CN105576257A - Method using underwater arc discharge to prepare graphene supported Pt catalyst - Google Patents

Method using underwater arc discharge to prepare graphene supported Pt catalyst Download PDF

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Publication number
CN105576257A
CN105576257A CN201510959784.5A CN201510959784A CN105576257A CN 105576257 A CN105576257 A CN 105576257A CN 201510959784 A CN201510959784 A CN 201510959784A CN 105576257 A CN105576257 A CN 105576257A
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CN
China
Prior art keywords
graphene
catalyst
arc discharge
water
chloride solution
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Pending
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CN201510959784.5A
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Chinese (zh)
Inventor
郭俊杰
闫晓丽
章海霞
侯莹
刘培植
段培
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Taiyuan University of Technology
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Taiyuan University of Technology
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Priority to CN201510959784.5A priority Critical patent/CN105576257A/en
Publication of CN105576257A publication Critical patent/CN105576257A/en
Pending legal-status Critical Current

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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/86Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88Processes of manufacture
    • H01M4/8825Methods for deposition of the catalytic active composition
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/86Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/90Selection of catalytic material
    • H01M4/92Metals of platinum group
    • H01M4/925Metals of platinum group supported on carriers, e.g. powder carriers
    • H01M4/926Metals of platinum group supported on carriers, e.g. powder carriers on carbon or graphite
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30Hydrogen technology
    • Y02E60/50Fuel cells

Abstract

The invention relates to a method using underwater arc discharge to prepare a graphene supported Pt catalyst. The method is characterized in that graphene is used as the supporter, an underwater arc discharge one-step method is used for allowing Pt to be supported, and Pt/graphene composite material which is uniform in size and dispersion is prepared. The Pt/graphene composite material has good catalytic activity to fuel such as methanol and is quite wide in application range and quite promising in application prospect.

Description

A kind of Graphene carries Pt catalyst arc discharge in water preparation method
Technical field
The present invention relates to the arc discharge preparation method that a kind of Graphene carries metallic atom, is specifically carrier with Graphene, adopts arc discharge in water one-step method that a kind of Graphene in Pt load is carried Pt catalyst arc discharge in water preparation method.
Background technology
Direct low-carbon alcohols fuel cell (DAFC) has the advantages such as energy conversion efficiency, high power capacity and low noise, with hydrogen oxygen fuel cell or from C-H compound through chemical cracking hydrogen-oxygen fuel cell compared with, DAFC can simplify the Storage and Processing of raw material, and therefore it is the best energy donor in the fields such as national defence, space cause, communication and communications and transportation.Metal platinum (Pt) is catalyst based to methyl alcohol, and the small molecule alcohols such as ethanol have superior electrocatalysis characteristic, is the unit metal catalyst of present stage DAFC the most effective the most frequently used anodic oxidation of methanol.Selection has the carrier of material with carbon element as Pt of high-specific surface area, as carbon black, carbon nano-tube (CNTs), Graphene, surface area and the reactivity point of catalyst can be increased, Pt is made to reach better dispersion, the consumption reducing Pt increases the utilance of Pt, have also been obtained the cost improving and also reduce catalyst useful life simultaneously.
Summary of the invention
Based on above-mentioned prior art, the object of this invention is to provide oneplant Graphene and carry Pt catalyst arc discharge in water preparation method.
The concrete technical scheme realizing the object of the invention is as follows.
A kind of Graphene carries Pt catalyst arc discharge in water preparation method, and described method follows these steps to carry out:
(1) 1 gram of chloroplatinic acid is dissolved in 50ml deionized water is made into the platinum acid chloride solution that concentration is 0.039mol/L, join in brown volumetric flask;
(2) get 5ml platinum acid chloride solution to add in 10L deionized water and be made into the platinum acid chloride solution that concentration is 0.00002mol/L, join in heatproof container;
(3) adopt spectroscopically pure graphite rod to make electrode, wherein cathode diameter is 30mm, and anode diameter is 8mm, and two electrodes arrange along horizontal linear, is immersed in 30mm place under liquid level;
(4) electric current and voltage control respectively at 79A and 25V, and the gap between two electrodes must be made after the starting the arc to be 1mm;
(5) arc discharge makes anode evaporate the carbon source providing graphene-structured to grow, and in salting liquid, metal cation reduction generates Pt metallic particles simultaneously, and load is on the surface of graphene-structured;
Stop electric discharge after (6) 10 minutes, the product on solution top layer in collection container after water cooling, in vacuum drying chamber, evaporating water just obtains Graphene and carries Pt catalyst.
The Graphene realized according to above-mentioned processing step carries Pt catalyst arc discharge in water method, its innovation is to adopt Graphene to be supported on carbon material surface by Pt as carrier simultaneously, its advantage and good effect are: (1) processing step is simple, and preparation time is short; (2) use graphene nano material can improve the specific area of Pt as carrier, thus increase operation rate; (3) avoid the use of the reagent such as strong acid, highly basic, avoid the introducing of impurity in preparation process simultaneously; (4) Graphene has high conductivity, as can conduction electron efficiently during electro-catalysis carrier; (5) in the Pt/ graphene composite material of arc discharge in water synthesis, Graphene and Pt particle pretend use, are conducive to the realization of catalytic process; (6) under Graphene carrier function, the decentralization of Pt greatly improves, and the existence of carrier simultaneously decreases Pt largely and assembles; (7) use the solution of low concentration to obtain year Pt and measure high catalyst material, significantly reduce cost.
Graphene prepared by above-mentioned processing step carries Pt catalyst, by after the product mortar grinder collected, get a little ultrasonic disperse in deionized water, by hanging drop on micro-grid copper mesh, with JEM-2010 type high-resolution-ration transmission electric-lens (HRTEM after dry, accelerating voltage 200kV, point resolution 0.19nm) observation sign is carried out to it, the Pt uniform particles finding that there is a large amount of size uniformity (about 2nm) is deposited in graphene-structured.Through detecting, this Pt/ graphene complex has excellent catalytic activity to fuel such as methyl alcohol, and range of application is very wide, and application prospect is very tempting.
Accompanying drawing explanation
Fig. 1 is the HRTEM figure of Pt/ Graphene of the present invention.
Embodiment
Below the specific embodiment of the present invention is further illustrated.
Execution mode 1
A kind of Graphene carries Pt catalyst arc discharge in water preparation method, and described method is that 0.039mol/L platinum acid chloride solution adds in 15L deionized water and is made into the platinum acid chloride solution that concentration is 0.0000013mol/L by 5ml concentration, joins in heatproof container.Adopt spectroscopically pure graphite rod to make electrode, wherein cathode diameter is 30mm, and anode diameter is 8mm, and two electrodes arrange along horizontal linear, is immersed in 30mm place under liquid level.Electric current and voltage control respectively at 79A and 25V, and the gap between two electrodes must be made after the starting the arc to be 1mm.Arc discharge makes anode evaporate the carbon source providing graphene-structured to grow, and in salting liquid, metal cation reduction generates Pt metallic particles simultaneously, and load is on the surface of graphene-structured.Stop electric discharge after 10 minutes, the product after water cooling bottom collection container, evaporating water just obtains Graphene and carries Pt catalyst.
Execution mode 2
A kind of Graphene carries Pt catalyst arc discharge in water preparation method, and described method is that 0.039mol/L platinum acid chloride solution adds in 10L deionized water and is made into the platinum acid chloride solution that concentration is 0.00002mol/L by 5ml concentration, joins in heatproof container.Adopt spectroscopically pure graphite rod to make electrode, wherein cathode diameter is 30mm, and anode diameter is 8mm, and two electrodes arrange along horizontal linear, is immersed in 30mm place under liquid level.Electric current and voltage control respectively at 79A and 25V, and the gap between two electrodes must be made after the starting the arc to be 1mm.Arc discharge makes anode evaporate the carbon source providing graphene-structured to grow, and in salting liquid, metal cation reduction generates Pt metallic particles simultaneously, and load is on the surface of graphene-structured.Stop electric discharge after 10 minutes, the product after water cooling bottom collection container, evaporating water just obtains Graphene and carries Pt catalyst.
Execution mode 3
A kind of Graphene carries Pt catalyst arc discharge in water preparation method, and described method is that 0.039mol/L platinum acid chloride solution adds in 5L deionized water and is made into the platinum acid chloride solution that concentration is 0.000039mol/L by 5ml concentration, joins in heatproof container.Adopt spectroscopically pure graphite rod to make electrode, wherein cathode diameter is 30mm, and anode diameter is 8mm, and two electrodes arrange along horizontal linear, is immersed in 30mm place under liquid level.Electric current and voltage control respectively at 79A and 25V, and the gap between two electrodes must be made after the starting the arc to be 1mm.Arc discharge makes anode evaporate the carbon source providing graphene-structured to grow, and in salting liquid, metal cation reduction generates Pt metallic particles simultaneously, and load is on the surface of graphene-structured.Stop electric discharge after 10 minutes, the product after water cooling bottom collection container, evaporating water just obtains Graphene and carries Pt catalyst.

Claims (1)

1. Graphene carries a Pt catalyst arc discharge in water preparation method, and described method follows these steps to carry out:
(1) 1 gram of chloroplatinic acid is dissolved in 50ml deionized water is made into the platinum acid chloride solution that concentration is 0.039mol/L, join in brown volumetric flask;
(2) get 5ml platinum acid chloride solution to add in 10L deionized water and be made into the platinum acid chloride solution that concentration is 0.00002mol/L, join in heatproof container;
(3) adopt spectroscopically pure graphite rod to make electrode, wherein cathode diameter is 30mm, and anode diameter is 8mm, and two electrodes arrange along horizontal linear, is immersed in 30mm place under liquid level;
(4) electric current and voltage control respectively at 79A and 25V, and the gap between two electrodes must be made after the starting the arc to be 1mm;
(5) arc discharge makes anode evaporate the carbon source providing graphene-structured to grow, and in salting liquid, metal cation reduction generates Pt metallic particles simultaneously, and load is on the surface of graphene-structured;
Stop electric discharge after (6) 10 minutes, the product on solution top layer in collection container after water cooling, in vacuum drying chamber, evaporating water just obtains Graphene and carries Pt catalyst.
CN201510959784.5A 2015-12-21 2015-12-21 Method using underwater arc discharge to prepare graphene supported Pt catalyst Pending CN105576257A (en)

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Application Number Priority Date Filing Date Title
CN201510959784.5A CN105576257A (en) 2015-12-21 2015-12-21 Method using underwater arc discharge to prepare graphene supported Pt catalyst

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106645340A (en) * 2017-01-04 2017-05-10 太原理工大学 Method for detecting carmine in food by using graphene-loaded Pt single-atom composite material
CN106680355A (en) * 2017-01-04 2017-05-17 太原理工大学 Method for detecting sunset yellow in food by using carbon onion-loaded Pt nano particle composite material

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101007273A (en) * 2007-01-26 2007-08-01 太原理工大学 In-situ synthesis of Pt-supported fullerene catalyst
CN102895997A (en) * 2012-10-25 2013-01-30 天津大学 Preparation method for direct methanol fuel cell supported Pt-based anode catalyst
JP2013099707A (en) * 2011-11-07 2013-05-23 Toyota Motor Corp Method of manufacturing ionomer-coated catalyst-supporting carbon nanotube
CN103480413A (en) * 2013-09-30 2014-01-01 江苏大学 Preparation method of cationic polymer functionalized graphene-loaded platinum nanocomposite

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101007273A (en) * 2007-01-26 2007-08-01 太原理工大学 In-situ synthesis of Pt-supported fullerene catalyst
JP2013099707A (en) * 2011-11-07 2013-05-23 Toyota Motor Corp Method of manufacturing ionomer-coated catalyst-supporting carbon nanotube
CN102895997A (en) * 2012-10-25 2013-01-30 天津大学 Preparation method for direct methanol fuel cell supported Pt-based anode catalyst
CN103480413A (en) * 2013-09-30 2014-01-01 江苏大学 Preparation method of cationic polymer functionalized graphene-loaded platinum nanocomposite

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106645340A (en) * 2017-01-04 2017-05-10 太原理工大学 Method for detecting carmine in food by using graphene-loaded Pt single-atom composite material
CN106680355A (en) * 2017-01-04 2017-05-17 太原理工大学 Method for detecting sunset yellow in food by using carbon onion-loaded Pt nano particle composite material
CN106645340B (en) * 2017-01-04 2019-06-28 太原理工大学 With method carmine in the monatomic composite material detection food of graphene-supported Pt
CN106680355B (en) * 2017-01-04 2019-06-28 太原理工大学 Utilize the method for sunset yellow in carbon onion supporting Pt nano particle composite material detection food

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