CN109277103A - A kind of high activity platinum bimetallic liberation of hydrogen catalyst and preparation method thereof - Google Patents
A kind of high activity platinum bimetallic liberation of hydrogen catalyst and preparation method thereof Download PDFInfo
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- CN109277103A CN109277103A CN201811466756.XA CN201811466756A CN109277103A CN 109277103 A CN109277103 A CN 109277103A CN 201811466756 A CN201811466756 A CN 201811466756A CN 109277103 A CN109277103 A CN 109277103A
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- catalyst
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8926—Copper and noble metals
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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
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
Abstract
The present invention relates to nano materials and catalysis technique crossing domain, disclose a kind of platinum bimetallic nanocatalyst of controllable structure and preparation method thereof for electrocatalytic hydrogen evolution reaction.In the method, with Pt (acac)2And CuCl2•2H2O is presoma, using simple liquid phase synthesizing method, restores to obtain the platinoid bimetal nano catalyst of different component using reducing agent.The size of the platinoid bimetal nano catalyst is 8 ~ 15nm, and unique pattern exposes a large amount of active site, compared with business Pt/C, shows smaller overpotential, Tafel slope and excellent cyclical stability.Platinoid bimetal nano crystalline substance is as electrolysis water evolving hydrogen reaction catalyst, and catalytic activity is high, and dosage is few, greatly enhances platinum utilization and alleviates energy crisis, keeps it following and is producing hydrogen field with preferable development prospect.
Description
Technical field
It is the present invention relates to nano material synthesis and electrolysis water liberation of hydrogen technical field, in particular to a kind of to be closed with simple liquid phase method
At the technology of platinum bimetallic liberation of hydrogen catalyst.
Background technique
As fossil fuel is increasingly exhausted, global warming and environmental pollution are got worse, and are explored and are tapped a new source of energy and compel
The eyebrows and eyelashes.Hydrogen causes the research interest of researchers as a kind of cleaning, renewable energy.Water electrolysis hydrogen production is to realize greatly
The main path of scale production hydrogen.Energy consumption is the greatest problem of water electrolysis hydrogen production at present, and it is most effective to solve energy consumption problem
Method is exactly to reduce cathode hydrogen evolution overpotential.Therefore, it is significant to develop new and effective hydrogen-precipitating electrode catalyst.
The hydrogen adsorption energy △ G of precious metals ptHIt is almost nil, it is considered to be ideal liberation of hydrogen material.But Pt resource is deficient
It is weary and expensive, constrain its commercialized development.At this stage, Pt based nano-material is still irreplaceable liberation of hydrogen catalysis
Agent.The development target of catalyst is the dosage that catalyst is reduced while guaranteeing its catalytic activity, stability and service life.
To solve the above-mentioned problems, method the most effective is exactly by transition metal (such as Fe, Co, Ni, Cu) part substitution Pt system
Standby metallic nano crystal in pairs, not only can improve the utilization rate of Pt, can also improve the catalytic activity of catalyst.Study table
It is bright, regulated and controled by size, component, the surface texture etc. to Pt base nanometer crystal, the key for influencing catalytic performance can be found
Factor, to improve its electrocatalysis characteristic [Bimetallic nanocrystals:syntheses, properties, and
applications, Chem. Rev. 2016, 116, 10414−10472；Nanocatalysts for hydrogen
Evolution reactions, Phys. Chem. Chem. Phys. 2018,20,6,777 6799].
Utilization rate and stability of the Pt base nanometer crystal in electrocatalytic reaction are how effectively improved, is the heat in electro-catalysis field
Point problem.Size, component and surface texture due to Pt base nanometer crystal etc. are closely related with its electrocatalytic properties, as long as finding it
Crucial influence factor, so that it may which the liberation of hydrogen catalysis to design new and effective provides new approaches.
Summary of the invention
The present invention provides a kind of particle size uniformity, high dispersive from the electrocatalysis characteristic for improving Pt base nanometer crystal
Property, high activity, simple process, the preparation method of easy to operate electrolysis aquatic products hydrogen catalyst.Pt and transition metal Cu phase are tied
It closes and the Pt-Cu bimetal nano crystalline substance with good dispersion is prepared using simple liquid phase synthesizing method, and the material is used as
Evolving hydrogen reaction catalyst shows excellent catalytic effect.
Pt-Cu nanocrystalline material proposed by the present invention is made by liquid phase synthesizing method.By regulation presoma platinum salt and
Molar ratio and oleyl amine, the volume ratio of oleic acid mixed solvent of mantoquita, can be nanocrystalline with the rich defective Pt-Cu of synthetic surface.
The material for electro-catalysis produce hydrogen when, have lesser overpotential and good cyclical stability, method have it is easy to operate,
Safety non-pollution, it is high-efficient the advantages that.
Pt-Cu proposed by the present invention it is nanocrystalline the preparation method is as follows:
1, with Pt (acac)2, CuCl2•2H2O is presoma, and glucose is reducing agent, oleyl amine and oleic acid as solvent, by 5.0-
10.0 mg Pt(acac)2With 25.0-50.0 mg CuCl2•2H2O is dissolved in the mixed solvent of 5.0-10.0 mL oleic acid and oleyl amine
In, obtain glaucous mixed solution.
2, by after glaucous mixed solution ultrasound 10-30 min, 180 oCAfter stirring 10-240 min under the conditions of oil bath
Form uniform black suspension.
3, it by mixed solution centrifuge washing 3-5 times of suspension hexamethylene obtained by previous step and dehydrated alcohol, then puts
Enter 55-65 in vacuum oven oCDry 6-12 h, it is brilliant to finally obtain Pt-Cu bimetal nano.
Pass through X-ray powder diffraction instrument (XRD), transmission electron microscope (TEM) and inductively coupled plasma spectrometry generator
(ICP-MS) component, the characterization of object phase and pattern are carried out to obtained Pt-Cu bimetal nano crystalline substance respectively, then passes through electrification
Test is learned, its Hydrogen Evolution Performance is evaluated.
Detailed description of the invention
Fig. 1 is obtained PtCu1.8The TEM photo of sample.
Fig. 2 is obtained PtCu1.8The XRD curve of sample.
Fig. 3 is obtained PtCu1.6The TEM photo of sample.
Fig. 4 is obtained PtCu1.6The XRD curve of sample.
The PtCu of Fig. 5 different condition preparation1.8、PtCu1.6Bimetal nano is brilliant and business Pt/C is in 0.5 M sulfuric acid solution
The middle polarization curve for carrying out evolving hydrogen reaction.
The PtCu of Fig. 6 different condition preparation1.8、PtCu1.6Bimetal nano is brilliant and business Pt/C is in 0.5 M sulfuric acid solution
The middle Tafel curve for carrying out evolving hydrogen reaction.
Specific embodiment
The present invention is clearly and completely described below in conjunction with specific embodiment in the present invention, it is clear that described
Embodiment is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, other are to this
What modification was made in invention equally falls into claims of the present invention limited range.
Embodiment 1
In 20 mL vials, by 10 mg Pt (acac)2、50 mg CuCl2•2H2O and 60 mg glucose are dissolved in 4 mL oil
The in the mixed solvent of acid and 6 mL oleyl amines, obtains glaucous mixed solution.Then 30 min of ultrasonic treatment, 180oC oil bath
After 240 min of middle stirring, stops heating, drop to room temperature to product, the mixing of gained precipitating hexamethylene and dehydrated alcohol is molten
Agent is washed three times, is then placed in 60 in vacuum ovenoC dries 6 h, and it is brilliant to finally obtain Pt-Cu bimetal nano.
By X-ray powder diffraction instrument (XRD) and transmission electron microscope (TEM) respectively to the object phase and shape of resulting materials
Looks are characterized, and discovery product is that petal-like Pt-Cu bimetal nano is brilliant, having a size of 10-15 nm.According to X-ray energy spectrum point
Analyzer (EDX) and inductively coupled plasma spectrometry generator (ICP-MS) test display atomic ratio are 1:1.8.Electro-catalysis
Evolving hydrogen reaction test discovery PtCu1.8It is nanocrystalline active with excellent evolving hydrogen reaction.
Embodiment 2
CuCl in mixed solution2•2H2The quantitative change of O is 25 mg, remaining is the same as embodiment 1.
By X-ray powder diffraction instrument (XRD) and transmission electron microscope (TEM) respectively to the object phase and shape of resulting materials
Looks are characterized, and discovery product is brilliant in the Pt-Cu bimetal nano of caged decahedron pattern, having a size of 9-12 nm.It is penetrated according to X
Line energy depressive spectroscopy (EDX) and inductively coupled plasma spectrometry generator (ICP-MS) test display atomic ratio are 1:
1.6.Electrocatalytic hydrogen evolution reaction test finds PtCu1.6It is nanocrystalline active with excellent evolving hydrogen reaction.
The test of electrochemistry liberation of hydrogen is as follows: the test of electrocatalysis characteristic involved in this research is all made of three-electrode system, wherein
(diameter is 5 mm to glass-carbon electrode, and area is 0.1963 cm2) it is working electrode, carbon-point is to electrode, and Ag/AgCl electrode is
Reference electrode.Used electrolyte is the sulfuric acid solution of 0.5 M, it is all test nitrogen saturation sulfuric acid solution in into
Row.
It in 30 mL bottles, disperses 20 mg conductive blacks (Vulcan XC-72) in 20 mL ethyl alcohol, is added 2
Mg Pt-Cu bimetal nano is brilliant, and 20 min of ultrasound are well dispersed in it on conductive black, and 36 h are stirred at room temperature, institute
Black suspension is obtained to be centrifugated with ethanol washing.
In order to remove the oleyl amine oleic acid solvent of resulting materials surface residual, the active material for being supported on conductive black is dispersed
In 30 mL acetums, in 80o12 h of return stirring under C.It is cooled to room temperature, three times with a large amount of ethanol washings, true
60 in empty drying boxoC dries 8 h.
Nafion solution, 735 μ L deionized waters and the 365 μ L for weighing above-mentioned sample addition 20 μ L, the 5 wt % of 5 mg are different
In propyl alcohol, ultrasonic 1 H-shaped is at the uniform dispersion of black, and wherein Nafion can effectively improve the dispersibility of sample and by sample
It is fixed on glassy carbon electrode surface.
The preparation of working electrode: first by glass-carbon electrode with 0.05 μm of Al2O3Polishing powder polishes 2 on polishing cloth
Min, then it is cleaned by ultrasonic 5 ~ 10 s in deionized water, it is demarcated in potassium ferricyanide solution, makes its potential difference less than 80
MV obtains drying after bright mirror surface spare.The catalyst dispersion drop of 10 μ L is drawn in polished glass carbon electricity with liquid-transfering gun
Pole surface, at room temperature naturally dry.In order to further remove the oleyl amine oleic acid of surface remnants, active object will be dripped after drying
The glass-carbon electrode of matter, which is placed under ultraviolet lamp, irradiates 10 h, and electrode and ultraviolet lamp tube about 0.5 cm of distance, wavelength are 254 nm.
High activity Pt-Cu bimetal nano partial crystallization hydrogen catalyst preparation method provided by the invention is simple, reduces production
Cost further improves the utilization rate of Pt, and alleviates crisis of resource, this is reacted for Pt based nano-material in electrocatalytic hydrogen evolution
In application provide a paths.
Claims (6)
1. a kind of high activity platinum bimetallic nanocrystalline hydrogen evolution catalyst, the catalyst have the property that
(1) main component of high activity platinum bimetallic nanocrystalline hydrogen evolution catalyst is that platinoid bimetal nano is brilliant；
(2) catalyst is black solid powder；
(3) content of Pt is 0.6-1 wt % in high activity platinum bimetallic nanocrystalline hydrogen evolution catalyst；
(4) high activity platinum bimetallic nanocrystalline hydrogen evolution catalyst can be saved for a long time in hexamethylene without settling, and
Its object phase and pattern do not change.
2. it is characterized in that the preparation method is as follows:
(1) with Pt (acac)2, CuCl2•2H2O is presoma, and glucose is reducing agent, and oleic acid and oleyl amine are solvent, by Pt
(acac)2, CuCl2•2H2O and glucose are dissolved in the in the mixed solvent of oleic acid and oleyl amine, obtain glaucous mixed solution；
(2) by after 30 min of glaucous mixed solution ultrasound, uniform black suspension is formed after heating stirring in oil bath
Liquid；
(3) by suspension hexamethylene obtained by previous step and dehydrated alcohol mixed solution centrifuge washing, it is dry to be then placed in vacuum
It is dry in dry case, it is brilliant to finally obtain Pt-Cu bimetal nano.
3. Pt-Cu bimetal nano as claimed in claim 2 is brilliant, it is characterised in that step (1) described Pt (acac)2Dosage is
5.0-10.0 mg, CuCl2•2H2O dosage is 25.0-50.0 mg, and oleic acid and oleyl amine dosage are respectively 1-9 and 1-9 mL.
4. Pt-Cu bimetal nano as described in claim 1 is brilliant, it is characterised in that step (2) the oil bath heating temperature is
170-180 oC, mixing time are 10-240 min.
5. Pt-Cu bimetal nano as claimed in claim 2 is brilliant, it is characterised in that step (3) hexamethylene and anhydrous second
Alcohol washing times are respectively 3-5 times, drying temperature 55-65oC, drying time are 6-12 h.
6. Pt-Cu bimetal nano as claimed in claim 2 is brilliant, the application in electrolysis water evolving hydrogen reaction.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110064406A (en) * | 2019-05-24 | 2019-07-30 | 扬州大学 | A kind of alkaline solution Electrocatalytic Activity for Hydrogen Evolution Reaction agent V2O3- NiPt and its preparation method and application |
| CN113818044A (en) * | 2021-09-29 | 2021-12-21 | 西安交通大学 | Preparation method of PtCu alloy catalyst for efficient electrocatalytic synthesis of ammonia |
| CN115094474A (en) * | 2022-06-23 | 2022-09-23 | 中山大学 | BiVO 4 Synthesis method of/PtNi nanowire and application of PtNi nanowire in seawater electrolysis hydrogen production |
| CN116765414A (en) * | 2023-06-17 | 2023-09-19 | 永氢(常州)能源科技有限公司 | Osmium metal alkene material, preparation method and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110064406A (en) * | 2019-05-24 | 2019-07-30 | 扬州大学 | A kind of alkaline solution Electrocatalytic Activity for Hydrogen Evolution Reaction agent V2O3- NiPt and its preparation method and application |
| CN110064406B (en) * | 2019-05-24 | 2021-11-23 | 扬州大学 | Alkaline solution hydrogen evolution electrocatalyst V2O3-NiPt and preparation method and application thereof |
| CN113818044A (en) * | 2021-09-29 | 2021-12-21 | 西安交通大学 | Preparation method of PtCu alloy catalyst for efficient electrocatalytic synthesis of ammonia |
| CN113818044B (en) * | 2021-09-29 | 2022-10-25 | 西安交通大学 | Preparation method of PtCu alloy catalyst for efficient electrocatalytic synthesis of ammonia |
| CN115094474A (en) * | 2022-06-23 | 2022-09-23 | 中山大学 | BiVO 4 Synthesis method of/PtNi nanowire and application of PtNi nanowire in seawater electrolysis hydrogen production |
| CN115094474B (en) * | 2022-06-23 | 2023-04-28 | 中山大学 | BiVO (binary organic acid) 4 Synthesis method of PtNi nanowire and application of PtNi nanowire in electrolysis of seawater hydrogen |
| CN116765414A (en) * | 2023-06-17 | 2023-09-19 | 永氢(常州)能源科技有限公司 | Osmium metal alkene material, preparation method and application thereof |
| CN116765414B (en) * | 2023-06-17 | 2024-01-26 | 永氢(江苏)能源科技有限公司 | Osmium metal alkene material, preparation method and application thereof |
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