CN107256973A - A kind of preparation method of three-dimensional structure graphene carbon nanotube composite carrier load PtSn catalyst - Google Patents
A kind of preparation method of three-dimensional structure graphene carbon nanotube composite carrier load PtSn catalyst Download PDFInfo
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- CN107256973A CN107256973A CN201710545538.4A CN201710545538A CN107256973A CN 107256973 A CN107256973 A CN 107256973A CN 201710545538 A CN201710545538 A CN 201710545538A CN 107256973 A CN107256973 A CN 107256973A
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- graphene
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- catalyst
- ethanol
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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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- 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
- H01M4/88—Processes of manufacture
- H01M4/8825—Methods for deposition of the catalytic active composition
-
- 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
- H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
- H01M4/926—Metals of platinum group supported on carriers, e.g. powder carriers on carbon or graphite
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention discloses a kind of preparation method of three-dimensional structure graphene carbon nanotube composite carrier load PtSn catalyst.Specifically related to one kind is first assembled graphene and CNT, form the complex carrier with three-D space structure, immersion reduction method loaded metal platinum tin (PtSn) on complex carrier is recycled, the new method with high performance ethanol oxidation catalyst is prepared.The present invention includes comprising the following steps that：Graphite oxide and the shortwall CNT of carboxylated are formed to the mixed liquor of graphene/carbon nano-tube compound in ethylene glycol solution first, the ionic liquid containing Pt metal and Sn is added into progress reduction reaction in mixed liquor respectively again to load to Pt metal Sn on graphene/carbon nano-tube complex carrier, preparing has high performance ethanol oxidation catalyst.
Description
Technical field
The present invention relates to a kind of preparation method of ethanol oxidation catalyst, and in particular to one kind first receives graphene and carbon
Mitron is assembled, and forms the complex carrier with three-D space structure, recycles immersion reduction method to be loaded on complex carrier
Metal platinum tin (PtSn), prepares the new method with high performance ethanol oxidation catalyst.
Background technology
With the rapid development of society, demand of the people to the energy and the requirement more and more higher to environmental protection, therefore exploitation
Turn into the choosing of certainty with efficient, cleaning new energy.Fuel cell is used as the substitute electric power of mobile electronic device, Yin Qigao
The advantage such as energy density, low disposal of pollutants, fuel variation and receive significant attention.And direct liquid alcohols combustion therein
Expect the advantages of battery is cleaned with it, efficient, safe, portable, operating condition is gentle, it is most extensive industrialization prospect to be described as
A types of fuel cells.But methanol has certain toxicity, so new liquid must be explored to substitute poisonous methanol, and ethanol
Source is wide, and price is low, renewable, and nontoxic, and practical application has a high potential, and is believed to substitute DMFC.
In the catalytic oxidation of ethanol, Pt shows higher catalytic activity, however, Pt is not only expensive but also catalytic process
In be easy to CO poisonings so as to causing catalytic activity to reduce, service life is short, hinders the commercialization of such battery.Therefore, people
Substantial amounts of exploration has been carried out to solve these technical problems, it is considered that there are two methods feasible effectively.One kind is by accurate
Control the pattern and size of nano platinum particle to change the microstructure of platinum catalyst, this method energy the efficient oxidation ethanol is improved
Catalyst is to CO tolerance, but its preparation process is extremely complex, and in the accurately microstructure of control platinum, its manufacturing cost is led to
Often very high, this brings the shortcoming of key to business application：Another method is to introduce the outer of lower cost to be metal to be formed
Pt bimetallics catalyst even multicomponent catalyst, general bianry alloy has：Pt Sn, Pt Ru, Pt Ni, Pt Au and Pt
Pb etc., wherein, Pt Sn bimetallic catalysts have shown that preferable catalytic performance.In addition, explore can dispersed Pt and
The carrier material of Pt base catalyst is also very important.The use of appropriate catalyst carrier material, is that a kind of improve is catalyzed
The shortcut of agent electro-chemical activity, and the use of noble metal can be reduced.
Recently, graphene is because of the theoretical specific surface area (2630m of its superelevation2/ g), excellent electric conductivity, enough porositys
And excellent mechanical performance is considered to be a kind of very promising catalyst carrier material.Generally, using electronation legal system
Standby graphene cost is relatively low, can carry out batch preparation.However, graphene prepared by this method is stronger because piece interlayer has
Intermolecular Van der Waals force, causes graphene sheet layer easily to be reunited, and greatly reduces the specific surface area utilization rate of carrier material, and hinders
Diffusion of the metal ion between graphene layer is hindered.Therefore, researcher starts a kind of effective method and tackled
This challenge：Supporter is introduced between graphene sheet layer, for example, is drawn CNT, metal oxide or conducting polymer
Enter interlayer and prepare graphene composite material；The specific surface area and chemical property of graphene can be so significantly increased, herein
Field, graphene/carbon nano-tube compound (g-cnts) is increasingly becoming a study hotspot.By to two dimension graphene and
One-dimensional CNT carries out assembling and forms the graphene/carbon nano-tube complex carrier with three-dimensional netted space structure, and leads to
The synergy crossed between them, shows the more excellent performance than any homogenous material, such as more preferable electric conductivity, mechanics
Performance and thermal conductivity factor, three-dimensional network characteristic etc..The introducing of CNT, can suppress graphene sheet layer and reunite, construct ion
The passage of diffusion, so that it is guaranteed that quickly diffusion and transmission are not to reunite catalyst preparation process intermediate ion, so that effectively
The size of ground control catalyst metal particles and distribution；Moreover, the graphene/carbon nano-tube complex carrier with three dimensions
Formed, expand the exposure area of graphenic surface, the shape that chance is beneficial to alloy is provided for the abundant contact of various ions
Into factors above can have vital influence to the activity for improving catalyst.Therefore it is this at present with three dimensions knot
The composite of structure has critically important Research Significance as catalyst carrier.
This patent is first assembled graphene and CNT, forms the complex carrier with three-D space structure,
Immersion reduction method loaded metal platinum tin (PtSn) on complex carrier is recycled, preparing has high performance support type oxidation of ethanol
Catalyst.
The content of the invention
It is an object of the present invention to provide a kind of using the Graphene/carbon nanotube composite material with three-D space structure as load
Body, carried metal PtSn prepares the new method with high performance ethanol oxidation catalyst.
The present invention is first mixed the shortwall CNT of carboxylated and graphite oxide in mass ratio 1: 1~4 (mg/mg)
Close, and mixture, 80ml ethylene glycol (EG), 5ml deionized waters are subjected to mixing ultrasonic disperse 2h；By mixed liquor in N2Air-flow
Lower magnetic agitation, 80~100 DEG C of hydro-thermal reactions 20 hours, are subsequently cooled to room temperature, and reduction obtains graphene/carbon nano-tube mixing
Solution；Then, by chloroplatinic acid EG solution (0.04mol/L) and stannous chloride EG solution (0.02mol/L) by volume 1: 1~3
(mL/mL) add in above-mentioned mixed liquor, ultrasound is carried out successively and is stirred each hour, it is uniformly mixed；Then hydrogen-oxygen is used
The pH value for changing sodium EG saturated solution de-regulation solution is more than 11；Then in N2Air-flow under, the reducing metal at 120~140 DEG C
2~4h of particle；Then solution magnetic agitation is cooled to room temperature, the pH value of solution is adjusted to less than 2 using concentrated nitric acid；Hold again
After continuous stirring 20h, it is repeatedly washed successively using absolute ethyl alcohol and deionized water, 40 DEG C of vacuum drying are obtained
PtSn/ graphene-carbon nano tubes catalyst with three-dimensional structure carries out electrochemical property test.
It is a feature of the present invention that：The compound load of graphene carbon nanotube is formed between CNT insertion graphene sheet layer
Body.The CNT of introducing plays the ratio constructed ion diffusion admittance and expand load graphene as the support of graphene sheet layer
The effect of surface area, so as to improve the utilization ratio of graphene.This composite gold-supported with three-D space structure
Belong to the catalyst formed, make metallic it is smaller, it is scattered evenly, content it is higher, these features are conducive to improving ethanol
Electrocatalysis characteristic.
Embodiment
Embodiment 1：The mixing that the shortwall CNT of carboxylated and graphite oxide in mass ratio 1: 2 (mg/mg) are constituted
Thing, 80ml ethylene glycol (EG), 5ml deionized waters carry out mixing ultrasonic disperse 2h；By mixed liquor in N2Air-flow under magnetic agitation,
Reacted 20 hours at 100 DEG C, be subsequently cooled to room temperature, reduction obtain graphene/CNT mixed solution；Then, by chlorine
1: 1 (mL/mL) adds above-mentioned mix by volume for platinic acid EG solution (0.04mol/L) and stannous chloride EG solution (0.02mol/L)
Close in liquid, ultrasound is carried out successively and is stirred each hour, it is uniformly mixed；Then gone with sodium hydroxide EG saturated solutions
The pH value for adjusting solution is more than 11；Then in N2Air-flow under, the reduced metal particle 3h at 120 DEG C；Then by solution magnetic force
Stirring is cooled to room temperature, and the pH value of solution is adjusted to less than 2 using concentrated nitric acid；Persistently use anhydrous second after stirring 20h again
Alcohol and deionized water are repeatedly washed to it successively, 40 DEG C vacuum drying, obtain the PtSn/ graphenes with three-dimensional structure-
Carbon nano-tube catalyst, metal particle size is 2.09nm or so.Using 0.5mol/L sulfuric acid and 1mol/L ethanol as electrolysis
Liquid, in -0.2~1.0v voltage ranges, measures current density for 690.34mAmg-1Pt。
Embodiment 2：The shortwall CNT and graphite oxide amount ratio for changing carboxylated are 1: 1, and other conditions are with implementation
Example 1, obtains the PtSn/ graphene-carbon nano tube catalyst with three-dimensional structure, and metal particle size is 2.21nm or so.With
0.5mol/L sulfuric acid and 1mol/L ethanol are electrolyte, and in -0.2~1.0v voltage ranges, measuring current density is
571.61mA·mg-1Pt。
Embodiment 3：The shortwall CNT and graphite oxide amount ratio for changing carboxylated are 1: 3, and other conditions are with implementation
Example 1, obtains the PtSn/ graphene-carbon nano tube catalyst with three-dimensional structure, and metal particle size is 2.27nm or so.With
0.5mol/L sulfuric acid and 1mol/L ethanol are electrolyte, and in -0.2~1.0v voltage ranges, measuring current density is
493.45mA·mg-1Pt。
Embodiment 4：The shortwall CNT and graphite oxide amount ratio for changing carboxylated are 1: 4, and other conditions are with implementation
Example 1, obtains the PtSn/ graphene-carbon nano tube catalyst with three-dimensional structure, and metal particle size is 2.51nm or so.With
0.5mol/L sulfuric acid and 1mol/L ethanol are electrolyte, and in -0.2~1.0v voltage ranges, measuring current density is
457.03mA·mg-1Pt。
Embodiment 5：Change chloroplatinic acid EG solution (0.04mol/L）With stannous chloride EG solution (0.02mol/L) amount ratio
For 1: 2, other conditions be the same as Example 1 obtains the PtSn/ graphene-carbon nano tube catalyst with three-dimensional structure, metallic
Size is 2.23nm or so.Using 0.5mol/L sulfuric acid and 1mol/L ethanol as electrolyte, in -0.2~1.0v voltage ranges
It is interior, current density is measured for 559.45mAmg-1Pt。
Embodiment 6：Change chloroplatinic acid EG solution (0.04mol/L) and stannous chloride EG solution (0.02mol/L) amount ratio
For 1: 3, other conditions be the same as Example 1 obtains the PtSn/ graphene-carbon nano tube catalyst with three-dimensional structure, metallic
Size is 2.42nm or so.Using 0.5mol/L sulfuric acid and 1mol/L ethanol as electrolyte, in -0.2~1.0v voltage ranges
It is interior, current density is measured for 480.67mAmg-1Pt。
Embodiment 7：It is 130 DEG C to change reduced metal particle temperature, other conditions be the same as Example 1, obtains having three-dimensional knot
The PtSn/ graphene-carbon nano tube catalyst of structure, metal particle size is 2.48nm or so.With 0.5mol/L sulfuric acid and
1mol/L ethanol is electrolyte, in -0.2~1.0v voltage ranges, measures current density for 460.83mAmg-1Pt。
Embodiment 8：It is 140 DEG C to change reduced metal particle temperature, other conditions be the same as Example 1, obtains having three-dimensional knot
The PtSn/ graphene-carbon nano tubes catalyst of structure is carried out, and metal particle size is 2.68nm or so.With 0.5mol/L sulfuric acid
Ethanol with 1mol/L is electrolyte, in -0.2~1.0v voltage ranges, measures current density for 430.26mAmg-1Pt。
Claims (5)
1. a kind of preparation method of three-dimensional structure graphene-carbon nano tube composite carrier load PtSn catalyst, it is characterised in that：
Comprise the following steps：The shortwall CNT of graphite oxide and carboxylated is formed into graphene/carbon in ethylene glycol solution first
The mixed liquor of nanotube complex, then in the addition mixed liquor of the ionic liquid containing Pt metal and Sn will reduce instead respectively
Pt metal Sn should be loaded on graphene/carbon nano-tube complex carrier, you can obtain described platinum tin/graphene-carbon nanometer
Pipe catalyst.
2. a kind of oxidation of ethanol electricity as claimed in claim 1 urges the preparation method of agent, it is characterised in that：The CNT and
The mass ratio of graphene is 1: 1~1: 4.
3. a kind of oxidation of ethanol electricity as claimed in claim 1 urges the preparation method of agent, it is characterised in that：The hydrothermal temperature is
80~100 DEG C.
4. a kind of oxidation of ethanol electricity as claimed in claim 1 urges the preparation method of agent, it is characterised in that：The chloroplatinic acid EG is molten
The volume ratio of liquid (0.04mol/L) and stannous chloride EG solution (0.02mol/L) is 1: 1~1: 3.
5. a kind of oxidation of ethanol electricity as claimed in claim 1 urges the preparation method of agent, it is characterised in that：The virgin metal particle
Temperature be 120~140 DEG C, soaking time be 2~4h.
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| CN201710545538.4A CN107256973A (en) | 2017-06-30 | 2017-06-30 | A kind of preparation method of three-dimensional structure graphene carbon nanotube composite carrier load PtSn catalyst |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108987757A (en) * | 2018-08-17 | 2018-12-11 | 佛山皖和新能源科技有限公司 | A kind of preparation method of anode of microbial fuel cell material |
| CN112599797A (en) * | 2020-12-16 | 2021-04-02 | 上海电力大学 | Bimetallic PtSn/C catalyst for high-activity fuel cell and preparation and application thereof |
| WO2022021946A1 (en) * | 2020-07-29 | 2022-02-03 | 天津大学 | Composite electrode material for oxygen reduction reaction, preparation method and use thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108987757A (en) * | 2018-08-17 | 2018-12-11 | 佛山皖和新能源科技有限公司 | A kind of preparation method of anode of microbial fuel cell material |
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| WO2022021946A1 (en) * | 2020-07-29 | 2022-02-03 | 天津大学 | Composite electrode material for oxygen reduction reaction, preparation method and use thereof |
| CN112599797A (en) * | 2020-12-16 | 2021-04-02 | 上海电力大学 | Bimetallic PtSn/C catalyst for high-activity fuel cell and preparation and application thereof |
| CN112599797B (en) * | 2020-12-16 | 2022-06-24 | 上海电力大学 | Bimetallic PtSn/C catalyst for high-activity fuel cell and preparation and application thereof |
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