CN101362093B - Carbon supported platinum composite catalyst of fuel cell and preparation method thereof - Google Patents
Carbon supported platinum composite catalyst of fuel cell and preparation method thereof Download PDFInfo
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- CN101362093B CN101362093B CN2008101987477A CN200810198747A CN101362093B CN 101362093 B CN101362093 B CN 101362093B CN 2008101987477 A CN2008101987477 A CN 2008101987477A CN 200810198747 A CN200810198747 A CN 200810198747A CN 101362093 B CN101362093 B CN 101362093B
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- 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 provides a fuel cell carbon platinum-carried compound catalyst with small amount of platinum and high catalytic activity, and a preparation method thereof. The compound catalyst is added with a cocatalyst ingredient, hydrogen tungsten gunmetal or hydrogen molybdenum gunmetal on the basis of a normal carbon platinum-carried compound catalyst. The preparation method of the compound catalyst comprises the steps that under appropriate temperature and acidity, tungstate or molybdate is added into a platinum compound solution and then chemical reduction reaction is carried out under the existence of a reducing agent to obtain the catalyst. The compound catalyst provided by the invention not only promotes the electro-catalytic activity of the platinum catalyst, and reduces the amount of the noble metal platinum, but also probably raises the reaction rate of catalyzed oxygen reduction under the condition of certain methanol concentration. The preparation method of the compound catalyst is simple in technology, convenient for operation, easy to be controlled and has low cost.
Description
Technical field
The invention belongs to fuel cell material manufacturing and electro-catalysis technical field.Be specifically related to a kind of carbon supported platinum composite catalyst of fuel cell simple to operation and preparation method thereof.
Background technology
DMFC is a kind of of Proton Exchange Membrane Fuel Cells, is electrolyte with the solid polymer membrane, uses liquid or gas methyl alcohol to act as a fuel.Have advantages such as pollution-free, clean and effective, do not reform or reforming unit in the middle of DMFC does not need in addition, in light weight, volume is little, battery design and simple to operate.
In DMFC, carbon supported platinum catalyst is often used as the eelctro-catalyst of cathodic oxygen reduction and anode methanol oxidation, and this mainly is to make Pt have big surface area, and helps obtaining high electro catalytic activity.The carbon carrier of high surface can make the decentralization of Pt higher as graphite, carbon black, activated carbon etc.Because noble metal platinum costs an arm and a leg, scarcity of resources has limited its practical application and commercialization, thus must take suitable preparation method and process conditions to reduce the consumption of platinum, and improve its catalytic activity and utilization rate.Document [Damia ' n A.Scherlis, Young Joo Lee, Carme Rovira, et al.Solid State Ionics[J], Concerning the origin of superstructures in hydrogen molybdenum bronzes H
xMoO
3, 2004 (168): 291-298.] and put down in writing hydrogen molybdenum bronze (H
xMoO
3) self have a proton owe to take off character; Document [Y.M.Wu, W.S.Li, J.Lu, et al.Journal of Power Sources[J], Electrocatalyticoxidation of small organic molecules on polyaniline-Pt-H
xMoO
3, 2005 (145): 286-291.] in mention hydrogen molybdenum bronze and self owe to take off the character of proton hydrogen reduction is had facilitation.Hydrogen tungsten bronze (H
xWO
3) similar with hydrogen molybdenum bronze, also possess self the character of owing to take off proton, so add auxiliary catalysis composition hydrogen tungsten bronze or hydrogen molybdenum bronze is expected to reduce the consumption of noble metal platinum and improves its catalyst activity.
Summary of the invention
The object of the invention is to provide a kind of carbon supported platinum composite catalyst of fuel cell, and this catalyst particle size is evenly distributed, the consumption of noble metal platinum is few and electro catalytic activity is high.
Another purpose of the present invention is to provide a kind of method for preparing above-mentioned composite catalyst, and this method is with low cost, environmental friendliness, and technological process is simple to operation, and process is easy to control.
Purpose of the present invention is achieved through the following technical solutions:
Carbon supported platinum composite catalyst of fuel cell provided by the invention, this catalyst comprise carbon carrier and platinum component as common carbon supported platinum catalyst, be characterized in also comprising helping catalyst component hydrogen tungsten bronze or hydrogen molybdenum bronze.
Platinum content preferred 10～20% in the above-mentioned catalyst.
The amount of substance of above-mentioned hydrogen tungsten bronze or hydrogen molybdenum bronze is that 10～40 times of amount of substance of above-mentioned amber are for good.
Above-mentioned carbon carrier is CNT, active carbon, acetylene black or graphite.
The preparation method of carbon supported platinum composite catalyst of fuel cell provided by the invention specifically can comprise the steps:
(1) contains in the platinum-like compounds solution and add complexing agent, add thermal agitation 4～5h, make the complete complexing of platinum and part;
(2) the pH value of regulating step (1) gained solution adds 10～40 times of above-mentioned tungstates or molybdates that contain the platinum-like compounds amount of substance 9～11;
(3) add a certain amount of carbon carrier in step (2) gained solution, heat ultrasonic 1～2h;
(4) slowly drip reductant solution under the strong agitation, continue to stir 2～3h simultaneously;
(5) filter, washing, 60～80 ℃ are drying to obtain product;
Above-mentioned institute all carries out under normal pressure in steps.
In the above-mentioned steps (1), containing platinum-like compounds is chloroplatinic acid, and complexing agent is ethylenediamine tetra-acetic acid (EDTA), sodium tartrate or imidazoles, and the complexing agent addition is identical with the chloroplatinic acid amount of substance.
In the above-mentioned steps (3), carbon carrier is CNT, active carbon, acetylene black or graphite, and its addition is calculated according to the required platinum content of product.
In the above-mentioned steps (4), reductant solution is sodium borohydride, formaldehyde, natrium citricum, sodium formate or ascorbic acid solution, and the reducing agent addition is the amount of substance of 1～1.5 times of chloroplatinic acid.
Simple principle of the present invention is as follows: composite catalyst of the present invention has very high electrochemical catalysis activity, the carbon supported platinum composite catalyst that contains hydrogen tungsten bronze and hydrogen molybdenum bronze is during as the DMFC eelctro-catalyst, because the proton embedding of hydrogen tungsten bronze and hydrogen molybdenum bronze self/take off function is all played very strong facilitation to methanol oxidation and oxygen reduction when proton embeds and deviates from the composite catalyzing agent material.And because methanol oxidation is had very high catalytic activity, when small amount of methanol existed, the cathodic oxygen reduction reaction was influenced hardly, and this also provides a new approach for solving the methanol crossover problem.
Compared with prior art, the present invention has following beneficial effect: composite catalyst of the present invention has improved the utilization rate of noble metal platinum, has reduced catalyst consumption, and has kept higher electrocatalysis characteristic.Preparation method provided by the invention is succinct, efficient, easy operating, cost are cheap relatively, can satisfy the development and utilization in electro-catalysis, pem cell field, use and the value of exploitation huge.
Description of drawings
Fig. 1 is the platinum catalyst (a) that obtains of embodiment 1 and the cyclic voltammogram of platinum-hydrogen tungsten bronze composite catalyst (b) catalysis methanol oxidation.
Fig. 2 is the platinum catalyst (a) that obtains of embodiment 1 and the cyclic voltammogram of platinum-hydrogen molybdenum bronze composite catalyst (b) catalysis methanol oxidation.
Fig. 3 is that the platinum catalyst that obtains of embodiment 1 and the linearity of platinum-hydrogen tungsten bronze composite catalyst catalytic cathode hydrogen reduction are swept curve.
Fig. 4 is that the linearity of the platinum catalyst that obtains of embodiment 1 and platinum-hydrogen molybdenum bronze composite catalyst catalytic cathode hydrogen reduction is swept curve.
Fig. 5 be platinum-hydrogen tungsten bronze composite catalyst that embodiment 1 obtains having/no methyl alcohol in the presence of the linear scan curve of catalytic cathode hydrogen reduction.
Fig. 6 be the platinum that obtains of embodiment 1-hydrogen molybdenum bronze composite catalyst having/no methyl alcohol in the presence of the linear scan curve of catalytic cathode hydrogen reduction.
Fig. 7 is that the linearity of the platinum catalyst that obtains of embodiment 2 and platinum-hydrogen molybdenum bronze composite catalyst catalytic cathode hydrogen reduction is swept curve.
Fig. 8 is that the linearity of the platinum catalyst that obtains of embodiment 3 and platinum-hydrogen molybdenum bronze composite catalyst catalytic cathode hydrogen reduction is swept curve.
The specific embodiment
The present invention is described in further detail below in conjunction with embodiment, but the working of an invention mode is not limited thereto.
At first preparation does not contain the common carbon supported platinum catalyst product in contrast that help catalyst component hydrogen tungsten bronze or hydrogen molybdenum bronze, may further comprise the steps:
(1) the 12.82ml chloroplatinic acid is placed the 50ml volumetric flask, add identical respectively with the chloroplatinic acid amount of substance or two times EDTA as complexing agent, add thermal agitation 3～4h, make platinum and part finish complexing.
(2) the pH value of regulating mixed solution stirs between 9～11.
(3) add the 100mg CNT, heat ultrasonic 1～2h.
(4) slowly drip sodium borohydride solution under the strong agitation, continue to stir 2h.
(5) use the second distillation water washing behind the vacuum filtration, filter, 70 ℃ of dryings in vacuum drying chamber make the catalyst of platinum content 20% in theory then.
Prepare carbon supported platinum composite catalyst of the present invention, may further comprise the steps:
(1) the 12.82ml chloroplatinic acid is placed the 50ml volumetric flask, add the EDTA of or two times amount of substances identical respectively, add thermal agitation 3～4h, make platinum and part finish complexing with platinum.
(2) the pH value of regulating mixed solution is between 9～11, and adding 11.4ml concentration is 200mol.L
-1Sodium tungstate or sodium molybdate, stir.
(3) add the 100mg CNT, heat ultrasonic 1～2h.
(4) slowly drip sodium borohydride solution under the strong agitation, continue to stir 2h.
(5) use the second distillation water washing behind the vacuum filtration, filter, 70 ℃ of dryings in vacuum drying chamber make the platinum of platinum content 20%-hydrogen tungsten bronze composite catalyst and platinum-hydrogen molybdenum bronze composite catalyst in theory then.
Take by weighing three kinds of each 1mg of catalyst respectively, get the 1ml mass fraction and be 5% naphthols ethanolic solution and size mixing, be dissolved in surely in the 2ml reagent bottle, the heating ultrasonic wave disperses 3h, pipette 5 μ l at every turn and be applied to the glass-carbon electrode surface that purified treatment is crossed, drying is carried out electro-chemical test.The electro-chemical test condition is as follows: each electrode that scribbles catalyst is at first at 0.5mol.L
-1H
2SO
4The cyclic voltammetric activation is 10 times in the solution; Partial electrode is at 1mol.L then
-1Carry out the catalysis methanol experiment in the methanol solution, sweep speed: 50mV.s
-1Partial electrode is at the saturated 0.5mol.L of oxygen
-1H
2SO
4Carry out hydrogen reduction linear scan in the solution, sweep speed: 5mV.s
-1, the speed of rotation: 800rpm; Part is carried out 50mol.L
-1Hydrogen reduction linear scan under the methyl alcohol, electrochemical parameter is the same.
A and b are respectively the curve of platinum catalyst and platinum-hydrogen tungsten bronze composite catalyst catalysis methanol oxidation among Fig. 1, and a and b are respectively the curve of platinum catalyst and platinum-hydrogen molybdenum bronze composite catalyst catalysis methanol oxidation among Fig. 2; Two curves among Fig. 3 are respectively the linear scan curve of platinum catalyst and platinum-hydrogen tungsten bronze composite catalyst catalytic cathode hydrogen reduction, and two curves among Fig. 4 are respectively the linear scan curve of platinum catalyst and platinum-hydrogen molybdenum bronze composite catalyst catalytic cathode hydrogen reduction.Contrast four sets of curves as can be known, the peak current of the methanol oxidation of composite catalyst and hydrogen reduction electro-catalysis electric current are all a lot of than exceeding of platinum catalyst.This is because there is following proton-exchange reaction in the composite catalyst:
0＜y＜x≤2
H
xMoO
3Or H
xWO
3Oxidation reaction takes place, and plays proton and supplies with body; On the contrary, H
xMoO
3Or H
xWO
3Reduction reaction takes place, and plays proton accepter.So proton owing in composite catalyst taken off the reaction rate of having accelerated oxidization of methanol and oxygen reduction.Illustrate that composite catalyst all has electro catalytic activity efficiently to methanol oxidation and hydrogen reduction.
In the comparison diagram 5 and 6 two sets of curves as can be known, at 50mol.L
-1When methyl alcohol existed, the activity of composite catalyst catalytic oxidation-reduction did not all have to reduce, and all increases to some extent on the contrary.The curve of composite catalyst a very little methanol oxidation peak occurs at 0.4V among Fig. 5; The curve take-off potential of composite catalyst does not change among Fig. 6, but the hydrogen reduction electric current between 0.6～0.4V reduces to some extent, and this is the hydrogen reduction electric current because methanol oxidation has disappeared mutually, and the hydrogen reduction electric current still increases when not having methyl alcohol to exist a lot after the 0.4V.The activity that composite catalyst catalytic oxidation-reduction when finite concentration methyl alcohol exists is described can not be affected.This proposes a new developing direction for solving the methanol crossover problem.
Present embodiment except that following characteristics with embodiment 1:
The preparation of carbon supported platinum catalyst reference substance:
Step (1) is used the 5.85ml chloroplatinic acid instead, makes the platinum catalyst reference substance of platinum content 10% in theory.
The preparation of carbon supported platinum composite catalyst of the present invention:
Step (1) is used the 5.85ml chloroplatinic acid instead; The addition of step (2) sodium tungstate or sodium molybdate is 2.85ml, and concentration is 200mol.L
-1.Make the platinum composite catalyst of platinum content 10% in theory.As shown in Figure 7, the peak current of platinum-hydrogen molybdenum bronze composite catalyst catalysis methanol oxidation is 30mA.cm
-2, and the peak current of platinum catalyst catalysis methanol oxidation is 15mA.cm separately
-2, platinum-hydrogen molybdenum bronze composite catalyst activity has improved 100%, and the performance of platinum-hydrogen tungsten bronze composite catalyst is close therewith.
Embodiment 3
Present embodiment except that following characteristics with embodiment 1:
The preparation of carbon supported platinum catalyst reference substance:
Step (1) is used the 10ml chloroplatinic acid instead, makes the carbon supported platinum catalyst reference substance of platinum content 17% in theory.
The preparation of carbon supported platinum composite catalyst of the present invention:
Step (1) is used the 10ml chloroplatinic acid instead; The addition of step (2) sodium tungstate or sodium molybdate is 4.87ml, and concentration is 200mol.L
-1.Make the composite catalyst of the present invention of platinum content 17% platinum in theory.As shown in Figure 8, platinum-hydrogen molybdenum bronze composite catalyst catalysis methanol oxidation peak current is 20mA.cm
-2, platinum catalyst catalysis methanol peak current is 17mA.cm separately
-2, the composite catalyst activity has improved 17%, and platinum-hydrogen tungsten bronze performance is close therewith.
Comparing embodiment 1,2 and 3 as seen, to be that 10% composite catalyst is active improve at most theoretical platinum content, this may be because the platinum carrying capacity is the cause that platinum more disperses in 10% the composite catalyst.This preparation for the low efficient platinum catalyst of carrying capacity provides an approach.
Present embodiment except that following characteristics with embodiment 1:
Adding sodium tungstate or sodium molybdate are 12.62ml in the step (2), and concentration is 200mol.L
-1
The performance of the platinum that obtains-hydrogen tungsten bronze composite catalyst or platinum-hydrogen molybdenum bronze composite catalyst and embodiment 1 gained catalyst is close.
Present embodiment except that following characteristics with embodiment 1:
Adding sodium tungstate or sodium molybdate are 25.24ml in the step (2), and concentration is 200mol.L
-1
The performance of the platinum that obtains-hydrogen tungsten bronze composite catalyst or platinum-hydrogen molybdenum bronze composite catalyst and embodiment 1 gained catalyst is close.
Present embodiment except that following characteristics with embodiment 1:
Complexing agent changes and makes the imidazoles identical with the chloroplatinic acid amount of substance in the step (1).
The performance of the platinum that obtains-hydrogen tungsten bronze composite catalyst or platinum-hydrogen molybdenum bronze composite catalyst and embodiment 1 gained catalyst is close.
Embodiment 7
Present embodiment except that following characteristics with embodiment 1:
Complexing agent changes and makes the sodium tartrate identical with the chloroplatinic acid amount of substance in the step (1).
The performance of the platinum that obtains-hydrogen tungsten bronze composite catalyst or platinum-hydrogen molybdenum bronze composite catalyst and embodiment 1 gained catalyst is close.
Present embodiment except that following characteristics with embodiment 1:
CNT in the step (1) changes active carbon into.
The performance of the platinum that obtains-hydrogen tungsten bronze composite catalyst or platinum-hydrogen molybdenum bronze composite catalyst and embodiment 1 gained catalyst is close.
Embodiment 9
Present embodiment except that following characteristics with embodiment 1:
CNT in the step (1) changes acetylene black into.
The performance of the platinum that obtains-hydrogen tungsten bronze composite catalyst or platinum-hydrogen molybdenum bronze composite catalyst and embodiment 1 gained catalyst is close.
Present embodiment except that following characteristics with embodiment 1:
CNT in the step (1) changes graphite into.
The performance of the platinum that obtains-hydrogen tungsten bronze composite catalyst or platinum-hydrogen molybdenum bronze composite catalyst and embodiment 1 gained catalyst is close.
Embodiment 11
Present embodiment except that following characteristics with embodiment 1:
Sodium borohydride solution in the step (4) changes formalin into, and the formaldehyde addition is the amount of substance of 1.5 times of chloroplatinic acids.
The performance of the platinum that obtains-hydrogen tungsten bronze composite catalyst or platinum-hydrogen molybdenum bronze composite catalyst and embodiment 1 gained catalyst is close.
Embodiment 12
Present embodiment except that following characteristics with embodiment 1:
Sodium borohydride solution in the step (4) changes sodium citrate solution into, and the natrium citricum addition is the amount of substance of 1 times of chloroplatinic acid.
The performance of the platinum that obtains-hydrogen tungsten bronze composite catalyst or platinum-hydrogen molybdenum bronze composite catalyst and embodiment 1 gained catalyst is close.
Embodiment 13
Present embodiment except that following characteristics with embodiment 1:
Sodium borohydride solution in the step (4) changes EWNN solution into.
The performance of the platinum that obtains-hydrogen tungsten bronze composite catalyst or platinum-hydrogen molybdenum bronze composite catalyst and embodiment 1 gained catalyst is close.
Embodiment 14
Present embodiment except that following characteristics with embodiment 1:
The baking temperature of step (5) is 60 ℃.
The performance of the platinum that obtains-hydrogen tungsten bronze composite catalyst or platinum-hydrogen molybdenum bronze composite catalyst and embodiment 1 gained catalyst is close.
Present embodiment except that following characteristics with embodiment 1:
The baking temperature of step (5) is 80 ℃.
The performance of the platinum that obtains-hydrogen tungsten bronze composite catalyst or platinum-hydrogen molybdenum bronze composite catalyst and embodiment 1 gained catalyst is close.
The foregoing description is a preferred implementation of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spiritual essence of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (5)
1. carbon supported platinum composite catalyst of fuel cell, its component comprises carbon carrier and platinum, it is characterized in that: its component also comprises hydrogen tungsten bronze or hydrogen molybdenum bronze;
The content of described platinum is 10～20%;
The content of described hydrogen tungsten bronze or hydrogen molybdenum bronze is the amount of substance of 10～40 times of described platinum;
Described carbon supported platinum composite catalyst of fuel cell prepares by the method that comprises following steps:
(1) contains in the platinum-like compounds solution and add complexing agent, add thermal agitation 4～5h, make the complete complexing of platinum and part;
(2) the pH value of regulating step (1) gained solution adds 10～40 times of above-mentioned tungstates or molybdates that contain the platinum-like compounds amount of substance 9～11;
(3) add carbon carrier in step (2) gained solution, heat ultrasonic 1～2h;
(4) slowly drip reductant solution under the strong agitation, continue to stir 2～3h simultaneously;
(5) filter, washing, 60～80 ℃ are drying to obtain product;
Above-mentioned institute all carries out under normal pressure in steps;
In the described step (1), containing platinum-like compounds is chloroplatinic acid, and complexing agent is ethylenediamine tetra-acetic acid, sodium tartrate or imidazoles, and the complexing agent addition is identical with the chloroplatinic acid amount of substance.
2. according to the described carbon supported platinum composite catalyst of fuel cell of claim 1, it is characterized in that: described carbon carrier is CNT, active carbon, acetylene black or graphite.
3. the preparation method of claim 1 or 2 described carbon supported platinum composite catalyst of fuel cell is characterized in that comprising following concrete steps:
(1) contains in the platinum-like compounds solution and add complexing agent, add thermal agitation 4～5h, make the complete complexing of platinum and part;
(2) the pH value of regulating step (1) gained solution adds 10～40 times of above-mentioned tungstates or molybdates that contain the platinum-like compounds amount of substance 9～11;
(3) add carbon carrier in step (2) gained solution, heat ultrasonic 1～2h;
(4) slowly drip reductant solution under the strong agitation, continue to stir 2～3h simultaneously;
(5) filter, washing, 60～80 ℃ are drying to obtain product;
Above-mentioned institute all carries out under normal pressure in steps;
In the described step (1), containing platinum-like compounds is chloroplatinic acid, and complexing agent is ethylenediamine tetra-acetic acid, sodium tartrate or imidazoles, and the complexing agent addition is identical with the chloroplatinic acid amount of substance.
4. according to the preparation method of the described carbon supported platinum composite catalyst of fuel cell of claim 3, it is characterized in that: in the described step (3), carbon carrier is CNT, active carbon, acetylene black or graphite, and its addition is calculated according to the required platinum content of product.
5. according to the preparation method of the described carbon supported platinum composite catalyst of fuel cell of claim 3, it is characterized in that: in the described step (4), reductant solution is sodium borohydride, formaldehyde, natrium citricum, sodium formate or ascorbic acid solution, and the reducing agent addition is the amount of substance of 1～1.5 times of chloroplatinic acid.
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| CN102762297B (en) * | 2010-02-05 | 2015-06-10 | 巴斯夫欧洲公司 | Process for producing a catalyst and catalyst |
| CN102513130A (en) * | 2011-12-05 | 2012-06-27 | 广东工业大学 | Preparation method and application of integral combustion catalyst for platinum-based honeycomb iron-chrome-aluminium wire mesh |
| CN103515620B (en) * | 2012-06-20 | 2015-09-30 | 江苏氢阳能源有限公司 | A kind of electrode material, its application, direct fuel cell and electrochemical hydrogenation electrolysis tank |
| CN103606687B (en) * | 2013-11-26 | 2015-08-26 | 华南师范大学 | A kind of anode catalyst porous array Pt-p-H for direct methanol fuel cell xmoO 3and preparation method thereof |
| CN108963273B (en) * | 2018-06-27 | 2022-01-18 | 华南理工大学 | Branch-shaped platinum electrocatalyst and preparation method and application thereof |
| CN111834642B (en) * | 2019-04-15 | 2021-12-17 | 武汉氢阳能源有限公司 | Organic matter electrocatalytic oxidation catalyst and preparation method and application thereof |
| CN112877728B (en) * | 2020-12-10 | 2022-08-09 | 上海航天智慧能源技术有限公司 | Platinum-carbon-layer-containing loaded foam nickel electrolytic water electrode and preparation method thereof |
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