CN108043423A - A kind of method for preparing platinum-nickel alloy catalyst - Google Patents
A kind of method for preparing platinum-nickel alloy catalyst Download PDFInfo
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- CN108043423A CN108043423A CN201711377594.8A CN201711377594A CN108043423A CN 108043423 A CN108043423 A CN 108043423A CN 201711377594 A CN201711377594 A CN 201711377594A CN 108043423 A CN108043423 A CN 108043423A
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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
- B01J23/892—Nickel and noble metals
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/342—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electric, magnetic or electromagnetic fields, e.g. for magnetic separation
Abstract
The present invention relates to a kind of method for preparing platinum-nickel alloy catalyst, including:Carbon-supported metal nano nickel particles are prepared with hydro-thermal method, it under certain magnetic field condition, is allowed to be chemically reacted with platinum acid chloride solution, utilizes the nickle atom of acid solution removal reaction-ure surface remnants, by centrifugation, filtering, drying the step of, obtain platinum-nickel alloy catalyst.The present invention prepares platinum-nickel alloy catalyst under magnetic fields using chemical deposition, and the content of noble metal platinum is high in platinum-nickel alloy catalyst prepared by such method, and catalytic performance is good.Compared with modern technologies, by influence of the magnetic field to platinum-nickel alloy forming core and growth course, the purpose that the platinum-nickel alloy catalyst with preferable catalytic activity is prepared under magnetic field is realized.
Description
Technical field
The present invention relates to platinum-nickel alloy catalyst material fabricating technology field, a kind of particularly platinum-nickel alloy for preparing is urged
The method of agent.
Background technology
Pt is widely used in the every field such as chemical industry, the energy and medicine as a kind of catalyst.But Pt metal is rare,
It is expensive, it restricts its application.For example, the fuel cell car of current 100 kW needs the metal of about 100g
Pt;And Pt metal explored reserves in the earth's crust are only 39000t.The scarcity of Pt metal determines fuel cell car
Cost will necessarily rise as it is widely popularized.Therefore, studying various low Pt or non-Pt catalyst has important meaning
Justice.At present, people develop various binary and ternary Pt alloy catalysts, such as Pt-Ni, Pt-Pd, Pt-Au, Pt-Ag-Au and
Pt-Fe alloys, but alloying metal is easy to run off in acid condition in such catalyst, so that alloy catalyst stability drops
It is low.Meanwhile people also begin to study other base metals Pt catalyst, such as carbide, oxide, nitrogen oxides, carbonitride
Deng, but so far, the catalytic performance of such no-Pt catalyst is all not as good as Pt catalyst.Therefore, exploitation is a kind of passes through reduction pair
The dependence of Pt, while lower-cost catalyst is of great significance.
In recent years the study found that can by being rationally designed on nanoscale to the structure of metal catalyst particles,
To change the physicochemical properties of metallic catalyst, the acquisition better catalyst of performance.Wherein nuclear shell structure nano metallic particles
With special electronic structure and surface nature, thus the application in fields such as catalysis is paid more and more attention, using Pt as shell structure
Catalyst can not only improve the catalytic activity of catalyst, the usage amount of Pt can also be reduced.Therefore, study using Pt as shell
Core-shell Structure Nanoparticles arouse widespread concern.
In metal material preparation process, the energy of high intensity can be contactlessly transferred to the atom ruler of substance by magnetic field
The behaviors such as degree or even the migration, matching and arrangement that directly affect atom in material, molecule, ion or crystal grain, so as to metal material
Material generates significant impact, realizes the preparation and modification of new material.Steady magnetic field mainly has two big effects in material preparation:One
It is that magnetic field generates MHD effect control fluid flowing by Lorentz force;Second is that the orientation effect in magnetic field, magnetic field can
Homogeneous orientation effect is integrally generated to material;The magnetic field intensity in magnetic field, magnetic direction are easy to control, and have flexibility;Therefore
The nano-catalyst material for preparing different Pt shell thicknesses can be realized by the regulation and control to high-intensity magnetic field.
The content of the invention
The object of the present invention is to provide a kind of methods for preparing platinum-nickel alloy catalyst.Technical solution is as follows:
A kind of method for preparing platinum-nickel alloy catalyst, including:
(a)Carbon-supported metal nano nickel particles are prepared using carbon carrier;
(b)The carbon-supported metal nano nickel particles are put into platinum acid chloride solution, and magnetic field is added to make the carbon-supported metal nickel nanometer
Particle is reacted with the platinum acid chloride solution, obtains platinum-nickel alloy reactant;
(c)The impurity of the platinum-nickel alloy reaction-ure surface is removed, it is post-treated to obtain platinum-nickel alloy catalyst.
The step(a)It is middle that the carbon-supported metal nano nickel particles are prepared using hydro-thermal method.
The step(a)In the carbon carrier be graphene, carbon nanotubes or carbon black.
The step(b)Described in platinum acid chloride solution temperature for 0~50 DEG C, concentration is 0.1~3mmol/L, pH value 3
~5.
The step(b)Described in magnetic field intensity be 0.1~4T, the carbon-supported metal nano nickel particles and the chlorine platinum
When the reaction time of acid solution is 0.5~12 small.
The step(c)The middle impurity that the platinum-nickel alloy reaction-ure surface is removed using acid solution etch, the acid are molten
The concentration of liquid is 0.2~4mmol/L, when the etch time 0.5~5 is small.
The step(c)Described in acid solution be hydrochloric acid, sulfuric acid or perchloric acid.
The step(c)In post processing include centrifugation, filtering and baking step.
Advantageous effect
In method provided by the invention, carbon-supported metal nano nickel particles are prepared with hydro-thermal method, under certain magnetic field condition, are allowed to
It is chemically reacted with platinum acid chloride solution, using the Ni atoms of acid solution removal reaction-ure surface remnants, by centrifugation, mistake
The step of filter, drying, obtain platinum-nickel alloy catalyst.The present invention prepares platinum-nickel alloy under magnetic fields using chemical deposition
Catalyst, the content of noble metal platinum is high in platinum-nickel alloy catalyst prepared by such method, and catalytic performance is good.With modern technologies phase
Than by influence of the magnetic field to platinum-nickel alloy forming core and growth course, realizing and being prepared under magnetic field with preferable catalytic activity
The purpose of platinum-nickel alloy catalyst.
Description of the drawings
Fig. 1:The X ray diffracting spectrum (XRD) of the Pt-Ni alloys formed after Ni particles and the reaction of Ni granular raws battery replacement
As a result;
Fig. 2:(a)、(b)、(c)Surface topography for the Pt-Ni alloys obtained under different magnetic field strength condition;
Fig. 3:Pt layer thickness variations for the Pt-Ni alloys obtained under different magnetic field strength condition;
Fig. 4:It is the Pt-Ni alloys that are obtained under different magnetic field strength condition to redox reaction(ORR)Catalytic performance test.
Specific embodiment
It elaborates with reference to embodiment to the present invention, but protection scope of the present invention is not limited only to following implementation
Example:
Embodiment one:
A kind of method for preparing platinum-nickel alloy catalyst, including:
Carbon-supported metal nano nickel particles are prepared using hydro-thermal method;
Then carbon-supported metal nano nickel particles are put into temperature as 0 DEG C, concentration 0.1mmol/L, pH value is 3 platinum acid chloride solution
In, while by the magnetic field of superconducting coil application 0.1T, make carbon-supported metal nano nickel particles and platinum acid chloride solution reaction 0.5 small
When;
The Ni atoms of surface residual are further removed using hydrochloric acid solution, concentration of hydrochloric acid solution 0.2mmol/L makes reactant exist
When etch 0.5 is small in hydrochloric acid solution.The step of obtained substance is by centrifuging, filtering, drying finally obtains platinum-nickel alloy catalysis
Agent.The platinum-nickel alloy catalyst of different Pt shell thicknesses can be made with the aforedescribed process by adopting.
Preparation process:Graphene and metallic nickel are placed in autoclave aqueous solution, under high temperature, condition of high voltage into
Row hydro-thermal reaction, then the post processings such as separating, washing, drying are made graphene and carry metallic nickel nano granule, the stone prepared
Black alkene carries metallic nickel nano granule and is slowly put into the platinum acid chloride solution prepared, will contain graphene and carry metal nickel nano
The platinum acid chloride solution of grain is transferred in the glassware for being placed with ice cube, and glassware is put into magnetic field, ensures substrate and magnetic field
Direction is parallel, intensity 0.1T, when deposition 0.5 is small;By the platinum-nickel alloy compound of acquisition in the hydrochloric acid solution of 0.2mmol/L
It when etch 0.5 is small, is then centrifuged for, filters and dries acquisition metal platinum nickel alloy nanoparticles.
Material phase analysis:Material phase analysis is carried out to obtained sample using X-ray diffractometer (XRD), as a result such as specification
Shown in attached drawing 1:Before primary battery displacement reaction, metal nickel particle is in the Ni that the position of 45.40 diffraction maximums is metallic nickel(111)Crystal face
Diffraction maximum;After primary battery displacement reaction, platinum-nickel alloy is located at Pt respectively in 40.65 and 46.60 diffraction maximum(111)And Ni
(111)Between crystallographic plane diffraction peak, as seen from the figure, after primary battery displacement reaction, Pt atomic substitutions or it is dissolved into the lattice of Ni, shape
Into platinum-nickel alloy.
Surface topography is observed:Platinum-nickel alloy catalyst table is carried to graphene obtained using transmission electron microscope (TEM)
Face pattern is observed, and Pt the and Ni composition measurements of particle are carried out using subsidiary energy disperse spectroscopy (EDS), and Pt is calculated according to result
Thickness of the shell, observation result is as shown in Figure of description 2:Fig. 2 (a), (b) and (c) are that magnetic field intensity is 0T, 0.1T and 4T respectively
Under the conditions of graphene carry platinum-nickel alloy catalyst surface pattern.As seen from the figure:Particle size about 4nm, after applying magnetic field,
Significant changes do not occur for the size of particle.Pt the and Ni composition measurements of particle are carried out by EDS, it is thick to calculate Pt shells according to result
Degree, analysis result is as shown in Figure of description 3:The thickness of Pt shells is 0.8nm in platinum-nickel alloy under the conditions of 0T in Fig. 3;In Fig. 3
The thickness of Pt shells is 1.1nm in platinum-nickel alloy under the conditions of 0.1T;The thickness of Pt shells is in platinum-nickel alloy under the conditions of 4T in Fig. 3
1.5nm.After applying high-intensity magnetic field, the thickness of Pt shells dramatically increases in the platinum-nickel alloy of acquisition.Therefore, can be regulated and controled by high-intensity magnetic field
The thickness of Pt shells in platinum-nickel alloy.
Catalytic performance test:Fig. 4 is that the platinum-nickel alloy obtained under different magnetic field strength condition surveys the catalytic performance of ORR
Examination.As seen from the figure:After applying magnetic field, higher ORR current densities and higher starting point position can be obtained.The result shows that:By
Increase in Pt layer thickness, the electrochemical catalysis performance that applying the platinum-nickel alloy catalyst that magnetic field is obtained has, which is better than, not to be applied
The catalyst that magnetic field is obtained.
Embodiment two:
A kind of method for preparing platinum-nickel alloy catalyst, including:
Carbon-supported metal nano nickel particles are prepared using hydro-thermal method;
Carbon-supported metal nano nickel particles are put into temperature as 25 DEG C, concentration 0.15mmol/L, pH value is 4 platinum acid chloride solution
In, while by the magnetic field of superconducting coil application 2.1T, make carbon-supported metal nano nickel particles and platinum acid chloride solution reaction 6.5 small
When;
The Ni atoms of surface residual are further removed using sulfuric acid solution, sulfuric acid solution concentration is 1.9mmol/L, and reactant is made to exist
When etch 3 is small in sulfuric acid solution.The step of obtained substance is by centrifuging, filtering, drying finally obtains platinum-nickel alloy catalysis
Agent.
The platinum-nickel alloy catalyst of different Pt shell thicknesses can be made with the aforedescribed process by adopting.
Preparation process:Carbon nanotubes and metallic nickel are placed in autoclave aqueous solution, under high temperature, condition of high voltage
Hydro-thermal reaction, then the carbon-supported metal nano nickel particles of the post processings such as separating, washing, drying are carried out, the carbon prepared carries
Metallic nickel nano granule is slowly put into the platinum acid chloride solution set, and the glass that is placed with ice cube will be transferred to containing platinum acid chloride solution
In glass vessel, glassware is put into magnetic field, ensures that substrate is parallel with magnetic direction, intensity 2.1T, when deposition 6.5 is small;
It when etch 3 is small in the sulfuric acid solution of 1.9mmol/L by the platinum-nickel alloy chemistry of acquisition, is then centrifuged for, filters and dries acquisition
Metal platinum nickel alloy nanoparticles.
Embodiment three:
A kind of method for preparing platinum-nickel alloy catalyst, including:
Charcoal is prepared using hydro-thermal method and carries metallic nickel nano granule;
Carbon-supported metal nano nickel particles are put into temperature as 50 DEG C, concentration 3mmol/L, pH value is in 5 platinum acid chloride solution,
Apply the magnetic field of 4T by superconducting coil simultaneously, when making carbon-supported metal nano nickel particles and small platinum acid chloride solution reaction 12;
The Ni atoms of surface residual are further removed using perchloric acid solution, perchloric acid solution concentration is 4mmol/L, makes reactant
When etch 5 is small in perchloric acid solution.The step of obtained substance is by centrifuging, filtering, drying, finally obtains platinum-nickel alloy and urges
Agent.The platinum-nickel alloy catalyst of different Pt shell thicknesses can be made with the aforedescribed process by adopting.
Preparation process:Carbon black and metallic nickel are placed in autoclave aqueous solution, carried out under high temperature, condition of high voltage
Hydro-thermal reaction, then the carbon-supported metal nano nickel particles of the post processings such as separating, washing, drying, the carbon-supported metal prepared
Nano nickel particles are slowly put into the platinum acid chloride solution set, and the vierics that are placed with ice cube will be transferred to containing platinum acid chloride solution
In ware, glassware is put into magnetic field, ensures that substrate is parallel with magnetic direction, intensity 4T, when deposition 12 is small;By acquisition
Platinum-nickel alloy chemistry is then centrifuged for, filters and dry the metal platinum of acquisition when etch 5 is small in the perchloric acid solution of 4mmol/L
Nickel alloy nanoparticles.
Claims (8)
- A kind of 1. method for preparing platinum-nickel alloy catalyst, which is characterized in that including:(a)Carbon-supported metal nano nickel particles are prepared using carbon carrier;(b)The carbon-supported metal nano nickel particles are put into platinum acid chloride solution, and magnetic field is added to make the carbon-supported metal nickel nanometer Particle is reacted with the platinum acid chloride solution, obtains platinum-nickel alloy reactant;(c)The impurity of the platinum-nickel alloy reaction-ure surface is removed, it is post-treated to obtain platinum-nickel alloy catalyst.
- A kind of 2. method for preparing platinum-nickel alloy catalyst according to claim 1, which is characterized in that the step(a) It is middle that the carbon-supported metal nano nickel particles are prepared using hydro-thermal method.
- A kind of 3. method for preparing platinum-nickel alloy catalyst according to claim 1, which is characterized in that the step(a) In the carbon carrier be graphene, carbon nanotubes or carbon black.
- A kind of 4. method for preparing platinum-nickel alloy catalyst according to claim 1, which is characterized in that the step(b) Described in platinum acid chloride solution temperature for 0~50 DEG C, concentration is 0.1~3mmol/L, and pH value is 3~5.
- A kind of 5. method for preparing platinum-nickel alloy catalyst according to claim 1, which is characterized in that the step (b)Described in magnetic field intensity be 0.1~4T, the reaction time of the carbon-supported metal nano nickel particles and the platinum acid chloride solution is 0.5~12 it is small when.
- A kind of 6. method for preparing platinum-nickel alloy catalyst according to claim 1, which is characterized in that the step(c) The middle impurity that the platinum-nickel alloy reaction-ure surface is removed using acid solution etch, the concentration of the acid solution for 0.2~ 4mmol/L, when the etch time 0.5~5 is small.
- A kind of 7. method for preparing platinum-nickel alloy catalyst according to claim 6, which is characterized in that the step(c) Described in acid solution be hydrochloric acid, sulfuric acid or perchloric acid.
- A kind of 8. method for preparing platinum-nickel alloy catalyst according to claim 1, which is characterized in that the step(c) In post processing include centrifugation, filtering and baking step.
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CN114457365A (en) * | 2022-01-20 | 2022-05-10 | 成都理工大学 | Pt-Ni composite material, preparation method thereof and application thereof as catalyst for hydrogen production by electrolyzing water |
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CN107069053A (en) * | 2017-02-03 | 2017-08-18 | 沈阳理工大学 | A kind of method for preparing pt-fe alloy catalyst |
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CN103990468A (en) * | 2014-05-30 | 2014-08-20 | 中国科学院长春应用化学研究所 | Post-processing method for carbon-supported Pt-Fe catalyst |
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CN114457365A (en) * | 2022-01-20 | 2022-05-10 | 成都理工大学 | Pt-Ni composite material, preparation method thereof and application thereof as catalyst for hydrogen production by electrolyzing water |
CN114457365B (en) * | 2022-01-20 | 2024-01-26 | 成都理工大学 | Pt-Ni composite material, preparation method thereof and application of Pt-Ni composite material as catalyst for hydrogen production by water electrolysis |
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Application publication date: 20180518 |