CN109950554A - A kind of graphene-supported metal nano island catalyst and the preparation method and application thereof - Google Patents
A kind of graphene-supported metal nano island catalyst and the preparation method and application thereof Download PDFInfo
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- Y02E60/30—Hydrogen technology
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Abstract
The present invention discloses a kind of graphene-supported metal nano island catalyst and the preparation method and application thereof, wherein preparation method is comprising steps of graphene and bleeding agent are dispersed in deionized water, to be mixed to prepare graphene dispersing solution；Metal ion compound is added into the graphene dispersing solution, is mixed to get graphene mixed slurry；The graphene mixed slurry is heated, so that the metal ion reduction is generated metal nano island and is attached to graphene between layers, the graphene-supported metal nano island catalyst is made.Graphene-supported metal nano island catalyst made from preparation method is less likely to occur to reunite in catalytic process through the invention, and cyclical stability is strong；After the graphene-supported metal nano island catalyst is applied to metal-air battery and fuel cell, the overpotential of oxygen cathode can be significantly reduced, improve the reaction rate and long-term cycle stability of oxygen cathode.
Description
Technical field
The present invention relates to metal nano catalyst field more particularly to a kind of graphene-supported metal nano island catalyst and
Preparation method and application.
Background technique
In past 20 years, the system optimization of new material, technology for preparing electrode and battery system promotes lithium ion battery
The continuous promotion of performance, in addition to for portable electronic device, lithium ion battery just gradually replaces other secondary cells, electronic
Automobile and beating in the large size column support types industry such as energy storage device is played a greater and greater role.For example, further to push electronic vapour
Vehicle comes into huge numbers of families, and government subsidizes vehicle enterprise on a large scale, while establishing multiple pilot projects in China, by
Step is promoted and applied.However, the energy density of conventional lithium ion battery is promoted empty already close to theoretical value (150Wh/kg)
Between it is limited, it is difficult to meet the requirement that electric car further provides for course continuation mileage.In order to further increase the energy of battery system
Density, some new systems are developed in succession, such as lithium-sulfur cell, metal-air battery and fuel cell etc., dependency basis
Plinth research and development has become domestic and international forward position research hotspot.
Fuel cell and metal-air battery all refer to hydrogen reduction process, and oxygen cathode reaction efficiency is low, and overpotential is high, at present
The catalyst being often used is based on Pt system noble metal.Pt belongs to noble metal, not only scarcity of resources, expensive, but also is urging
It is easy to reunite during changing, cyclical stability is poor, it is difficult to which large-scale promotion application seriously hinders metal-air battery and combustion
Expect the commercialization process of battery.Therefore, the research and development of efficient, stable and cheap type catalyst is to improve urging for oxygen cathode
Change performance and pushes the key point of system industrial application.
Therefore, the existing technology needs to be improved and developed.
Summary of the invention
In view of above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of graphene-supported metal nano islands to urge
Agent and the preparation method and application thereof, it is intended to solve existing metal nano catalyst and be easy to reunite in catalytic process, circulation is steady
It is qualitative poor, it is difficult to which that large-scale promotion application seriously hinders asking for the commercialization process of metal-air battery and fuel cell
Topic.
Technical scheme is as follows:
A kind of preparation method of graphene-supported metal nano island catalyst, wherein comprising steps of
Graphene and bleeding agent are dispersed in deionized water, to be mixed to prepare graphene dispersing solution；
Metal ion compound is added into the graphene dispersing solution, mixing makes the metal ion in metal ion compound point
It is scattered to graphene between layers, obtains graphene mixed slurry；
Under vacuum conditions, the graphene mixed slurry is heated, the metal ion reduction is made to generate metal
Nano island is simultaneously attached to graphene between layers, and the graphene-supported metal nano island catalyst is made.
The preparation method of the graphene-supported metal nano island catalyst, wherein according to rubbing for graphene and bleeding agent
You disperse graphene and bleeding agent in deionized water, to be mixed to prepare graphene dispersing solution than the ratio for being 1:0.5-3.
The preparation method of the graphene-supported metal nano island catalyst, wherein in the graphene dispersing solution, graphite
The mass percent of alkene is 0.3-2%.
The preparation method of the graphene-supported metal nano island catalyst, wherein the number of plies of the graphene is 2-6
Layer.
The preparation method of the graphene-supported metal nano island catalyst, wherein the bleeding agent is (NH4)4·
EDTA and (NH4)4One or both of PTDA.
The preparation method of the graphene-supported metal nano island catalyst, wherein the metal ion compound is can
Dissolubility Fe salt, soluble Co salt, soluble Ni salt, soluble Au salt, soluble Ag salt, soluble Pt salt, soluble Pd salt can
Dissolubility Rb salt, one of soluble Rh salt and solubility Ru salt or a variety of.
The preparation method of the graphene-supported metal nano island catalyst, wherein press metal ion compound and graphite
The molar ratio of alkene is the ratio of 0.2-0.5:1, and metal ion compound is added in graphene dispersing solution, graphite is mixed to get
Alkene mixed slurry.
The preparation method of the graphene-supported metal nano island catalyst, wherein under vacuum conditions, in 450-600
Heat treatment 6-10h is carried out to the graphene mixed slurry under conditions of DEG C, so that the metal ion reduction is generated metal and receives
Rice island is simultaneously attached to graphene between layers, and the graphene-supported metal nano island catalyst is made.
A kind of graphene-supported metal nano island catalyst, wherein be prepared using preparation method of the present invention.
A kind of application of graphene-supported metal nano island catalyst, wherein by graphene-supported gold of the present invention
Belong to the oxygen cathode elctro-catalyst that nano island catalyst is used as in metal-air battery or fuel cell.
The utility model has the advantages that the present invention provides a kind of preparation method of graphene-supported metal nano island catalyst, the system
Preparation Method has the characteristics that easy to operate, at low cost, suitable large-scale promotion application；Stone made from preparation method through the invention
Black alkene carried metal nano island catalyst is less likely to occur to reunite in catalytic process, and cyclical stability is strong；The graphene
After carried metal nano island catalyst is applied to metal-air battery and fuel cell, the excessively electric of oxygen cathode can be significantly reduced
Gesture improves the reaction rate and long-term cycle stability of oxygen cathode.
Detailed description of the invention
Fig. 1 is a kind of preparation method preferred embodiment of graphene-supported metal nano island catalyst provided by the invention
Flow chart.
Fig. 2 is the transmission electron microscope figure of graphene-supported platinum nano island catalyst in the embodiment of the present invention 1.
Fig. 3 is the transmission electron microscope figure of graphene-supported rubidium nano island catalyst in the embodiment of the present invention 3.
Specific embodiment
The present invention provides a kind of graphene-supported metal nano island catalyst and the preparation method and application thereof, to make this hair
Bright purpose, technical solution and effect are clearer, clear, and the present invention is described in more detail below.It should be appreciated that herein
Described specific examples are only used to explain the present invention, is not intended to limit the present invention.
Referring to Fig. 1, Fig. 1 be a kind of preparation method of graphene-supported metal nano island catalyst provided by the invention compared with
The flow chart of good embodiment, as shown, itself comprising steps of
S10, graphene and bleeding agent are dispersed in deionized water, to be mixed to prepare graphene dispersing solution；
Be added metal ion compound in S20, Xiang Suoshu graphene dispersing solution, mixing make the metal in metal ion compound from
Son is distributed to graphene between layers, obtains graphene mixed slurry；
S30, under vacuum conditions, heats the graphene mixed slurry, generates the metal ion reduction
Metal nano island is simultaneously attached to graphene between layers, and the graphene-supported metal nano island catalyst is made.
Specifically, graphene is a kind of carbon atom with SP2The two-dimensional layer material that hydridization is formed, good electric conductivity
Be conducive to the conduction of electronics, high-specific surface area is conducive to the dispersion of supported catalyst, while the high mechanical strength of graphene and steady
Fixed chemical property is it is possible to prevente effectively from catalyst loss caused by being destroyed due to carrier, to improve the steady of catalyst
It is qualitative.In consideration of it, the present invention does carrier material with graphene, growth in situ monodisperse type metal nano island is urged on the surface of graphene
Agent, compared with individual metal nanoparticle, graphene-supported metal nano island catalyst prepared by the present invention can mentioned
Its dosage is reduced while high catalyst stability, to reduce catalyst use cost and improve the catalytic efficiency of catalyst.
However, the preparation of conventional doping type graphene is directed to water-heat process, hydro-thermal method needs high temperature and high pressure environment, to equipment and production
The requirement of technique is high, and energy consumption is high, it is difficult to realize scale application；And the present invention is by improving existing production technology, it is real
Showed batch efficiently preparation low cost the graphene-supported metal nano island catalyst of functional form, pushed metal-air battery and
Commercializing fuel cells application.
In some embodiments, according to the molar ratio of graphene and bleeding agent be 1:0.5-3 ratio, by graphene with
Bleeding agent disperses in deionized water, to be mixed to prepare graphene dispersing solution.In the present embodiment, by the way that graphene and bleeding agent are divided
Dissipate in deionized water, bleeding agent described in mixed process can to graphene carry out intercalation, thus slacken graphene layer with
Van der Waals force between layer, this advantageously reduces the resistance that subsequent metal ionic compound is spread between layers in graphene,
The metal nano island catalyst for generating sequential reduction is dispersed in the surface of graphene layer.
In some embodiments, the bleeding agent is the nonionic chelate of hydrophilic and oleophilic, it is preferred that the bleeding agent
For (NH4)4EDTA and (NH4)4One or both of PTDA, but not limited to this.
In some embodiments, in the graphene dispersing solution, the mass percent of graphene is 0.3-2%.
In some specific embodiments, the number of plies of the graphene is 2-6 layers, and the present invention is directly made using graphene
Carrier material, rather than graphene oxide, can be to avoid the destruction restored after oxidation to graphene lattice, while can also reduce
Process and energy consumption, improve efficiency.
In some embodiments, the ratio for being 0.2-0.5:1 in the molar ratio of metal ion compound and graphene, will
Metal ion compound is added in graphene dispersing solution, and mixing makes in metal ion and graphene in metal ion compound
Layer adequately contact, so that metal ion be made to be distributed to graphene between layers, obtains graphene mixed slurry.The present embodiment
Select the graphene of specific surface big, electric conductivity and high mechanical strength as carrier material, using strong between metal and graphene
Interaction, is tightly anchored at graphene internal layer surface for metal nano island, can significantly improve the dispersion on metal nano island
Property and stability, alleviate the reuniting effect in long-term electrochemistry cyclic process.
In some embodiments, the metal ion compound is Dissolvable Fe salt, soluble Co salt, soluble Ni
Salt, soluble Au salt, soluble Ag salt, soluble Pt salt, soluble Pd salt, soluble Rb salt, soluble Rh salt and solubility
One of Ru salt is a variety of, but not limited to this.
In some embodiments, under vacuum conditions, to the graphene mixed slurry under conditions of 450-600 DEG C
Heat treatment 6-10h is carried out, so that the metal ion reduction is generated metal nano island and is attached to graphene between layers, makes
Obtain the graphene-supported metal nano island catalyst.
In the present embodiment, the graphene mixed slurry is transferred in closed container, is first stirred under vacuum, then into
The reaction of row temperature-pressure.Specifically, stirring 0.5-4h to the graphene mixed slurry under the power of agitator of 18-26ps；So
Afterwards, in nitrogen atmosphere and under conditions of pressure is 2-4 atmospheric pressure, the graphene is mixed with 450-600 DEG C of heating temperature
It closes slurry and heats 6-10h, the metal ion reduction is made to generate metal nano island and be attached to graphene between layers,
It can be prepared by the graphene-supported metal nano island catalyst after drying process.
The present invention also provides a kind of graphene-supported metal nano island catalyst, wherein uses preparation method system of the present invention
It is standby to obtain.The graphene-supported metal nano island catalyst prepared by the method for the invention, which has, to be not easy to send out in catalytic process
The characteristics of raw reunion, cyclical stability is strong, high catalytic efficiency.
Further, the present invention also provides a kind of applications of graphene-supported metal nano island catalyst, by institute of the present invention
The graphene-supported metal nano island catalyst stated is used as the oxygen cathode elctro-catalyst in metal-air battery or fuel cell, can
To significantly reduce the overpotential of oxygen cathode, the reaction rate and long-term cycle stability of oxygen cathode are improved.
A kind of preparation method of graphene-supported metal nano island catalyst of the present invention is done below by specific embodiment
Further explanation explanation:
Embodiment 1
1) 0.3g graphene and 99.7g deionized water, are weighed, the graphene aqueous solution that mass fraction is 0.3% is prepared, according to stone
Black alkene: bleeding agent=1:0.5 molar ratio weighs 5.8g(NH4)4PTDA bleeding agent is added in graphene aqueous solution, high speed
Emulsification pretreatment machine handles 30min, forms uniform and stable graphene dispersing solution；
2), according to graphene: metal ion compound=1:0.2 molar ratio weighs 1.68g PtCl4It is added in step 1)
In graphene dispersing solution, magnetic agitation 6h comes into full contact with platinum ion with graphene internal layer, and it is mixed to form evenly dispersed graphene
Close slurry；
3), the graphene mixed slurry in step 2 is transferred in closed container, is first vacuumized, then mechanical stirring 1h, most
Temperature-pressure reaction is carried out afterwards, and temperature is 450 DEG C, time 10h；
4) it, is cooled to room temperature, then the product in step 3) is washed and is freeze-dried, graphene-supported platinum can be obtained
The perspective electron microscope figure of metal nano island catalyst, the graphene-supported platinum nano island catalyst is as shown in Figure 2.
Embodiment 2
1) 0.6g graphene and 99.4g deionized water, are weighed, the graphene aqueous solution that mass fraction is 0.6% is prepared, according to stone
Black alkene: bleeding agent=1:1 molar ratio weighs 18.1g(NH4)4EDTA bleeding agent is added in graphene aqueous solution, ultrasound
Disperse 30min, forms uniform and stable graphene dispersing solution；
2), according to graphene: metal ion compound=1:0.3 molar ratio weighs 2.55g AgNO3It is added in step 1)
In graphene dispersing solution, magnetic agitation 4h comes into full contact with silver ion with graphene internal layer, and it is mixed to form evenly dispersed graphene
Close slurry；
3), the graphene mixed slurry in step 2 is transferred in closed container, is first vacuumized, then mechanical stirring 2h, most
Temperature-pressure reaction is carried out afterwards, and temperature is 500 DEG C, time 8h；
4) it, is cooled to room temperature, then the product in step 3) is washed and is dried in vacuo, graphene-supported silver can be obtained
Metal nano island catalyst.
Embodiment 3
1) 1g graphene and 99g deionized water, are weighed, the graphene aqueous solution that mass fraction is 1% is prepared, according to graphene: seeping
The molar ratio of saturating agent=1:1.5, weighs 58g(NH4)4PTDA bleeding agent is added in graphene aqueous solution, high energy ball mill point
Processing 2h is dissipated, uniform and stable graphene dispersing solution is formed；
2), according to graphene: metal ion compound=1:0.4 molar ratio weighs the stone that 4.03g RbCl is added in step 1)
In black alkene dispersion liquid, magnetic agitation 4h comes into full contact with rubidium ion with graphene internal layer, forms evenly dispersed graphene mixing
Slurry；
3), the graphene mixed slurry in step 2 is transferred in closed container, is first vacuumized, then mechanical stirring 2h, most
Temperature-pressure reaction is carried out afterwards, and temperature is 550 DEG C, time 7h；
4) it, is cooled to room temperature, washing and supercritical drying then are carried out to the product in step 3), can be obtained graphene-supported
Rubidium metal nano island catalyst, perspective electron microscope figure such as Fig. 3 institute of graphene-supported rubidium metal nano island catalyst
Show.
Embodiment 4
1) 1.5g graphene and 98.5g deionized water, are weighed, the graphene aqueous solution that mass fraction is 1.5% is prepared, according to stone
Black alkene: bleeding agent=1:2 molar ratio weighs 90.5g(NH4)4EDTA bleeding agent is added in graphene aqueous solution, ultrasound
Disperse 1.5h, forms uniform and stable graphene dispersing solution；
2), according to graphene: metal ion compound=1:0.45 molar ratio weighs 13.8g Pd (NH3)4Cl2Step is added
1) in the graphene dispersing solution in, magnetic agitation 4h comes into full contact with palladium ion with graphene internal layer, forms graphene mixing slurry
Material；
3), the graphene mixed slurry in step 2 is transferred in closed container, is first vacuumized, then mechanical stirring 3h, most
Temperature-pressure reaction is carried out afterwards, and temperature is 600 DEG C, time 6h；
4) it, is cooled to room temperature, then the product in step 3) is washed and is freeze-dried, graphene-supported palladium can be obtained
Metal nano island catalyst.
Embodiment 5
1) 2g graphene and 98g deionized water, are weighed, the graphene aqueous solution that mass fraction is 2% is prepared, according to graphene: seeping
The molar ratio of saturating agent=1:3, weighs 181g(NH4)4EDTA bleeding agent is added in graphene aqueous solution, uses cell pulverization
Machine decentralized processing 2h, forms uniform and stable graphene dispersing solution；
2), according to graphene: metal ion compound=1:0.5 molar ratio weighs 20.15g Fe (NO3)3Step 1) is added
In graphene dispersing solution in, ultrasonic disperse handle 1h, come into full contact with iron ion with graphene internal layer, formed evenly dispersed
Graphene mixed slurry；
3), the graphene mixed slurry in step 2 is transferred in closed container, is first vacuumized, then mechanical stirring 4h, most
Temperature-pressure reaction is carried out afterwards, and temperature is 500 DEG C, time 8h；
4) it, is cooled to room temperature, then the product in step 3) is washed and is freeze-dried, graphene-supported iron can be obtained
Metal nano island catalyst.
In conclusion the present invention provides a kind of preparation method of graphene-supported metal nano island catalyst, the system
Preparation Method has the characteristics that easy to operate, at low cost, suitable large-scale promotion application；Stone made from preparation method through the invention
Black alkene carried metal nano island catalyst is less likely to occur to reunite in catalytic process, and cyclical stability is strong；The graphene
After carried metal nano island catalyst is applied to metal-air battery and fuel cell, the excessively electric of oxygen cathode can be significantly reduced
Gesture improves the reaction rate and long-term cycle stability of oxygen cathode.
It should be understood that the application of the present invention is not limited to the above for those of ordinary skills can
With improvement or transformation based on the above description, all these modifications and variations all should belong to the guarantor of appended claims of the present invention
Protect range.
Claims (10)
1. a kind of preparation method of graphene-supported metal nano island catalyst, which is characterized in that comprising steps of
Graphene and bleeding agent are dispersed in deionized water, to be mixed to prepare graphene dispersing solution；
Metal ion compound is added into the graphene dispersing solution, mixing makes the metal ion in metal ion compound point
It is scattered to graphene between layers, obtains graphene mixed slurry；
Under vacuum conditions, the graphene mixed slurry is heated, the metal ion reduction is made to generate metal
Nano island is simultaneously attached to graphene between layers, and the graphene-supported metal nano island catalyst is made.
2. the preparation method of graphene-supported metal nano island catalyst according to claim 1, which is characterized in that according to stone
The molar ratio of black alkene and bleeding agent is the ratio of 1:0.5-3, and graphene and bleeding agent are dispersed in deionized water, to be mixed to prepare
Graphene dispersing solution.
3. the preparation method of graphene-supported metal nano island catalyst according to claim 2, which is characterized in that the stone
In black alkene dispersion liquid, the mass percent of graphene is 0.3-2%.
4. the preparation method of graphene-supported metal nano island catalyst according to claim 2, which is characterized in that the stone
The number of plies of black alkene is 2-6 layers.
5. the preparation method of graphene-supported metal nano island catalyst according to claim 2, which is characterized in that the infiltration
Saturating agent is (NH4)4EDTA and (NH4)4One or both of PTDA.
6. the preparation method of graphene-supported metal nano island catalyst according to claim 1, which is characterized in that the gold
Category ionic compound is Dissolvable Fe salt, soluble Co salt, soluble Ni salt, soluble Au salt, soluble Ag salt, soluble Pt
Salt, soluble Pd salt, soluble Rb salt, one of soluble Rh salt and solubility Ru salt or a variety of.
7. the preparation method of graphene-supported metal nano island catalyst according to claim 1, which is characterized in that press metal
The molar ratio of ionic compound and graphene is the ratio of 0.2-0.5:1, and metal ion compound is added to graphene dispersion
In liquid, it is mixed to get graphene mixed slurry.
8. the preparation method of graphene-supported metal nano island catalyst according to claim 1, which is characterized in that in vacuum
Under the conditions of, heat treatment 6-10h is carried out to the graphene mixed slurry under conditions of 450-600 DEG C, make the metal from
Son reduction generates metal nano island and is attached to graphene between layers, and the graphene-supported metal nano island catalysis is made
Agent.
9. a kind of graphene-supported metal nano island catalyst, which is characterized in that use any one the preparation side claim 1-8
Method is prepared.
10. a kind of application of graphene-supported metal nano island catalyst, which is characterized in that by graphite as claimed in claim 9
Alkene carried metal nano island catalyst is used as the oxygen cathode elctro-catalyst in metal-air battery or fuel cell.
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Application publication date: 20190628 |