CN105244513A - Graphite-phase carbon nitride-modified carbon black-loaded platinum-palladium alloy nano electrocatalyst and preparation method - Google Patents
Graphite-phase carbon nitride-modified carbon black-loaded platinum-palladium alloy nano electrocatalyst and preparation method Download PDFInfo
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- CN105244513A CN105244513A CN201510629798.0A CN201510629798A CN105244513A CN 105244513 A CN105244513 A CN 105244513A CN 201510629798 A CN201510629798 A CN 201510629798A CN 105244513 A CN105244513 A CN 105244513A
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- H01M4/90—Selection of catalytic material
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- H01M4/88—Processes of manufacture
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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
- H01M4/90—Selection of catalytic material
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- H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
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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
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/921—Alloys or mixtures with metallic elements
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Abstract
The invention discloses a graphite-phase carbon nitride-modified carbon black-loaded platinum-palladium alloy nano electrocatalyst and a preparation method. The method comprises the steps as follows: melamine is adopted as a precursor for the first time; graphite-phase carbon nitride grows on a carbon black surface, so that the electrochemical corrosion resistance of the carbon black in an acidic electrolyte is improved; and with platinum nitrate and palladium nitrate as the precursors and hydrazine hydrate as a reducing agent, platinum-palladium alloy nanoparticles of which the average particle size is 5nm are evenly deposited on the graphite-phase carbon nitride-modified carbon black surface, so as to obtain the graphite-phase carbon nitride-modified carbon black-loaded platinum-palladium alloy nano electrocatalyst. Reaction conditions are mild; a surfactant does not need to be used; and the graphite-phase carbon nitride-modified carbon black-loaded platinum-palladium alloy nano electrocatalyst has relatively high electrochemical catalytic activity, stability and electrochemical corrosion resistance, and has relatively good application prospect and economic benefits in the aspects of direct alcohol fuel cells.
Description
Technical field
The invention belongs to Nano-composite materials field, specifically relate to carbon black loadings platinum-nickel alloys nanometer electrical catalyst of a kind of graphite phase carbon nitride modification and preparation method thereof.
Background technology
Platinum/carbon (Pt/C) and palladium/carbon (Pd/C) catalyst are widely used in organic catalysis, the key areas such as fuel cell and electrochemical catalysis.Research shows, Pt/C or Pd/C catalyst is when for fuel cell anode catalytic oxidation, all there is electrochemical corrosion phenomenon [Quantitativecharacterizationofcatalystlayerdegradationin PEMfuelcellsbyX-rayphotoelectronspectroscopy [J] .ElectrochimicaActa in noble metal and carbon support material, 2009,54:4025-4030].The electrochemical corrosion of electrode catalyst will directly cause fuel battery performance rapid decay [PEMfuelcellcathodecarboncorrosionduetotheformationofair/ fuelboundaryattheanode [J] .JournalofPowerSources, 2006,158:1306-1312], cannot application request be met.
Graphite phase carbon nitride has the advantageous characteristic of electrochemically resistant corrosion as the new material of a kind graphene-structured.Graphite phase carbon nitride is used for modifying carbon black, the object of stability and the resistance to electrochemical corrosion energy improving catalyst can be reached.Still there is more serious defect in the preparation method of the graphite phase carbon nitride modification carbon black that present stage is reported.Document " Synthesisofcarbonclack/carbonnitrideintercalationcompoun dcompositeforefficienthydrogenproduction [J] .DaltonTrans., 2014,43:12013-12017 " report the method that molten salt growth method prepares carbonitride modified carbon black.The method grinds melamine, carbon black, sodium chloride, potassium chloride, lithium chloride into powder mixing, and calcines at 500 DEG C, obtains the carbon black of carbonitride modification.But the raw material of the method is complicated, and productive rate is low, and the carbon content of product is low, poorly conductive.Higher calcining heat, destroys the surface functional group of carbon black, hinders noble metal nano particles in the nucleation of carbon blacksurface, and then has influence on the activity of eelctro-catalyst.
Summary of the invention
The object of the invention is to propose a kind of with melamine and carbon black for raw material, the carbon black that graphite phase carbon nitride is modified is obtained under lower calcining heat, and with this material for carrier, the carbon black loadings platinum-nickel alloys nanometer electrical catalyst that preparation graphite phase carbon nitride is modified.This catalyst has excellent electrochemical catalysis performance and resistance to electrochemical corrosion energy.
The technical solution realizing the object of the invention is: carbon black loadings platinum-nickel alloys nanometer electrical catalyst that a kind of graphite phase carbon nitride is modified and preparation method thereof, comprises the following steps:
The first step, obtains acid-treated carbon black by carbon black hydrothermal treatment consists in red fuming nitric acid (RFNA);
Second step, by melamine and the stirring and dissolving dispersion in a solvent of acid-treated carbon black;
3rd step, instills second step gained dispersion liquid and stirs, is separated, obtains melamine/black stock with straight alcohol washing, drying by dust technology;
4th step, under nitrogen protection, calcines the 3rd step gained melamine/black stock, obtains graphite phase carbon nitride/carbon black compound at 300 ~ 400 DEG C;
5th step, by graphite phase carbon nitride/carbon black compound ultrasonic disperse in a solvent, add platinum nitrate solution, palladium nitrate solution, hydrazine hydrate solution successively, and stir, after reaction terminates, after centrifugation, washing, drying, obtain the carbon black loadings platinum-nickel alloys nanometer electrical catalyst that graphite phase carbon nitride is modified.
In step one, described carbon black is Vulcan
xC-72R, carbon black and red fuming nitric acid (RFNA) mass ratio are 1:100 ~ 120, and the concentration of red fuming nitric acid (RFNA) is 68wt%; Heat treatment temperature is 120 DEG C; Heat treatment time is 8 ~ 12h; The reaction vessel that heat treatment adopts is teflon-lined stainless steel hydro-thermal counteracting tank, loading 50%.
In step 2, the mass ratio of described melamine and acid-treated carbon black is 4 ~ 0.5:1; Solvent select in deionized water and ethylene glycol any one, wherein the quality of water is 300 ~ 500 times of melamine, and the quality of ethylene glycol is 50 ~ 100 times of melamine.
In step 3, described dust technology concentration is 0.1 ~ 0.2mol/L, and the quality of dust technology is 100 ~ 150 times of melamine.
In step 4, described calcination time is 1 ~ 3h.
In step 5, one or more of deionized water, ethanol, ethylene glycol selected by described solvent; The concentration of platinum nitrate solution is 0.77mol/L, and the concentration of palladium nitrate solution is 0.94mol/L; The mass ratio of platinum nitrate, palladium nitrate and graphite phase carbon nitride/carbon black compound is 0.27:0.18:1, and hydrazine hydrate solution concentration is 85wt%, and the quality of hydrazine hydrate solution is 80 ~ 100 times of noble metal gross mass.
Compared with prior art, its advantage is in the present invention: the carbon black that (1) adopts lower calcining heat synthetic graphite phase carbon nitride to modify, and production technology is simple, and energy consumption is low; (2) reduce platinum nitrate, palladium nitrate at normal temperatures and pressures, form platinum-nickel alloys, reaction condition is gentle, without the need to using surfactant; (3) carbon black that graphite phase carbon nitride is modified has high dispersive effect, and platinum palladium nano-particles particle diameter can be made less, and dispersiveness is better; (4) the carbon black loadings platinum-nickel alloys nanometer electrical catalyst applying graphite phase carbon nitride modification prepared by the present invention has: electrochemical catalytic oxidation performance is good, multi-functional catalysis, the advantage that resistance to electrochemical corrosion energy is strong, will have good application prospect and economic benefit in fuel cell.
Accompanying drawing explanation
Accompanying drawing 1 is schematic diagram prepared by the carbon black loadings platinum-nickel alloys nanometer electrical catalyst of graphite phase carbon nitride of the present invention modification.
Accompanying drawing 2 is the XRD collection of illustrative plates of the carbon black loadings platinum-nickel alloys nanometer electrical catalyst that example 2 gained graphite phase carbon nitride of the present invention is modified.
Accompanying drawing 3 is the TEM photos of the carbon black loadings platinum-nickel alloys nanometer electrical catalyst that example 2 gained graphite phase carbon nitride of the present invention is modified.
Accompanying drawing 4 is cyclic voltammograms of example 3 gained graphite phase carbon nitride of the present invention/carbon black compound resistance to electrochemical corrosion energy.
Accompanying drawing 5 is the cyclic voltammograms of the different alcohols of carbon black loadings platinum-nickel alloys nanometer electrical catalyst catalytic oxidation that example 2 gained graphite phase carbon nitride of the present invention is modified.
Embodiment
Mechanism of the present invention is: (1), by low temperature calcination, makes melamine react with the oxygen-containing functional group through the carbon blacksurface of nitric acid treatment and forms strong chemical bond effect, form stable graphite phase carbon nitride/carbon black compound.(2) peptizaiton of the carbon black utilizing carbonitride to modify by softening method, loads to the carbon blacksurface that carbonitride is modified by platinum-nickel alloys nano particle, obtain the carbon black loadings platinum-nickel alloys nanometer electrical catalyst that graphite phase carbon nitride is modified.By reference to the accompanying drawings 1, the carbon black loadings platinum-nickel alloys nanometer electrical catalyst that graphite phase carbon nitride is modified, prepared by following steps and obtain:
Carbon black 120 DEG C of hydrothermal treatment consists 8 ~ 12h in 68% red fuming nitric acid (RFNA) are obtained acid-treated carbon black by the first step;
Second step, by melamine and the stirring and dissolving dispersion in a solvent of acid-treated carbon black;
3rd step, instills second step gained dispersion liquid and stirs, is separated, obtains melamine/black stock with straight alcohol washing, drying by dust technology;
4th step, under nitrogen protection, calcines the 3rd step gained melamine/black stock, obtains graphite phase carbon nitride/carbon black compound at 300 ~ 400 DEG C;
5th step, by graphite phase carbon nitride/carbon black compound ultrasonic disperse in a solvent, add platinum nitrate solution, palladium nitrate solution, hydrazine hydrate solution successively, and stir, after reaction terminates, after centrifugation, washing, drying, obtain the carbon black loadings platinum-nickel alloys nanometer electrical catalyst that graphite phase carbon nitride is modified.
Embodiment 1: the preparation method of the carbon black loadings platinum-nickel alloys nanometer electrical catalyst that graphite phase carbon nitride of the present invention (30%) is modified, comprises the following steps:
The first step, by 1gVulcan
xC-72R is placed in 100g red fuming nitric acid (RFNA), stirs, and is transferred in 200mL water heating kettle, at 120 DEG C of reaction 12h.By product centrifugation, drying obtains acid-treated carbon black;
Second step, by 300mg melamine and the acid-treated carbon black dispersion of 700mg in 100mL deionized water;
3rd step, 40mL dust technology (0.1mol/L) is instilled the dispersion liquid of second step gained and stirs 1h, centrifugation, and ethanol washs 3 times, dry;
4th step, by the 3rd step gained melamine/black stock, calcines 2h, obtains graphite phase carbon nitride/carbon black compound in 400 DEG C of nitrogen atmospheres;
5th step, is distributed in 40mL deionized water by graphite phase carbon nitride/carbon black compound 20mg, ultrasonic disperse 1h.22 μ L0.77mol/LPt (NO are instilled in dispersion liquid
3)
2solution, 18 μ L0.94mol/LPd (NO
3)
2solution, stirs 5min.Add 500 μ L85wt% hydrazine hydrate solutions, at room temperature stir 4h.End product is through centrifugation, and deionized water-alcohol mixeding liquid washing, obtains the carbon black loadings platinum-nickel alloys nanometer electrical catalyst that graphite phase carbon nitride (30%) is modified after drying.
Embodiment 2: the preparation method of the carbon black loadings platinum-nickel alloys nanometer electrical catalyst that graphite phase carbon nitride of the present invention (50%) is modified, comprises the following steps:
The first step, with the first step in embodiment 1, drying obtains acid-treated carbon black;
Second step, by 500mg melamine and the acid-treated carbon black dispersion of 500mg in 22mL ethylene glycol;
3rd step, 66mL dust technology (0.12mol/L) is instilled the dispersion liquid of second step gained and stirs 1h, centrifugation, and ethanol washs 3 times, dry;
4th step, by the 3rd step gained melamine/black stock, calcines 1h, obtains graphite phase carbon nitride/carbon black compound in 350 DEG C of nitrogen atmospheres;
5th step, is distributed in 40mL ethylene glycol by graphite phase carbon nitride/carbon black compound 20mg, ultrasonic disperse 1h.22 μ L0.77mol/LPt (NO are instilled in dispersion liquid
3)
2solution, 18 μ L0.94mol/LPd (NO
3)
2solution, stirs 5min.Add 500 μ L85wt% hydrazine hydrate solutions, at room temperature stir 4h.End product is through centrifugation, and deionized water-alcohol mixeding liquid washing, obtains the carbon black loadings platinum-nickel alloys nanometer electrical catalyst that graphite phase carbon nitride (50%) is modified after drying.
In accompanying drawing 2 and accompanying drawing 3, XRD and the TEM characterization result of product proves successfully to have synthesized the carbon black loadings platinum-nickel alloys nanometer electrical catalyst that graphite phase carbon nitride is modified.The carbon black loadings platinum-nickel alloys nanometer electrical catalyst that the cyclic voltammogram proof graphite phase carbon nitride that in accompanying drawing 5, product catalyst is oxidized different alcohols is modified has the performance of the different alcohols of high catalytic oxidation.
Embodiment 3: the preparation method of the carbon black loadings platinum-nickel alloys nanometer electrical catalyst that graphite phase carbon nitride of the present invention (70%) is modified, comprises the following steps:
The first step, with the first step in embodiment 1, drying obtains acid-treated carbon black;
Second step, by 700mg melamine and the acid-treated carbon black dispersion of 300mg in 62.5mL ethylene glycol;
3rd step, 100mL dust technology (0.15mol/L) is instilled the dispersion liquid of second step gained and stirs 1h, centrifugation, and ethanol washs 3 times, dry;
4th step, by the 3rd step gained melamine/black stock, calcines 3h, obtains graphite phase carbon nitride/carbon black compound in 350 DEG C of nitrogen atmospheres;
5th step, is distributed in 40mL ethylene glycol by graphite phase carbon nitride/carbon black compound 20mg, ultrasonic disperse 1h.22 μ L0.77mol/LPt (NO are instilled in dispersion liquid
3)
2solution, 18 μ L0.94mol/LPd (NO
3)
2solution, stirs 5min.Add 500 μ L85wt% hydrazine hydrate solutions, at room temperature stir 4h.End product is through centrifugation, and deionized water-alcohol mixeding liquid washing, obtains the carbon black loadings platinum-nickel alloys nanometer electrical catalyst that graphite phase carbon nitride (70%) is modified after drying.
Graphite phase carbon nitride in accompanying drawing 4/carbon black compound resistance to electrochemical corrosion can cyclic voltammogram demonstrate carbon black through the rear stability of the modification of graphite phase carbon nitride and be improved, can effectively resist electrochemical corrosion effect.
Claims (6)
1. a preparation method for the carbon black loadings platinum-nickel alloys nanometer electrical catalyst of graphite phase carbon nitride modification, is characterized in that, comprise the following steps:
The first step, obtains acid-treated carbon black by carbon black hydrothermal treatment consists in red fuming nitric acid (RFNA);
Second step, by melamine and the stirring and dissolving dispersion in a solvent of acid-treated carbon black;
3rd step, instills second step gained dispersion liquid and stirs, is separated, obtains melamine/black stock with straight alcohol washing, drying by dust technology;
4th step, under nitrogen protection, calcines the 3rd step gained melamine/black stock, obtains graphite phase carbon nitride/carbon black compound at 300 ~ 400 DEG C;
5th step, by graphite phase carbon nitride/carbon black compound ultrasonic disperse in a solvent, add platinum nitrate solution, palladium nitrate solution, hydrazine hydrate solution successively, and stir, after reaction terminates, after centrifugation, washing, drying, obtain the carbon black loadings platinum-nickel alloys nanometer electrical catalyst that graphite phase carbon nitride is modified.
2. the preparation method of the carbon black loadings platinum-nickel alloys nanometer electrical catalyst of graphite phase carbon nitride modification as claimed in claim 1, it is characterized in that, in step one, described carbon black is Vulcan
xC-72R, carbon black and red fuming nitric acid (RFNA) mass ratio are 1:100 ~ 120, and the concentration of red fuming nitric acid (RFNA) is 68wt%; Heat treatment temperature is 120 DEG C; Heat treatment time is 8 ~ 12h; The reaction vessel that heat treatment adopts is teflon-lined stainless steel hydro-thermal counteracting tank, loading 50%.
3. the preparation method of the carbon black loadings platinum-nickel alloys nanometer electrical catalyst of graphite phase carbon nitride modification, it is characterized in that, in step 2, the mass ratio of described melamine and acid-treated carbon black is 4 ~ 0.5:1; Solvent select in deionized water and ethylene glycol any one, wherein the quality of water is 300 ~ 500 times of melamine, and the quality of ethylene glycol is 50 ~ 100 times of melamine.
4. the preparation method of the carbon black loadings platinum-nickel alloys nanometer electrical catalyst of graphite phase carbon nitride modification, it is characterized in that, in step 3, described dust technology concentration is 0.1 ~ 0.2mol/L, and the quality of dust technology is 100 ~ 150 times of melamine.
5. the preparation method of the carbon black loadings platinum-nickel alloys nanometer electrical catalyst of graphite phase carbon nitride modification, it is characterized in that, in step 4, described calcination time is 1 ~ 3h.
6. the preparation method of carbon black loadings platinum-nickel alloys nanometer electrical catalyst that modifies of graphite phase carbon nitride, is characterized in that, in step 5, one or more of deionized water, ethanol, ethylene glycol selected by described solvent; The concentration of platinum nitrate solution is 0.77mol/L, and the concentration of palladium nitrate solution is 0.94mol/L; The mass ratio of platinum nitrate, palladium nitrate and graphite phase carbon nitride/carbon black compound is 0.27:0.18:1, and hydrazine hydrate solution concentration is 85wt%, and the quality of hydrazine hydrate solution is 80 ~ 100 times of noble metal gross mass.
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| CN107634207A (en) * | 2017-09-19 | 2018-01-26 | 大连海事大学 | A kind of silicon mosaic redox graphene/graphite phase carbon nitride composite and its preparation and application |
| CN109216716A (en) * | 2018-08-06 | 2019-01-15 | 浙江高成绿能科技有限公司 | A kind of preparation method of the fuel cell Pt/C catalyst of high Pt carrying capacity |
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