CN105013475A - Mono-dispersed Pd-Pt nano-catalyst and preparation method therefor - Google Patents
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Abstract
The invention discloses a mono-dispersed Pd-Pt nano-catalyst and a preparation method therefor. According to the invention, with H2PtCl6.6H2O and PdCl2 as metal precursors, octa(amidocarboxyl silsesquioxane) as a protecting agent, and formaldehyde as a reducing agent, the mono-dispersed Pd-Pt nano-catalyst is prepared by a hydrothermal method. The prepared nano-catalyst has the advantages of good dispersing performance, higher electrochemical active specific surface area, and high electrocatalytic activity. The preparation provided by the invention is simple in required equipment and convenient in operation, and has great utilization value in a commercialization process of direct formic acid fuel cells.
Description
Technical field
The invention belongs to fuel cell catalyst technical field, relate to monodispersed Pt-Pd nanocatalyst and preparation method thereof.
Background technology
In recent years, due to the day by day loss of increase, the fossil fuel day by day of energy demand and the day by day serious of global environmental pollution, green energy resource and the energy transition equipment of exploitation efficient pollution-free have caused increasing concern.Fuel cell a kind of chemical energy is converted to the energy conversion of electric energy without burning, and having efficient, clean, the advantage such as startup fast, is the generation technology of the new type of continuous after hydroelectric generation, thermal power generation and nuclear energy power generation.Wherein, because formic acid is nontoxic, low to the infiltration of Nafion film, to store and transportation safety is convenient and high-energy-density, substitute with formic acid the extensive concern that direct methanoic acid fuel cell that methyl alcohol and hydrogen does fuel obtains scientific circles.But the commercial applications of aminic acid fuel battery is still had any problem: the utilization rate of mainly conventional platinum catalyst is low, expensive, easily poisoning.Therefore, in order to impel direct methanoic acid fuel cell to realize commercialization, a kind of anode catalyst efficiently of synthesis is crucial.
At present, bimetallic is prepared or trimetallic catalyst is considered to a kind of effective method improving pure pt utilization and electro catalytic activity.Wherein, due to its abundance and outstanding catalytic performance, palladium is considered to the replacer of most potentiality.And the atomic radius of palladium and platinum, electronegativity and lattice paprmeter are relatively, are easily reduced simultaneously.
In addition, the catalytic activity height of catalyst depends on dispersiveness and the active surface area of nano particle.Improve the decentralization of nano particle, the active site enriched can be obtained, and then the catalytic activity of catalyst and utilization rate are all increased.At present, great majority are prepared in the method for metal nanoparticle, usually use high molecular surfactant and high molecular polymer to improve the decentralization of nano particle.But in preparation process, high molecular polymer easily forms micelle, these micelles only have under given conditions could stable existence.Macromolecules adsorption, on the surface of nano particle, greatly reduces catalytic activity.Therefore, the key preparing the nano particle of high catalytic performance finds novel protective agent or stabilizing agent.In recent years, due to its good biocompatibility, high chemistry and heat endurance, large specific area, nontoxic corrosion resistance, polyhedral oligomeric silsesquioxane causes great concern in material science and catalyst application.The skeleton of silsesquioxane is Si-O-Si, Si-R is pendant group, and as amino, mercaptan, the different group such as carboxyl, can make silsesquioxane have different character like this.In Au and the Pd nano particle synthesis of high degree of dispersion, just use silsesquioxane and done stabilizing agent and protective agent.The application of silsesquioxane has following advantage: on the one hand, the silsesquioxane of different functional groups and the preparation method of silsesquioxane metal composite simple; On the other hand, silsesquioxane metal composite has good stability, easily departs from from solution, less to the performance impact of nano particle.The stabilizing agent of the people such as Li using silsesquioxane dendritic macromole as nano metal bunch, prepare stable finely dispersed Pt, Pd, Ru, Au metal nanometre cluster and PtPd, PtAu, PtAg alloy nanocluster catalyst, and study its high active of hydrogenation catalysis to aromatic aldehyde.
Summary of the invention
Technical problem: the invention provides electrochemically active specific surface area large, single dispersing Pt-Pd that electro catalytic activity is high, yardstick be the nanocatalyst of 3-20nm, provides its preparation method simultaneously.
Technical scheme: the preparation method of monodispersed Pt-Pd nanocatalyst of the present invention, comprises the following steps:
(1) metal precursor chloroplatinic acid and palladium bichloride are dissolved in ultra-pure water, again stabilizing agent eight acid amides acidic group silsesquioxane is added above-mentioned solution, sonic oscillation, magnetic agitation makes stabilizing agent fully contact complexing with Pd ion with Pt ion, obtain active metal presoma mixed liquor, wherein metal precursor molal quantity is the molal quantity sum of palladium bichloride and chloroplatinic acid;
(2) the active metal presoma mixed liquor of described step (1) gained is transferred in hydrothermal reaction kettle, adds formalin, at 100 ~ 180 DEG C, react 6 ~ 12h;
(3) described step (2) products therefrom is added ultra-pure water centrifuge washing repeatedly, drier in vacuum desiccator.
Further, the Pt element of metal precursor and Pd elemental mole ratios are 1:1 ~ 10 in described step (1).
Further, the mol ratio of metal precursor and eight acid amides acidic group silsesquioxanes is 1:1 ~ 6, and the molal quantity of described metal precursor is wherein Pt element and Pd element molal quantity summation.
Further, in described step (2), in formaldehyde and step (1), the volume ratio of ultra-pure water used is 1:1 ~ 6.
Further, in described step (1), pH value to 3 ~ 11 of mixed liquor after sonic oscillation, are regulated.
In the preferred version of the inventive method, in step (1), use hydrochloric acid or NaOH adjust ph.
Monodispersed Pt-Pd nanocatalyst of the present invention, prepares according to the method described above.
The monodispersed Pt-Pd nanocatalyst that eight acid amides acidic group silsesquioxanes of the present invention are stable, in Pd and the Pt metal precursor aqueous solution, add stabilizing agent eight acid amides acidic group silsesquioxane, then the Viability metal precursor mixed liquor of this mixed solution complexing under ultrasound condition, with after to obtain after reduction, centrifugal, drying, the mol ratio of described metal precursor and silsesquioxane is 1:1 ~ 6.
In the preferred version of the monodispersed Pt-Pd nanocatalyst that eight acid amides acidic group silsesquioxanes of the present invention are stable, the pH value of metal precursor mixed liquor is 3 ~ 11.
In the preferred version of the monodispersed Pt-Pd nanocatalyst that a kind of eight acid amides acidic group silsesquioxanes of the present invention are stable, this catalyst prepares according to said method.
The present invention is monodispersed, yardstick is the application of 3-20nm Pt-Pd nanocatalyst in formic acid electro-catalysis, improves 5-6 doubly compared to commercial catalysts catalytic performance.
The present invention is with eight acid amides acidic group silsesquioxanes for stabilizing agent, and take formaldehyde as reducing agent, prepare monodispersed Pt-Pd nanocatalyst by hydrothermal method, catalyst particle size is distributed between 3-20nm; In single dispersing Pt-Pd nanocatalyst Pt, Pd, Si mass ratio be (20-75): (15-50): (1-10).Catalyst of the present invention has huge application prospect in direct methanoic acid fuel cell anode catalyst.
Beneficial effect: the present invention compared with prior art, has the following advantages:
(1) the present invention's surfactant of not using polyvinylpyrrolidone (PVP) affecting catalytic activity etc. traditional, and make stabilizing agent with eight acid amides acidic group silsesquioxanes, prepare monodispersed Pt-Pd nanocatalyst by simple hydro-thermal method.
(2) the monodispersed Pt-Pd nanocatalyst prepared not only increases the utilization rate of fuel battery anode catalyst, and high degree improves the catalytic performance of catalyst.
Three kinds of monodispersed Pt-Pd nanocatalysts provided by the present invention, with business Pt/C catalyst and other patterns Pt-Pd catalyst (Wang, Chemistry ofMaterials, 2009) compare, in catalysis formic acid electro-oxidation process, monodispersed Pt-Pd nanocatalyst has lower oxidizing potential (-0.14V), higher catalytic activity (catalytic activity improves 5-6 doubly) and outstanding resisting CO poisoning ability.This is because after introducing Pd atom formation Pt-Pd nanocatalyst, through the redistribution of Pt and Pd atom, continuous print Pt can be kept apart, reduce CO
adsadsorbance on Pt, what promote the direct oxidation of formate dehydrogenase approach and suppress formic acid dehydration approach connects oxidation indirectly, thus improves the activity of formic acid catalytic oxidation.Use eight acid amides acidic group silsesquioxanes as the stabilizing agent of Pt-Pd nanocatalyst and protective agent in the present invention first; wherein; nitrogen in eight acid amides acidic group silsesquioxanes and oxygen can interact with metal precursor; and; this interaction can weaken the rate of reduction of metal precursor, thus improves the decentralization of nano material.Zhou (Zhou, Mater.Chem.Phys, 2010) has reported using eight aniline ethanedioic acid base silsesquioxanes as macromolecule dispersant, has synthesized a kind of Pt nanocatalyst that can be recycled of novelty.The Pt nano particle generation self aggregation of preparation can be made by the pH value changing solution system and disperse again.When the pH value of working environment is greater than 4.0, Pt nano particle is dispersed; When the pH value of working environment is less than 2.5, Pt nano particle generation self aggregation.And electroxidation experimental result shows that Pt nanoparticle shows outstanding catalytic performance as recycling catalyst, has potential value in industrial applications.Be used for preparing the catalyst of olefinic polymerization and organic epoxidation reaction.Eight acid amides acidic group silsesquioxanes make as stabilizing agent and protective agent, and nano material preparation process can be made simple; In addition, after having prepared, compare other polymeric complexing agents, eight acid amides acidic group silsesquioxanes are easier to be separated from solution, even if there is portion of residual, the impact of its catalytic performance on catalyst is less, and has the advantage such as good biocompatibility, high chemistry and heat endurance, large specific area, nontoxic corrosion resistance due to eight acid amides acidic group silsesquioxanes, in fuel cell operations, avoid the reduction of the catalytic activity using the corrosion of business Pt/C catalyst to cause.
Accompanying drawing explanation
Fig. 1 is the electron microscope picture of single dispersing Pt1Pd1 nano particle in embodiment 1.
Fig. 2 be in embodiment 1 single dispersing Pt1Pd1 nano particle at 0.5mol/LH
2sO
4the cyclic voltammetry curve of electro-catalysis formic acid in+0.5mol/L HCOOH solution.
Fig. 3 is the electron microscope picture of single dispersing Pt1Pd5 nano particle in embodiment 2.
Fig. 4 is that embodiment 2 single dispersing Pt1Pd5 nano particle is at 0.5mol/LH
2sO
4the cyclic voltammetry curve of electro-catalysis formic acid in+0.5mol/L HCOOH solution.
Fig. 5 is the electron microscope picture of single dispersing Pt1Pd10 nano particle in embodiment 3.
Fig. 6 be in embodiment 3 single dispersing Pt1Pd10 nano particle at 0.5mol/LH
2sO
4the cyclic voltammetry curve of electro-catalysis formic acid in+0.5mol/L HCOOH solution.
Detailed description of the invention
Below in conjunction with embodiment and Figure of description, the present invention is further illustrated.
The preparation of embodiment 1, single dispersing Pt1Pd1 nano particle
Get the mixed liquor (first formaldehyde and water volume ratio are 1:1) that chloroplatinic acid and palladium bichloride (platinum palladium mol ratio is 1:1) are dissolved in formaldehyde and water; Eight acid amides acidic group silsesquioxanes (mol ratio of metal precursor and eight acid amides acidic group silsesquioxanes is 1:1) are added again in above-mentioned solution, 5mol/L sodium hydroxide solution is used to regulate the pH value to 11 of above-mentioned mixed liquor after sonic oscillation, keep stirring to make stabilizing agent fully contact complexing with Pd ion with Pt ion, obtain active metal presoma mixed liquor; Be transferred in hydrothermal reaction kettle by the material liquid of preparation, reaction temperature is 180 DEG C, and the reaction time is 6h; By the product ultra-pure water repeatedly eccentric cleaning after reduction, then in vacuum desiccator dry (60 DEG C), gained solid product is the Pt-Pd nanocatalyst that is uniformly dispersed.
The preparation of embodiment 2, single dispersing Pt1Pd5 nano particle
Get the mixed liquor (first formaldehyde and water volume ratio are 1:6) that chloroplatinic acid and palladium bichloride (platinum palladium mol ratio is 1:5) are dissolved in formaldehyde and water; Eight acid amides acidic group silsesquioxanes (mol ratio of metal precursor and eight acid amides acidic group silsesquioxanes is 1:6) are added again in above-mentioned solution, 5mol/L hydrochloric acid or 5mol/L sodium hydroxide solution is used to regulate the pH value to 7 of above-mentioned mixed liquor after sonic oscillation, keep stirring to make stabilizing agent fully contact complexing with Pd ion with Pt ion, obtain active metal presoma mixed liquor; Be transferred in hydrothermal reaction kettle by the material liquid of preparation, reaction temperature is 100 DEG C, and the reaction time is 9h; By the product ultra-pure water repeatedly eccentric cleaning after reduction, then in vacuum desiccator dry (60 DEG C), gained solid product is the Pt-Pd nanocatalyst that is uniformly dispersed.
The preparation of embodiment 3, single dispersing Pt1Pd10 nano particle
Get the mixed liquor (first formaldehyde and water volume ratio are 1:3) that chloroplatinic acid and palladium bichloride (platinum palladium mol ratio is 1:10) are dissolved in formaldehyde and water; Eight acid amides acidic group silsesquioxanes (mol ratio of metal precursor and eight acid amides acidic group silsesquioxanes is 1:3) are added again in above-mentioned solution, 5mol/L hydrochloric acid or 5mol/L sodium hydroxide solution is used to regulate the pH value to 3 of above-mentioned mixed liquor after sonic oscillation, keep stirring to make stabilizing agent fully contact complexing with Pd ion with Pt ion, obtain active metal presoma mixed liquor; Be transferred in hydrothermal reaction kettle by the material liquid of preparation, reaction temperature is 140 DEG C, and the reaction time is 12h; By the product ultra-pure water repeatedly eccentric cleaning after reduction, then in vacuum desiccator dry (60 DEG C), gained solid product is the Pt-Pd nanocatalyst that is uniformly dispersed.
Embodiment 1,2,3 gained catalyst is carried out high resolution transmission electron microscopy, and its result is as shown in Fig. 1, Fig. 3, Fig. 5.
A certain amount of single dispersing Pt-Pd nanocatalyst is scattered in ultra-pure water, getting 5ul sample drop at diameter is on 3mm glass-carbon electrode, after drying completely under room temperature, the Nafion dissolution homogeneity getting 2ul is coated on catalyst surface, and namely room temperature can be used as working electrode and use after drying.
By embodiment 1,2,3 gained catalyst electrode and business Pt/C catalyst at 0.5mol/LH
2sO
4in+0.5mol/LHCOOH solution, the cyclic voltammetry curve of electro-catalysis formic acid is as Fig. 2,4,6.
From Fig. 1,3,5, can find out single dispersing Pt-Pd nanocatalyst respectively, and distribution of particles is relatively uniform, overall dimensions is respectively 7.5 ± 2nm, 9.5 ± 2nm, 13.0 ± 2nm.
From Fig. 2,4,6, good all than business Pt/C catalyst of the formic acid electro catalytic activity of single dispersing Pt-Pd nanocatalyst can be found out respectively, and maximum peak current density is 1.02Amg
-1, 0.94Amg
-1, 0.83Amg
-1.
Above-described embodiment is only the preferred embodiment of the present invention; be noted that for those skilled in the art; under the premise without departing from the principles of the invention; some improvement and equivalent replacement can also be made; these improve the claims in the present invention and are equal to the technical scheme after replacing, and all fall into protection scope of the present invention.
Claims (6)
1. a preparation method for monodispersed Pt-Pd nanocatalyst, is characterized in that: the method comprises the following steps:
(1) metal precursor chloroplatinic acid and palladium bichloride are dissolved in ultra-pure water, again stabilizing agent eight acid amides acidic group silsesquioxane is added above-mentioned solution, sonic oscillation, magnetic agitation makes stabilizing agent fully contact complexing with Pd ion with Pt ion, obtain active metal presoma mixed liquor, wherein metal precursor molal quantity is the molal quantity sum of palladium bichloride and chloroplatinic acid;
(2) the active metal presoma mixed liquor of described step (1) gained is transferred in hydrothermal reaction kettle, adds formalin, at 100 ~ 180 DEG C, react 6 ~ 12h;
(3) described step (2) products therefrom is added ultra-pure water centrifuge washing repeatedly, drier in vacuum desiccator.
2. the monodispersed Pt-Pd nanocatalyst that eight acid amides acidic group silsesquioxanes according to claim 1 are stable, is characterized in that: Pt element and the Pd elemental mole ratios of the middle metal precursor of described step (1) are 1:1 ~ 10.
3. the monodispersed Pt-Pd nanocatalyst that eight acid amides acidic group silsesquioxanes according to claim 1 are stable, it is characterized in that: the mol ratio of described metal precursor and eight acid amides acidic group silsesquioxanes is 1:1 ~ 6, the molal quantity of described metal precursor is wherein Pt element and Pd element molal quantity summation.
4. the monodispersed Pt-Pd nanocatalyst that eight acid amides acidic group silsesquioxanes according to claim 1,2 or 3 are stable, it is characterized in that: in described step (2), in formaldehyde and step (1), the volume ratio of ultra-pure water used is 1:1 ~ 6.
5. the monodispersed Pt-Pd nanocatalyst that eight acid amides acidic group silsesquioxanes according to claim 1,2 or 3 are stable, is characterized in that: in described step (1), regulate pH value to 3 ~ 11 of mixed liquor after sonic oscillation.
6. a monodispersed Pt-Pd nanocatalyst, is characterized in that, this catalyst prepares according to method described in claim 1,2,3,4 or 5.
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Cited By (6)
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| CN106450359A (en) * | 2016-12-08 | 2017-02-22 | 天津工业大学 | Preparation method of oxide@ precious metal core-shell nanowire catalyst |
| CN107887619A (en) * | 2017-10-27 | 2018-04-06 | 北京航天动力研究所 | A kind of Pt Pd alloy catalysts of morphology controllable and preparation method and application |
| CN109289840A (en) * | 2018-10-15 | 2019-02-01 | 天津工业大学 | A kind of preparation method of the network-like palladium nano chain catalyst of methanol electro-oxidizing |
| CN113909487A (en) * | 2021-11-05 | 2022-01-11 | 南京师范大学 | Curled PtPd nano dendrite and preparation method and application thereof |
| CN113948729A (en) * | 2021-10-20 | 2022-01-18 | 江苏大学 | Preparation method of binary metal platinum-palladium prismatic catalyst and application of catalyst in direct methanol fuel cell |
| CN116273051A (en) * | 2023-03-21 | 2023-06-23 | 榆林学院 | Gamma-Al 2 O 3 Supported ruthenium-nickel catalyst and application thereof in phenol hydrogenation reaction |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106450359A (en) * | 2016-12-08 | 2017-02-22 | 天津工业大学 | Preparation method of oxide@ precious metal core-shell nanowire catalyst |
| CN106450359B (en) * | 2016-12-08 | 2019-12-31 | 天津工业大学 | Preparation method of oxide @ noble metal core-shell nanowire catalyst |
| CN107887619A (en) * | 2017-10-27 | 2018-04-06 | 北京航天动力研究所 | A kind of Pt Pd alloy catalysts of morphology controllable and preparation method and application |
| CN107887619B (en) * | 2017-10-27 | 2020-05-08 | 北京航天动力研究所 | Morphology-controllable Pt-Pd alloy catalyst and preparation method and application thereof |
| CN109289840A (en) * | 2018-10-15 | 2019-02-01 | 天津工业大学 | A kind of preparation method of the network-like palladium nano chain catalyst of methanol electro-oxidizing |
| CN113948729A (en) * | 2021-10-20 | 2022-01-18 | 江苏大学 | Preparation method of binary metal platinum-palladium prismatic catalyst and application of catalyst in direct methanol fuel cell |
| CN113909487A (en) * | 2021-11-05 | 2022-01-11 | 南京师范大学 | Curled PtPd nano dendrite and preparation method and application thereof |
| CN113909487B (en) * | 2021-11-05 | 2023-08-25 | 南京师范大学 | Coiled PtPd nano dendrite and preparation method and application thereof |
| CN116273051A (en) * | 2023-03-21 | 2023-06-23 | 榆林学院 | Gamma-Al 2 O 3 Supported ruthenium-nickel catalyst and application thereof in phenol hydrogenation reaction |
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