chloride=1:0.5~3 molar ratio is with 10~20s/ drops, and palladium dichloride solution is added in the drop speed of 30 μ L/ drops, after 20~100s of reaction, by palladium chloride:Ascorbic acid=1:Palladium dichloride solution is added in 15~25 molar ratio, reacts 1~5min, is disperseed and the silver-colored palladium core-shell nanospheres of uniform particle diameter.Preparation process of the present invention is simple, environmentally protective, of low cost, and synthesized silver-colored Pd nano particle pattern is easily controllable, nucleocapsid is apparent, favorable dispersibility and has good catalytic activity.
Description
Technical field
The present invention relates to a kind of preparation methods of nano material.
Background technology
There are many excellent performances for noble metal nanometer material, they are in the side such as catalysis, plasma resonance, sensing, spectroscopy
Face has important application.In numerous nano materials, spherical noble metal nano particles are shown good due to dimensional effect
Good catalysis characteristics.Storage capacity of the palladium element in nature is abundant, and Pd nano particle shows to compare in alkaline solution
Higher catalytic activity.But palladium is as elctro-catalyst, some properties limit being widely used for it, for example, be easy poisoning,
React cross products complexity, high cost etc..Silver-colored presence can be removed effectively in oxidation reaction generation in palladium-based catalyst
Mesosome, to improve the anti-toxicity and stability of catalyst.Silver-colored palladium nanoparticle catalytic performance with nucleocapsid
Raising mainly due to the electronic effect between its unique structure and nucleocapsid.
Currently, the method for preparing silver-colored palladium nano-particles has polyol process, sol-gel method, coprecipitation and ultrasonic method etc..
However, the general low output of these methods, preparation process is more complicated, and cost is higher；Using organic solvent, growth directed agents and steady
Determine the chemical substances such as agent, lead to particle aggregation and environmental hazard, then affects its production and application.
Invention content
The simple and controllable, metal ladings the purpose of the present invention is to provide a kind of of low cost, environmentally protective, preparation process
The method of high galactic nucleus palladium shell nanosphere.Acetic acid Vapreotide template is mainly carried out sour processing by the present invention, it is made to expose band
The amino acid residue of charge is combined with silver ion and restores to obtain Vapreotide ping-pong ball shell.Nano silver grain is added in palladium chloride
In, the part silver hair life displacement reaction on part palladium chloride and silver-colored shell surface can be made, a part of small palladium particle is made to be attached to silver-colored shell
Surface, then remaining palladium chloride by the effect of reducing agent can Restore All are palladium particle, these palladium particles all wrap up
On Argent grain surface, to obtain the easily-controllable galactic nucleus palladium shell nanosphere of favorable dispersibility, pattern.
Technical scheme of the present invention is specific as follows：
(1) acetic acid Vapreotide is dissolved in the hydrochloric acid solution that pH is 1~3, is configured to the acetic acid of a concentration of 0.1~0.3mM
Vapreotide solution；
(2) according to acetic acid Vapreotide：The molar ratio of silver nitrate is 1:5~20 ratio is added into step (1) solution
Then silver nitrate aqueous solution is put it into the double-deck gas bath oscillator, in 100~200rpm, 25 DEG C of 10~30h of incubation；
(3) silver nitrate is pressed:The molar ratio of sodium borohydride is 1:5~10 ratio, it is fast in the solution being incubated to step (2)
The sodium borohydride aqueous solution that 5~25mM that 80~120 μ L are newly prepared is added in speed is restored, and solution becomes blue-black from transparent rapidly
Color；
(4) solution for obtaining step (3) dilutes 5~10 times with distilled water, under magnetic stirring, by silver nitrate:Dichloro
The molar ratio for changing palladium is 1:0.5~3 ratio is added into the good solution of above-mentioned dilution with 10~20 seconds/drop, the drop speed of 30 μ L/ drops
Enter palladium dichloride solution, after 20~100s of reaction, by palladium chloride:Ascorbic acid molar ratio is 1:15~25 ratio adds
Enter palladium dichloride solution, the control reaction time is 1~5min, solution colour becomes taupe, is disperseed and uniform particle diameter
Silver-colored palladium core-shell nanospheres.
The present invention has the following advantages that compared with prior art：
1, use acetic acid Vapreotide for template, molecular formula D-Phe-Cys-Tyr-D-Trp-Lys-Val-Cys-Trp-
NH2(Cys2-Cys7), simple in structure, it is easy to analysis and Control, contains the bases such as the disulfide bond and amino specifically bound with metal
Group.
2, in acid condition, acetic acid Vapreotide surface carry a large amount of positive charge, can by electrostatic force adsorbing metal from
Son.
3, nanosphere preparation process is simple, environmentally protective and silver-colored introducing reduces cost.
4, the metal ladings of nanosphere are high, and good dispersion, electrochemical surface active area is big, and catalytic activity is high.
5, the displacement reaction that reducing agent mediates can adjust the grain size and palladium layers thickness of this nanosphere, silver-colored Pd nano particle shape
Looks are easily controllable, nucleocapsid is apparent.
Description of the drawings
Fig. 1 is the TEM figures for the galactic nucleus palladium shell nanosphere that the embodiment of the present invention 1 obtains.
Fig. 2 is the TEM figures for the galactic nucleus palladium shell nanosphere that the embodiment of the present invention 2 obtains.
Fig. 3 is the TEM figures for the galactic nucleus palladium shell nanosphere that the embodiment of the present invention 3 obtains.
Fig. 4 is the Zeta potential figure for the galactic nucleus palladium shell nanosphere that the embodiment of the present invention 3 obtains.
Fig. 5 is the EDS figures for the galactic nucleus palladium shell nanosphere that the embodiment of the present invention 3 obtains.
Fig. 6 is the cyclic voltammogram for the galactic nucleus palladium shell nanosphere that the embodiment of the present invention 3 obtains.
Specific implementation mode
Embodiment 1
Acetic acid Vapreotide (the Wuhan sources Dong Kang Science and Technology Ltd.) is dissolved in the hydrochloric acid solution of pH=1.0, obtains 0.1mM's
Acid acetic acid Vapreotide solution；Above-mentioned 200 μ L of acetic acid Vapreotide solution are taken, silver nitrate solution (Beijing of 200 μ L1.5mM is added
Bei Hua fine chemicals Co., Ltd) after mixing, it is put into digital display bilayer gas bath constant temperature oscillator, in 100rpm,
It is incubated 10h at 25 DEG C, the sodium borohydride that a concentration of 10mM of 80 μ L Fresh is rapidly added into the solution being incubated is water-soluble
Liquid restores, and solution becomes black-and-blue from transparent；By above-mentioned solution with distilled water dilute 5 times, under magnetic agitation, into dilution with
10~20 seconds/drop, the Vitamin C of 6mM was added after reacting 20s in the 500 μ L of palladium chloride of the drop speed addition 0.8mM of 30 μ L/ drops
800 μ L of acid solution, continuing stirring 1min makes its solution colour become taupe to get silver-colored palladium core-shell nanospheres.
Morphology characterization is carried out to galactic nucleus palladium shell nanosphere using transmission electron microscope, as shown in Figure 1, the silver-colored palladium core of synthesis
Shell nanosphere grain size is 120nm or so, and nucleocapsid is apparent, and monodispersity is good, and gold is good with template bonding state.
Embodiment 2
Acetic acid Vapreotide (the Wuhan sources Dong Kang Science and Technology Ltd.) is dissolved in the hydrochloric acid solution of pH=2.0, obtains 0.2mM's
Acid acetic acid Vapreotide solution；Above-mentioned 200 μ L of acetic acid Vapreotide solution are taken, the silver nitrate solution (Beijing North of 200 μ L3mM is added
Change fine chemicals Co., Ltd) after mixing, it is put into digital display bilayer gas bath constant temperature oscillator, in 150rpm, 25
It is incubated 20h at DEG C, the sodium borohydride aqueous solution of a concentration of 15mM of 90 μ L Fresh is rapidly added into the solution being incubated
Reduction, solution become black-and-blue from transparent；Above-mentioned solution distilled water is diluted 7 times, under magnetic agitation, into dilution with 10
~20 seconds/drop, the ascorbic acid of 8mM was added after reacting 70s in the 600 μ L of palladium chloride of the drop speed addition 0.9mM of 30 μ L/ drops
900 μ L of solution, continuing stirring 3min makes its solution colour become taupe to get silver-colored palladium core-shell nanospheres.
Morphology characterization is carried out to silver-colored palladium core-shell nanospheres using transmission electron microscope, as shown in Fig. 2, the silver-colored palladium core of synthesis
Shell nanosphere grain size is 100nm or so, and nucleocapsid is apparent, and monodispersity is good, and gold is good with template bonding state.
Embodiment 3
Acetic acid Vapreotide (the Wuhan sources Dong Kang Science and Technology Ltd.) is dissolved in the hydrochloric acid solution of pH=3.0, obtains 0.3mM's
Acid acetic acid Vapreotide solution；Above-mentioned 200 μ L of acetic acid Vapreotide solution are taken, silver nitrate solution (Beijing of 200 μ L4.5mM is added
Bei Hua fine chemicals Co., Ltd) after mixing, it is put into digital display bilayer gas bath constant temperature oscillator, in 200rpm,
It is incubated 30h at 25 DEG C, the sodium borohydride that a concentration of 20mM of 100 μ L Fresh is rapidly added into the solution being incubated is water-soluble
Liquid restores, and solution becomes black-and-blue from transparent；Above-mentioned solution distilled water is diluted 10 times, under magnetic agitation, into dilution
With 10~20 seconds/drop, the 700 μ L of palladium chloride of 1.0mM were added in the drop speed of 30 μ L/ drops, and after reacting 100s, the anti-of 10mM is added
1000 μ L of bad hematic acid solution, continuing stirring 5min makes its solution colour become taupe to get silver-colored palladium core-shell nanospheres.
Morphology characterization is carried out to silver-colored palladium core-shell nanospheres using transmission electron microscope, as shown in figure 3, the silver-colored palladium core of synthesis
Shell nanosphere grain size is 85nm or so, and nucleocapsid is apparent, and monodispersity is good, and gold is good with template bonding state.
The current potential of Vapreotide, ping-pong ball shell and silver-colored palladium core-shell nanospheres is characterized using potential test instrument, such as Fig. 4 institutes
Show, the current potential of individual Vapreotide is 15.86mV, and potential value is 20.53mV after Vapreotide forms ping-pong ball shell with silver combination, works as palladium
Particle is combined with ping-pong ball shell to form silver-colored palladium core-shell nanospheres after potential value increase to 34.83mV, illustrate Nano silver grain with cut down it is general
Peptide and Pd nano particle are well combined and silver-colored palladium core-shell nanospheres have good stability.
Silver-colored palladium core-shell nanospheres are characterized using energy disperse spectroscopy, as shown in figure 5, occurring C, O, Ag, Pd, Cu member in power spectrum
The corresponding peak of element, wherein Cu, C element come from the copper mesh of carbon film covering, in addition, also containing C and O elements in Vapreotide；Al members
Usually from transmission electron microscope metal sample bar；Ag elements are incorporated in the Nano silver grain generation on Vapreotide surface；Pd elements are
Silver particles are replaced by palladium chloride and ascorbic acid restores what palladium chloride generated, illustrate that Vapreotide is combined with silver-colored Pd nano particle
Well, and purity is very high, without impurity.Vapreotide plays well as the template of space confinement in the arrangement of nano-particle
Effect, and then the performance of silver-colored Pd nano particle can be made more effectively to play, therefore Vapreotide is to prepare nano silver palladium material very
Good template.
Applied Electrochemistry work station carries out electro catalytic activity test to silver-colored palladium core-shell nanospheres, as shown in fig. 6, cyclic voltammetric
The reduction peak of the silver-colored palladium nanosphere of middle phase homogenous quantities is apparently higher than the reduction peak of commercially available Pd/C.By to silver-colored palladium nanosphere and commercially available
It is respectively 35.29m that numerical value, which is calculated, in the electrochemical surface effective active area (ECSA) of Pd/C2g-1And 175.07m2g-1。
Electrochemical surface effective active area (ECSA) calculation formula is：Sact=QH/mqH 0；QH=∫ Idt=∫ IdE/v.It should
The result shows that silver-colored palladium nanosphere has higher electrochemical surface active area, therefore silver-colored palladium core-shell nano ball compared to commercially available Pd/C
There is higher catalytic activity.
Claims (1)
1. a kind of preparation method of the silver-colored palladium core-shell nanospheres with catalytic activity, it is characterised in that：
(1) by acetic acid Vapreotide be dissolved in pH be 1~3 hydrochloric acid solution in, be configured to a concentration of 0.1~0.3mM acetic acid cut down it is general
Peptide solution；
(2) according to acetic acid Vapreotide：The molar ratio of silver nitrate is 1:Nitric acid is added into step (1) solution in 5~20 ratio
Then silver-colored aqueous solution is put it into the double-deck gas bath oscillator, in 100~200rpm, 25 DEG C of 10~30h of incubation；
(3) silver nitrate is pressed:The molar ratio of sodium borohydride is 1:5~10 ratio, in the solution being incubated to step (2) quickly plus
The sodium borohydride aqueous solution for entering 5~25mM of 80~120 μ L Fresh is restored, and solution becomes blue-black from transparent rapidly
Color；
(4) solution for obtaining step (3) dilutes 5~10 times with distilled water, under magnetic stirring, by silver nitrate:Palladium chloride
Molar ratio be 1:0.5~3 ratio is added two into the good solution of above-mentioned dilution with 10~20 seconds/drop, the drop speed of 30 μ L/ drops
Palladium chloride solution, after 20~100s of reaction, by palladium chloride:Ascorbic acid molar ratio is 1:15~25 ratio is added two
Palladium chloride solution, control reaction time are 1~5min, and solution colour becomes taupe, are disperseed and the silver-colored palladium of uniform particle diameter
Core-shell nanospheres.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109848440A (en) * | 2019-04-10 | 2019-06-07 | 燕山大学 | A kind of palladium method for preparing Nano cube |
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| JPH07150206A (en) * | 1993-12-01 | 1995-06-13 | Daido Steel Co Ltd | Production of ag-pd powder |
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2018
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| CN104841948B (en) * | 2015-05-15 | 2016-10-05 | 燕山大学 | A kind of method preparing starlike Pd nano particle for template with lanreotide acetate |
| CN105880624A (en) * | 2016-04-29 | 2016-08-24 | 燕山大学 | Method for self-assembling and synthesizing spherical gold nanoparticles by using bacitracin as template |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109848440A (en) * | 2019-04-10 | 2019-06-07 | 燕山大学 | A kind of palladium method for preparing Nano cube |
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