CN106129420A - The preparation of polypeptide R5 template nano palladium material, Morphological control and application in a fuel cell - Google Patents

The preparation of polypeptide R5 template nano palladium material, Morphological control and application in a fuel cell Download PDF

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CN106129420A
CN106129420A CN201610459709.7A CN201610459709A CN106129420A CN 106129420 A CN106129420 A CN 106129420A CN 201610459709 A CN201610459709 A CN 201610459709A CN 106129420 A CN106129420 A CN 106129420A
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polypeptide
palladium
preparation
nanometer
electrode
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唐正华
杨宏宇
陈少伟
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South China University of Technology SCUT
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88—Processes of manufacture
    • H01M4/8803—Supports for the deposition of the catalytic active composition
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88—Processes of manufacture
    • H01M4/8825—Methods for deposition of the catalytic active composition
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/90—Selection of catalytic material
    • H01M4/92—Metals of platinum group
    • H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
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Abstract

The invention discloses the preparation of a kind of nanometer Pd material with polypeptide as template, Morphological control and as effective catalyst application in fuel cell oxygen reduction.The advantage of this invention: the polypeptide introduced in the preparation of (1) this material has multiformity and specificity, biodegradable, containing self assembly fragment, can have the template of the nanometer Pd material of different-shape as synthesis；(2) nanometer Pd material building-up process convenient and swift (carrying out under simple agitation), green energy conservation (make solvent with water, synthesize under room temperature), the morphology controllable polypeptide nanometer Pd material of different-shape feature (the different Pd/R5 ratio controllable synthesis have), and this product property is sufficiently stable；(3) show in terms of hydrogen reduction with the polypeptide R5 (SSKKSGSYSGSKGSKRRIL) a series of palladium nanocatalysts as templated synthesis and be better than the catalytic performance of commercial platinum carbon, provide a kind of new cathode material for fuel cell, have a good application prospect.

Description

The preparation of polypeptide R5 template nano palladium material, Morphological control and at fuel cell In application
Technical field
Present invention application polypeptide nano material reacts for efficient catalytic oxidation-reduction, belongs to catalyst and new energy materials skill Art field.It is related specifically to the preparation of a kind of noble metal Bio-Nano-Materials catalyst, Morphological control and cloudy at fuel cell Application in terms of the material of pole.
Background technology
Proton Exchange Membrane Fuel Cells (Proton Exchange Membrane Fuel Cell, PEMFC) is fuel electricity One in pond, have that operating temperature is low, it is fast to start, specific power height, simple in construction, the advantage such as easy to operate, be acknowledged as electricity The first-selected energy at electrical automobile, stationary power generation station etc..PEMFC monocell is made up of anode, negative electrode and PEM, and anode occurs The oxidation of hydrogen fuel, the reduction of negative electrode generation oxygen, the catalyst accelerating electrode electro Chemical reaction is all contained at the two poles of the earth, due to negative electrode Reaction rate is low, so cathode reaction is rate-determing step.The main bottle of the large-scale commercial development of restriction PEMPC at present It is not ideal enough that neck is exactly the platinum material with carbon element catalysis activity of cathode reaction employing, and stability is the highest, and platinum is noble metal in addition, and the earth's crust contains Measure limited, relatively costly.Palladium is also noble metal, but relative to platinum, the most a lot, palladium catalyst is widely used for organic synthesis In field.
The noble metal nano particles such as Au Ag Pt Pd are owing to having quantum limitation effect, skin effect and macroscopic quantum tunnel The characteristics such as channel effect, show the performance mutually totally different with bulk noble metal solid, as surface plasmon resonance, surface peening are drawn The characteristics such as graceful scattering and fluorescence so that it is be widely used in catalysis, sensing, information storage, biomedical and energy storage and conversion In field.The performance of noble metal nano particles is affected very big by its size, pattern and structure etc., adjustable in order to obtain performance Nano material, introduce DNA, proteins and peptides etc. and inorganic matrix had the biomolecule of specificity affinity.
Polypeptide, owing to its structure is relatively easy, sequence is adjustable, is widely used in the reducing agent of noble metal nanometer material, guarantor Protecting agent, adjusting control agent and guiding agent, it is achieved the control to noble metal difference crystal face relative growth rate, induction composite structure function is many The nano material of sample.
According to having studied, polypeptide R5 (SSKKSGSYSGSKGSKRRIL) has specific effect, and end to Metal Palladium The RRIL sequence fragment of end can realize self assembly, and with R5 as template, different proportion based on palladium/R5 can get different-shape knot The nanometer Pd material of structure.Coupling that this kind of material is used in organic catalysis and reduction reaction, the application in electrochemical catalysis Seldom.Originating rare, expensive in view of the platinum material with carbon element as oxygen reduction catalyst, stability is low, the property that development substitutes Can be good, other cheap metal materials are the most necessary, are used for using R5 as the nanometer Pd material of templated synthesis different-shape Based on data with existing, hydrogen reduction catalytic applications, illustrates that its performance is better than platinum carbon, and the convenient and swift (room of this catalyst synthesis processes The lower stirring of temperature), green energy conservation (with water as solvent, biodegradable), meet sustainable development idea, before there is good application Scape.
The present invention uses the polypeptide nanometer Pd material of different-shape to study for hydrogen reduction catalytic performance, there is not yet disclosed Document or patent report.
Summary of the invention
In order to solve above-mentioned technical problem, the present invention provides a kind of Bio-Nano-Materials with polypeptide as template for efficiently The performance study of hydrogen reduction catalysis.
The present invention is achieved by the following technical solutions, specifically includes following step:
(1) according to mol ratio 1:60/90/120/150 of polypeptide Yu palladium element, under room temperature, by many for four parts of different volumes Peptide solution is diluted to same volume and mixes with equivalent potassium chloropalladite solution, stirs under certain speed.
(2) according to mol ratio 5:1 of sodium borohydride Yu palladium element, sodium borohydride (NaBH4) solution newly joined is added to mixed Close in liquid, and continue magnetic agitation, polypeptide palladium nanocatalyst.
Step (1) described polypeptide solution concentration is 4.97mmol/L；Potassium chloropalladite solution concentration is 38.54mmol/L； Mixing speed is 300rpm, and mixing time is 15min.
Step (2) described sodium borohydride (NaBH4) concentration is 0.1mol/L, mixing speed is 300rpm, and mixing time is 1h。
The unified load capacity of step (3) described catalyst is 80.8 μ g.cm-2。
In sum, compared with existing research, the invention have benefit that:
(1) preparation method of the present invention uses biodegradable, to have specific recognition and self-assembling function polypeptide R5 is template, and induction synthesizes the nanometer Pd material that a series of patterns are different.
(2) building-up process only needs stirring at normal temperature, convenient and swift；With water as solvent, green energy conservation；Avoid using poisonous examination Agent, environmental friendliness, meet the theory of sustainable development.
(3) the polypeptide palladium nano-particles synthesized preserves in aqueous solution, and stable in properties is nontoxic, biodegradable.
(4) the polypeptide nanometer Pd material hydrogen reduction take-off potential synthesized is high, and electric current density is big, and good cycle, electronics turns Shifting number is high, and catalysis activity is good, is better than the performance of commercial platinum carbon.
Accompanying drawing explanation
Fig. 1 is the uv-vis spectra of the polypeptide palladium nanocatalyst of different proportion prepared by example 1-4.
Fig. 2 is the high power transmission electron microscope (HRTEM) point of the polypeptide palladium nanocatalyst of different proportion prepared by example 1-4 Analysis.
Fig. 3 is the particle diameter column scattergram of the HRTEM analysis gained of example 1.
Fig. 4 is the cyclic voltammetry curve figure of the polypeptide palladium nanocatalyst of different proportion prepared by example 1-4.
Fig. 5 is the rotating disc electrode polarization curve of the polypeptide palladium nanocatalyst of different proportion prepared by example 1-4.
Fig. 6 is the polypeptide palladium nanocatalyst cyclic voltammetry curve figure contrast with commercial Pt/C catalyst of example 2 preparation.
Fig. 7 is the polypeptide palladium nanocatalyst rotating disc electrode polarization song with commercial Pt/C catalyst of example 2 preparation Line chart contrasts.
Fig. 8 is that the polypeptide palladium nanocatalyst of different proportion prepared by example 1-4 is at different rotation rates (100rpm Rotating disc electrode polarization curve under 2500rpm).
Fig. 9 is that the polypeptide palladium nanocatalyst of different proportion prepared by example 1-4 is by the KOUTECKY-of polarization curve gained LEVICH schemes.
Figure 10 is that the polypeptide palladium nanocatalyst of different proportion prepared by example 1-4 turns with the electronics of commercial Pt/C catalyst Move number (n) and hydrogen peroxide yield test figure.
Figure 11 is the polypeptide palladium nanocatalyst Tafel curve with commercial Pt/C catalyst of example 2 preparation.
Figure 12 is the polypeptide palladium nanocatalyst stability test figure with commercial Pt/C catalyst of example 2 preparation.
Figure 13 is that the polypeptide palladium nanocatalyst of different proportion prepared by example 1-4 is surveyed with commercial Pt/C catalyst electrochemistry Examination performance design parameter contrast.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further described, but the present invention is not limited to following example.
Embodiment 1.
(1) according to mol ratio 1:60 of polypeptide Yu palladium element, under room temperature, by dilute for the R5 polypeptide solution (4.97mM) of 9.86 μ L Release to 1776.72 μ L, add 76.28 μ L potassium chloropalladite solution (38.54mM) mixing, stir under the speed of 300rpm 15min。
(2) according to mol ratio 5:1 of sodium borohydride Yu palladium element, the sodium borohydride (NaBH that 147 μ L newly join is added4) solution (0.1M) in mixed liquor, and continue former speed magnetic agitation 1h, polypeptide palladium nanocatalyst.
Catalytic performance is tested:
It is to have three electrode body on the CHI 750E electrochemical workstation that Shanghai Chen Hua company produces that electro-chemical test characterizes The test pond of system is carried out.Wherein, platinum filament is to electrode, and Ag/AgCl electrode is reference electrode, is loaded with the glass carbon of catalyst Electrode is working electrode.24.78 μ L aqueous catalyst solutions are dripped in glassy carbon electrode surface, after its natural drying, drips 10 μ 5%Nafion solution (is diluted 100 times) by L Nafion ethanol solution in ethanol, and obtaining catalyst loadings is 80.8 μ g/ cm-2.Working electrode is placed in oxygen-saturated 0.1M KOH solution and carries out a volt-ampere cycle characteristics test.Test result such as Fig. 4,5, 8, shown in 9,10.
Fig. 4 is the VA characteristic curve of oxygen reduction reaction.It is loaded with the electrode of polypeptide palladium nanocatalyst prepared by this example Reduction peak position is 0.87V, and reduction peak current density is-0.41mA.cm-2。
Fig. 5 is the polarization curve of oxygen reduction reaction.It is loaded with the initial electricity of electrode of polypeptide palladium nanocatalyst prepared by this example Position relative standard hydrogen electeode is+0.99V, slightly above Pt/C (+0.98V).Limiting current density is～4.87mA.cm-2, higher than same Pt/C under the conditions of Deng (～4.0mA.cm-2)。
Fig. 8 is the polarization curve under the electrode different rotating speeds loading this sample, and along with rotating speed increases, its limiting current density becomes Greatly.
Fig. 9 is KOUTECKY-LEVICH curve, illustrate this sample under different voltages, the square root of its electric current density and rotating speed Inverse linear, explain its kinetics.
Figure 10 is electron transfer number and hydrogen peroxide yield curve.Electron transfer number is 3.92～3.95, and hydrogen peroxide yield is 2.63%～3.95%.Noticing that 1 molecule oxygen is directly reduced to water, electron transfer number is 4, and H2O2For by-product, its value is more Little the best.These results illustrate that its catalytic performance is superior.
Embodiment 2.
(1) according to mol ratio 1:90 of polypeptide Yu palladium element, under room temperature, by dilute for the R5 polypeptide solution (4.97mM) of 6.57 μ L Release to 1776.72 μ L, add 76.28 μ L potassium chloropalladite solution (38.54mM) mixing, stir under the speed of 300rpm 15min。
(2) according to mol ratio 5:1 of sodium borohydride Yu palladium element, the sodium borohydride (NaBH that 147 μ L newly join is added4) molten Liquid (0.1M) is in mixed liquor, and continues former speed magnetic agitation 1h, polypeptide palladium nanocatalyst.
Catalytic performance is tested:
It is to have three electrode body on the CHI 750E electrochemical workstation that Shanghai Chen Hua company produces that electro-chemical test characterizes The test pond of system is carried out.Wherein, platinum filament is to electrode, and Ag/AgCl electrode is reference electrode, is loaded with the glass carbon of catalyst Electrode is working electrode.25.28 μ L aqueous catalyst solutions are dripped in glassy carbon electrode surface, after its natural drying, drips 10 μ 5%Nafion solution (is diluted 100 times) by L Nafion ethanol solution in ethanol, and obtaining catalyst loadings is 80.8 μ g/ cm-2.Working electrode is placed in oxygen-saturated 0.1M KOH solution and carries out a volt-ampere cycle characteristics test.Test result such as Fig. 4,5, 6, shown in 7,8,9,10,11,12.
Fig. 4 and Fig. 6 is the VA characteristic curve of oxygen reduction reaction.It is loaded with the electricity of polypeptide palladium nanocatalyst prepared by this example The reduction peak position of pole is 0.88V, and higher than Pt/C (0.82V), reduction peak current density is-0.59mA.cm-2, higher than other three kinds Polypeptide nanometer Pd material, the most slightly above Pt/C (-0.57mA.cm-2)。
Fig. 5 and Fig. 7 is the polarization curve of oxygen reduction reaction.The electrode being loaded with polypeptide palladium nanocatalyst prepared by this example rises Beginning current potential relative standard hydrogen electeode is+0.99V, slightly above Pt/C (+0.98V).Limiting current density is 5.04mA.cm-2, it is higher than Other three peptide species nanometer Pd material and Pt/C (～4.0mA.cm-2)。
Fig. 8 is the polarization curve under the electrode different rotating speeds loading this sample, and along with rotating speed increases, its limiting current density becomes Greatly.
Fig. 9 is KOUTECKY-LEVICH curve, illustrate this sample under different voltages, the square root of its electric current density and rotating speed Inverse linear, explain its kinetics.
Figure 10 is electron transfer number and hydrogen peroxide yield curve.Electron transfer number is 3.94～3.96, and hydrogen peroxide yield is 2.14%～3.01%, it is better than other three peptide species nanometer Pd material and commercial Pt/C catalyst.
Figure 11 is Tafel curve, and the Tafel slope of this sample is 67mV/decade, close to the 64mV/decade of platinum carbon, says Its mechanism of catalytic reaction bright is identical with platinum carbon.
Figure 12 is the stability test of this sample, and test condition is that the electrode being loaded with catalyst is molten at oxygen-saturated 0.1M KOH With continuous firing 30000s under the electrode rotating speed of 900rpm in liquid, load the electrode current density decay 14.97% of this sample, and Platinum carbon has decayed 34.04%.
Embodiment 3.
(1) according to mol ratio 1:120 of polypeptide Yu palladium element, under room temperature, by the R5 polypeptide solution (4.97mM) of 4.93 μ L It is diluted to 1776.72 μ L, adds 76.28 μ L potassium chloropalladite solution (38.54mM) mixing, stir under the speed of 300rpm 15min。
(2) according to mol ratio 5:1 of sodium borohydride Yu palladium element, the sodium borohydride (NaBH that 147 μ L newly join is added4) solution (0.1M) in mixed liquor, and continue former speed magnetic agitation 1h, polypeptide palladium nanocatalyst.
Catalytic performance is tested:
It is to have three electrode body on the CHI 750E electrochemical workstation that Shanghai Chen Hua company produces that electro-chemical test characterizes The test pond of system is carried out.Wherein, platinum filament is to electrode, and Ag/AgCl electrode is reference electrode, is loaded with the glass carbon of catalyst Electrode is working electrode.25.56 μ L aqueous catalyst solutions are dripped in glassy carbon electrode surface, after its natural drying, drips 10 μ 5%Nafion solution (is diluted 100 times) by L Nafion ethanol solution in ethanol, and obtaining catalyst loadings is 80.8 μ g/ cm-2.Working electrode is placed in oxygen-saturated 0.1M KOH solution and carries out a volt-ampere cycle characteristics test.Test result such as Fig. 4,5, 8, shown in 9,10.
Fig. 4 is the VA characteristic curve of oxygen reduction reaction.It is loaded with the electrode of polypeptide palladium nanocatalyst prepared by this example Reduction peak position is 0.88V, and reduction peak current density is-0.52mA.cm-2。
Fig. 5 is the polarization curve of oxygen reduction reaction.It is loaded with the initial electricity of electrode of polypeptide palladium nanocatalyst prepared by this example Position relative standard hydrogen electeode is+0.99V, slightly above Pt/C (+0.98V).Limiting current density is 4.84mA.cm-2, higher than Pt/C (～4.0mA.cm-2)。
Fig. 8 is the polarization curve under the electrode different rotating speeds loading this sample, and along with rotating speed increases, its limiting current density becomes Greatly.
Fig. 9 is KOUTECKY-LEVICH curve, illustrate this sample under different voltages, the square root of its electric current density and rotating speed Inverse linear, explain its kinetics.
Figure 10 is electron transfer number and hydrogen peroxide yield curve.Electron transfer number is 3.90～3.95, and hydrogen peroxide yield is 2.35%～5.00%.
Embodiment 4.
(1) according to mol ratio 1:150 of polypeptide Yu palladium element, under room temperature, by the R5 polypeptide solution (4.97mM) of 3.94 μ L It is diluted to 1776.72 μ L, adds 76.28 μ L potassium chloropalladite solution (38.54mM) mixing, stir under the speed of 300rpm 15min。
(2) according to mol ratio 5:1 of sodium borohydride Yu palladium element, the sodium borohydride (NaBH that 147 μ L newly join is added4) molten Liquid (0.1M) is in mixed liquor, and continues former speed magnetic agitation 1h, polypeptide palladium nanocatalyst.
Catalytic performance is tested:
It is to have three electrode body on the CHI 750E electrochemical workstation that Shanghai Chen Hua company produces that electro-chemical test characterizes The test pond of system is carried out.Wherein, platinum filament is to electrode, and Ag/AgCl electrode is reference electrode, is loaded with the glass carbon of catalyst Electrode is working electrode.25.72 μ L aqueous catalyst solutions are dripped in glassy carbon electrode surface, after its natural drying, drips 10 μ 5%Nafion solution (is diluted 100 times) by L Nafion ethanol solution in ethanol, and obtaining catalyst loadings is 80.8 μ g/ cm-2.Working electrode is placed in oxygen-saturated 0.1M KOH solution and carries out a volt-ampere cycle characteristics test.Test result such as Fig. 4,5, 8, shown in 9,10.
Fig. 4 is the VA characteristic curve of oxygen reduction reaction.It is loaded with the electrode of polypeptide palladium nanocatalyst prepared by this example Reduction peak position is 0.88V, and reduction peak current density is-0.37mA.cm-2。
Fig. 5 is the polarization curve of oxygen reduction reaction.It is loaded with the initial electricity of electrode of polypeptide palladium nanocatalyst prepared by this example Position relative standard hydrogen electeode is+0.99V, slightly above Pt/C (+0.98V).Limiting current density is～4.30mA.cm-2, it is higher than Pt/C (～4.0mA.cm-2)。
Fig. 8 is the polarization curve under the electrode different rotating speeds loading this sample, and along with rotating speed increases, its limiting current density becomes Greatly.
Fig. 9 is KOUTECKY-LEVICH curve, illustrate this sample under different voltages, the square root of its electric current density and rotating speed Inverse linear, explain its kinetics.
Figure 10 is electron transfer number and hydrogen peroxide yield curve.Electron transfer number is 3.89～3.95, and hydrogen peroxide yield is 2.63%～5.59%.
Above-described embodiment is the present invention preferably detailed description of the invention, and wherein the catalytic effect of example 2 is optimal, but the present invention Protection domain be not limited thereto, the change made under other any spirit without departing from the present invention and principle, repair Adorn, substitute, combine, simplify, all should be the substitute mode of equivalence, within being included in protection scope of the present invention.

Claims (5)

1. a preparation for the palladium nano-particles with polypeptide as template, Morphological control and as effective catalyst at fuel cell Application in hydrogen reduction, it is characterised in that: comprise the steps:
(1) according to mol ratio 1:60/90/120/150 of polypeptide Yu palladium element, under room temperature, by molten for the polypeptide of four parts of different volumes Liquid be diluted to same volume and with equivalent potassium chloropalladite (K2PdCl4) solution mixing, stir under certain speed；
(2) according to mol ratio 5:1 of sodium borohydride Yu palladium element, the sodium borohydride (NaBH newly joined is added4) solution extremely mixing In liquid, and continue magnetic agitation, polypeptide palladium nanocatalyst；
(3) it is applied to hydrogen reduction catalytic applications with a series of polypeptide nanometer Pd materials prepared, obtains being better than the catalytic of platinum carbon Energy.
2. the peptide sequence used according to claim 1 is R5, and its amino acid range is SSKKSGSYSGSKGSKRRIL, its It is characterised by: there is the performance of self assembly, it is possible to by the pattern of self assembly regulation and control nano material, obtain spherical nanoparticle, Linear nanometer rods, network nano structure etc..
The preparation method of a peptide species palladium nanocatalyst the most according to claim 1, it is characterised in that: step (1) is described Polypeptide solution concentration is 4.97 mmol/L；Potassium chloropalladite solution concentration is 38.54 mmol/L；Mixing speed is 300 Rpm, mixing time is 15 min.
The preparation method of a peptide species palladium nanocatalyst the most according to claim 1, it is characterised in that: step (2) is described Sodium borohydride (NaBH4) concentration is 0.1 mol/L, mixing speed is 300 rpm, and mixing time is 1 h.
The preparation method of a peptide species palladium nanocatalyst the most according to claim 1, it is characterised in that: step (3) is described The unified load capacity of catalyst is 80.8 μ g.cm-2。
CN201610459709.7A 2016-06-21 2016-06-21 The preparation of polypeptide R5 template nano palladium material, Morphological control and application in a fuel cell Pending CN106129420A (en)

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