CN101596453A - A kind of is the Pt Preparation of catalysts method of carrier with the carbon carrier - Google Patents
A kind of is the Pt Preparation of catalysts method of carrier with the carbon carrier Download PDFInfo
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Abstract
The invention belongs to fuel cell field.The present invention relates to a kind of is the Pt Preparation of catalysts method of carrier with the carbon carrier, and comprise following each step: configuration concentration is the glucose solution of 50g/l; With adding concentration in the glucose solution is the XC-72 of 0.433g/l～1.677g/l, makes that the two mass ratio is 30～100, changes in the reactor, and 160 ℃ are reacted 12h down, the water washing of product distill repeatedly is totally promptly got complex carrier C/XC-72; With the complex carrier C/XC-72 and the concentration of above-mentioned preparation is 10g/l H
2PtCl
6Press mass ratio 0.5～2 and mix, add polyvinylpyrrolidone and cook protective agent, wherein the mass ratio of polyvinylpyrrolidone and C/XC-72 is 1: 4, after stirring, adds hot reflux 4h, obtains catalyst Pt/C/XC-72.The present invention can realize autoreduction by the characteristic of support C/XC-72 itself, and the Pt slaine is reduced into the Pt nano particle, and hydrogen reduction is had good catalytic action.
Description
Technical field
The present invention relates to a kind ofly be used for cathode in direct methanol fuel cells hydrogen reduction carbon carrier and be the Pt Preparation of catalysts method of carrier, belong to fuel cell material science and technology field and electro-catalysis technical field with it.
Background technology
DMFC (DMFC) be with polymer film as electrolytical new proton exchange film fuel battery, be on the basis of Proton Exchange Membrane Fuel Cells, to grow up.DMFC is made of methyl alcohol anode, oxygen cathode and PEM.Anode and cathode electrode catalyst commonly used are respectively PtRu/C and Pt/C noble metal catalyst.The invertibity of cathodic oxygen reduction reaction is very little, the theoretical current potential of its 4 electronic reduction reaction is 1.23V, even but use precious metals pt, oxygen electrode catalyst surfaces such as Pd, at open-circuit condition, its overpotential is also about 0.2V, in DMFC, because methanol crossover to negative electrode causes mixed potential, and make the OCP 0.1V that descends at least, therefore for DMFC, open-circuit condition only, negative electrode just loses about 25% energy.And the dynamic process of oxygen reduction reaction is 4 complicated electron reactions, occurs multiple intermediate state particle in the reaction mechanism mechanism of reaction, as: hydrogen peroxide, intermediate state contain oxygen adsorbing species or metal oxide etc.Particularly when hydrogen peroxide occurring, at least simultaneously there are three pairs of redox systems, consider from the thermodynamics angle, hydrogen peroxide is unsettled middle particle, its concentration is almost always by dynamics but not thermodynamics decision, therefore cause the reaction mechanism mechanism of reaction quite complicated, this complicated course is further complicated owing to the oxidation reaction of the alcohols generation that infiltrates into negative electrode.Therefore, no matter research still be that the commercialized development of DMFC all is extremely important in the basic research field to the highly active fuel battery cathod catalyst of hydrogen reduction.
With regard to DMFC, the cathod catalyst of research mainly contains the Pt catalyst at present, the Pt/C catalyst, the Pt-M catalyst, Pt-M/C multi-component alloy catalytic agent (M=Cr, Co, Ni, V, Ti, Fe etc.), transition metal macrocyclic compound catalyst (phthalein cyanogen (Pc), tetraphenylporphyrin (TPP), tetramethylphenyl porphyrin (TMPP) etc.), transition metal sulfide catalyst (the transient metal sulfide of chevrel phase, the non-qualitative transient metal sulfide of active carbon adsorption), the front is referred to as the noble metal catalyst series for four kinds, and back two kinds are called the base metal catalyst series.Non-precious metal catalyst is because its cost is low also was widely studied in recent years, but that ubiquity catalytic activity is not high, the shortcoming that stability is low.What have most at present practical future remains the noble metal carbon-carried platinum-based catalyst, and platinum group catalyst is considered to best oxygen reduction catalyst.Being its stability in the highly acid electrolyte on the one hand, is that it self has very high ORR catalytic activity on the other hand.Because Pt costs an arm and a leg, therefore resource-constrained will realize the commercialization of fuel cell, must further reduce the use amount of platinum, and improve catalytic performance.For improving the cathodic oxygen reduction activity, researcher mainly addresses this problem from following two aspects: the alloy of on the one hand synthetic Pt and transition metal
[1]Yolanda Vasquez, Amandeep K.Sra, and Raymond E.Schaak One-PotSynthesis of Hollow Superparamagnetic CoPt Nanospheres.J.AM.CHEM.SOC.2005,127,12504-12505 selects the suitable Pt/C catalyst that the carbon carrier preparation is uniformly dispersed, particle is tiny on the other hand
[2]Jinghong Li, Zhenhai Wen.Core/Shell Pt/CNanoparticles Embedded in Mesoporous Carbon as a Methanol-TolerantCathode Catalyst in Direct Methanol Fuel Cell[J].
Adv.Mater.2008.20.743-747，Pt-M/C
[3]Hui?Yang，Walter?Vogel，ClaudeLamy，and?Nicola′s?Alonso-Vante.Structure?and?ElectrocatalyticActivity?of?Carbon-Supported?Pt-Ni?Alloy?Nanoparticles?Toward?theOxygen?Reduction?React?ion[J].J.Phys.Chem.B?2004，108，11024-11034。Carbon carrier commonly used has Vulcan XC-72 or CNT etc.Though these carbon carriers have good dispersiveness, but because the hydrophobicity on surface, make that loading process is difficult for carrying out, generally need modify its surface, promptly boil or add heat soaking a few hours with strong oxidizing property material such as concentrated acid or concentrated base etc., make its surface generation-OH ,-COOH, functional groups such as-C=O increase its surperficial hydrophilic functional groups and the loading process that helps metal carries out.In addition, when carried metal, often need to add various reducing agents and make the chloroplatinic acid reduction, make the Pt/C catalyst attached to carrier surface thereby generate platinum nanoparticles.From above introduction as can be seen, its process of these methods is complicated, and makes operation have certain danger owing to needing use to have corrosive strong oxidation material and reducing agent etc., causes environment unfriendly simultaneously.
Seek a kind of carbon carrier and both had good dispersiveness, do not need simultaneously to use the strong oxidizing property material to carry out the functionalization on surface, and the surface nature of utilizing carrier itself to have prepares good dispersion under the condition that does not add any reducing agent, and the Pt/ carbon carrier catalyst that particle is tiny all will have great importance to practicability and the theoretical research that promotes DMFC.
Summary of the invention
The purpose of this invention is to provide a kind of novel carbon carrier (C/XC-72) [4] YuJJ with autoreduction performance, Du W, Zhao FQ, Zeng BZ High sensitive simultaneous determinationof catechol and hydroquinone at mesoporous carbon CMK-3 electrode incomparison with multi-walled carbon nanotubes and Vulcan XC-72 carbonelectrodes[J] .Electrochimica acta.2009.54.984-988 and be the Pt/C/XC-72 Preparation of catalysts method of carrier with it.Preparation method of the present invention adopts nontoxic glucose to handle carbon carrier Vulcan XC-72 commonly used, make the novel carriers of favorable dispersibility, this carrier does not need any activation processing is carried out on its surface, simultaneously do not need to add any reducing agent yet, adopt the simple heating reflow method just chloroplatinic acid can be reduced, thereby prepare Pt/C/XC-72 catalyst with good dispersion and good electric chemical property.This method technology is simple, and operation is easily gone, and is nontoxic, with low cost and environmental friendliness.
It is the Pt/C/XC-72 Preparation of catalysts method of carrier that a kind of autoreduction support C/XC-72 that the present invention proposes reaches with it.It is characterized in that adopting nontoxic glucose to handle carbon carrier VulcanXC-72 commonly used, make the novel carriers of favorable dispersibility, utilize the surface nature of this carrier itself under the condition that does not add any reducing agent, to prepare the catalyst of function admirable, comprise following each step:
1, configuration concentration is the glucose solution of 50g/l.
2, be the XC-72 (U.S. cabot company) of 0.433g/l～1.677g/l with adding concentration in the above-mentioned glucose solution that makes, make that the two mass ratio is 30～100, change in the reactor, 160 ℃ of following reaction 12h, the complex carrier C/XC-72 that the water washing of product distill repeatedly is totally promptly made.
3, with the complex carrier C/XC-72 and the H of above-mentioned preparation
2PtCl
6(10g/l) press mass ratio 0.5～2 and mix, (PVP, 0.167g/l), wherein the mass ratio of PVP: C/XC-72 is 1: 4, after stirring, adds hot reflux 4h, obtains catalyst Pt/C/XC-72 to add polyvinylpyrrolidone.
Below in conjunction with accompanying drawing effect of the present invention is described:
Fig. 1 is the SEM figure of Vulcan XC-72, and as can be seen from the figure, this carbon powder particle is of a size of 40nm.Fig. 2 is that we adopt glucose to coat the SEM figure of the novel carriers C/XC-72 of Vulcan XC-72 preparation down for the carbon source hydrothermal condition, this particle size is 90nm, compare original Vulcan XC-72 particle, its size increases, and illustrates that we have successfully coated the carbon film that generates after one deck glucose aromatisation and the carbonization in the outside of XC-72.Fig. 3 is with Vulcan XC-72 and H
2PtCl
6The XRD figure that directly adds the product of hot reflux, the crystal characteristic diffraction maximum that Pt as can be seen from the figure between 10 °～90 °, do not occur, the carbon peak that some carbon carriers itself just occurred illustrates that Vulcan XC-72 carrier itself does not have the performance that chloroplatinic acid is reduced to metal Pt under this reaction condition.Fig. 4 is with complex carrier C/XC-72 and H
2PtCl
6The XRD figure that under similarity condition, adds the product of hot reflux.As can be seen from the figure, between 10 °～90 ° of sweep limits, 2 θ values are at 39.7 °, 46.2 °, 67.4 °, 81.4 °, locate to have occurred corresponding Pt (111) respectively, (200) for 85.4 °, (220), (3I1), the characteristic diffraction peak of (222) crystal face, prove this carrier successfully autoreduction go out the Pt nano particle.Fig. 5, Fig. 6 are the TEM figure under the different enlargement ratios of catalyst Pt/C/XC-72, and as can be seen from the figure our prepared catalyst is uniformly dispersed, and particle is tiny.Fig. 7 is that the commercial platinum amount of carrying is that 20% Pt/C catalyst is at O in the various catalyst Pt/C/XC-72 that prepare among the embodiment and the Comparative Examples 2
2Saturated 0.5MH
2SO
4Rotating speed in the solution is the LSV comparison diagram under the 2500rpm, as can be seen from the figure under identical rotating speed, these several catalyst have all shown electrocatalysis characteristic to hydrogen reduction, can draw by the size that compares carrying current, the catalyst of preparation has good catalytic activity to hydrogen reduction among the embodiment 5, the carrying current of this catalyst can reach-70A/g, and can draw in conjunction with TEM figure is that particle is tiny just can to show good catalytic action because this catalyst is uniformly dispersed.
Description of drawings:
Fig. 1 is the sem photograph of the commercial carrier Vulcan XC-72 in the comparative example 1
Fig. 2 is the sem photograph of the complex carrier C/XC-72 among the embodiment 2
Fig. 3 is the XRD figure of prepared sample in the comparative example 1
Fig. 4 is the XRD figure of prepared catalyst among the embodiment 5
Fig. 5 is the transmission electron microscope picture of the low range of the catalyst Pt/C/XC-72 of preparation among the embodiment 5
Fig. 6 is the powerful transmission electron microscope picture of the catalyst Pt/C/XC-72 of preparation among the embodiment 5
Fig. 7 be in the various catalyst Pt/C/XC-72 that prepare among the embodiment and the Comparative Examples 2 the Pt/C catalyst at O
2Saturated 0.5MH
2SO
4Rotating speed in the solution is the LSV comparison diagram under the 2500rpm
The specific embodiment
Further specify the present invention below by embodiment and Comparative Examples.
Embodiment 1
1. configuration concentration is the glucose solution of 50g/l.
2. be the XC-72 (0.1g) of 0.433g/l with adding concentration in glucose (3g) solution of above-mentioned configuration, make that the two mass ratio is 30: 1, change in the reactor, 160 ℃ are reacted 12h down, the water washing of product distill repeatedly are totally promptly made complex carrier C/XC-72 of the present invention.
3. with the 0.2g complex carrier C/XC-72 and the H0.2g of above-mentioned preparation
2PtCl
6(10g/l) pressed mass ratio 1: 1,5mgPVP (0.167g/l) cooks protective agent, and wherein the mass ratio of PVP:C/XC-72 is 1: 4, after stirring, adds hot reflux 4h, obtains catalyst Pt/C/XC-72.
Electrochemical results shows, this Pt/C/XC-72 has shown electrocatalysis characteristic to hydrogen reduction, illustrate that this complex carrier successfully goes out the Pt catalyst with the chloroplatinic acid autoreduction, but catalytic effect is not clearly, this catalyst is to the carrying current value-4.07A/g of hydrogen reduction, this is because the Pt catalyst particle size that generates is bigger, due to some is reunited.
Embodiment 2
1. configuration concentration is the glucose solution of 50g/l.
2. be the XC-72 (0.06g) of 0.433g/l with adding concentration in glucose (3g) solution of above-mentioned configuration, make that the two mass ratio is 50: 1, change in the reactor, 160 ℃ are reacted 12h down, the water washing of product distill repeatedly are totally promptly made complex carrier C/XC-72 of the present invention.
3. with the 0.2g complex carrier C/XC-72 and the 0.2g H of above-mentioned preparation
2PtCl
6(10g/l) pressed mass ratio 1: 1,5mgPVP (0.167g/l) cooks protective agent, and wherein the mass ratio of PVP:C/XC-72 is 1: 4, after stirring, adds hot reflux 4h, obtains catalyst Pt/C/XC-72.
Electrochemical results shows, this Pt/C/XC-72 has shown electrocatalysis characteristic to hydrogen reduction, illustrate that this complex carrier successfully goes out the Pt catalyst with the chloroplatinic acid autoreduction, catalytic effect strengthens, this catalyst reaches-34.31A/g the carrying current value of hydrogen reduction, shows hydrogen reduction catalytic performance preferably.
1. configuration concentration is the glucose solution of 50g/l.
2. be the XC-72 (0.02g) of 0.433g/l with adding concentration in glucose (3g) solution of above-mentioned configuration, make that the two mass ratio is 100: 1, change in the reactor, 160 ℃ are reacted 12h down, the water washing of product distill repeatedly are totally promptly made complex carrier C/XC-72 of the present invention.
3. with the 0.2g complex carrier C/XC-72 and the 0.2g H of above-mentioned preparation
2PtCl
6(10g/l) pressed mass ratio 1: 1,5mgPVP (0.167g/l) cooks protective agent, and wherein the mass ratio of PVP:C/XC-72 is 1: 4, after stirring, adds hot reflux 4h, obtains catalyst Pt/C/XC-72.
Electrochemical results shows, this Pt/C/XC-72 has shown electrocatalysis characteristic to hydrogen reduction, illustrate that this complex carrier successfully goes out the Pt catalyst with the chloroplatinic acid autoreduction, but catalytic effect is general, this catalyst reaches-17.94A/g the carrying current value of hydrogen reduction, shows hydrogen reduction catalytic performance preferably.
Embodiment 4
1. configuration concentration is the glucose solution of 50g/l.
2. be the XC-72 (0.1g) of 0.433g/l with adding concentration in glucose (3g) solution of above-mentioned configuration, make that the two mass ratio is 30: 1, change in the reactor, 160 ℃ are reacted 12h down, the water washing of product distill repeatedly are totally promptly made complex carrier C/XC-72 of the present invention.
3. with the 0.2g complex carrier C/XC-72 and the 0.2g H of above-mentioned preparation
2PtCl
6(10g/l) pressed mass ratio 2: 1,5mgPVP (0.167g/l) cooks protective agent, and wherein the mass ratio of PVP:C/XC-72 is 1: 4, adds hot reflux 4h, obtains catalyst Pt/C/XC-72.
Electrochemical results shows, this Pt/C/XC-72 has shown electrocatalysis characteristic to hydrogen reduction, illustrate that this complex carrier successfully goes out the Pt catalyst with the chloroplatinic acid autoreduction, but catalytic effect is not very remarkable, this catalyst reaches-28.32A/g the carrying current value of hydrogen reduction, shows hydrogen reduction catalytic performance preferably.
Embodiment 5
1. configuration concentration is the glucose solution of 50g/l.
2. be the XC-72 (0.1g) of 0.433g/l with adding concentration in glucose (3g) solution of above-mentioned configuration, make that the two mass ratio is 30: 1, change in the reactor, 160 ℃ are reacted 12h down, the water washing of product distill repeatedly are totally promptly made complex carrier C/XC-72 of the present invention.
3. with the 0.2g complex carrier C/XC-72 and the 0.2g H of above-mentioned preparation
2PtCl
6(10g/l) pressed mass ratio 1: 1,5mgPVP (0.167g/l) cooks protective agent, and wherein the mass ratio of PVP:C/XC-72 is 1: 4, after stirring, adds hot reflux 4h, obtains catalyst Pt/C/XC-72.
Electrochemical results shows, this Pt/C/XC-72 has shown electrocatalysis characteristic to hydrogen reduction, illustrate that this complex carrier successfully goes out the Pt catalyst with the chloroplatinic acid autoreduction, but catalytic effect significantly strengthens, this catalyst reaches-66.45A/g the carrying current value of hydrogen reduction, shows good hydrogen reduction catalytic performance, and this is because the catalyst that generates is uniformly dispersed, particle is tiny, just can show good electrocatalysis characteristic.
Embodiment 6
1. configuration concentration is the glucose solution of 50g/l.
2. be the XC-72 (0.1g) of 0.433g/l with adding concentration in glucose (3g) solution of above-mentioned configuration, make that the two mass ratio is 30: 1, change in the reactor, 160 ℃ are reacted 12h down, the water washing of product distill repeatedly are totally promptly made complex carrier C/XC-72 of the present invention.
3. with the 0.2g complex carrier C/XC-72 and the 0.2g H of above-mentioned preparation
2PtCl
6(10g/l) pressed mass ratio 1: 2,5mgPVP (0.167g/l) cooks protective agent, and wherein the mass ratio of PVP:C/XC-72 is 1: 4, after stirring, adds hot reflux 4h, obtains catalyst Pt/C/XC-72.
Electrochemical results shows, this Pt/C/XC-72 has shown electrocatalysis characteristic to hydrogen reduction, illustrate that this complex carrier successfully goes out the Pt catalyst with the chloroplatinic acid autoreduction, this catalyst reaches-36.81A/g the carrying current value of hydrogen reduction, shows hydrogen reduction catalytic performance preferably.
Comparative Examples 1
With 0.2mg VulcanXC-72 and 0.2g H
2PtCl
6(10g/l) press mass ratio 1: 1, add 5mgPVP and cook protective agent, added hot reflux after mixing 4 hours.
XRD result shows directly with VulcanXC-72 and H
2PtCl
6Mix in proportion, add hot reflux 4h, can not generate the Pt catalyst, illustrate that VulcanXC-72 itself does not have the autoreduction performance, have only to coat one deck carbon film outside and the chloroplatinic acid autoreduction could be become the Pt metal nanoparticle.
Comparative Examples 2
Test platinum load quality is the chemical property of 20% commercial Pt/C (U.S. E-tek company).
Claims (1)
1. one kind is the Pt Preparation of catalysts method of carrier with the carbon carrier, it is characterized in that, comprises following each step:
1) configuration concentration is the glucose solution of 50g/l;
2) be the XC-72 of 0.433g/l～1.677g/l with adding concentration in the above-mentioned glucose solution that makes, make that the two mass ratio is 30～100, change in the reactor, 160 ℃ are reacted 12h down, the water washing of product distill repeatedly are totally promptly got complex carrier C/XC-72;
3) complex carrier C/XC-72 and the concentration with above-mentioned preparation is 10g/l H
2PtCl
6Press mass ratio 0.5～2 and mix, add polyvinylpyrrolidone and cook protective agent, wherein the mass ratio of polyvinylpyrrolidone and C/XC-72 is 1: 4, after stirring, adds hot reflux 4h, obtains catalyst Pt/C/XC-72.
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| CN102903537A (en) * | 2012-10-17 | 2013-01-30 | 东南大学 | Preparation method of multi-walled carbon nanotube loaded high-density high-dispersion nano platinum counter electrode |
| CN103928691A (en) * | 2014-04-10 | 2014-07-16 | 哈尔滨工业大学 | Platinum-based catalyst carrier of direct methanol fuel cell and preparation method thereof |
| CN110931805A (en) * | 2019-11-19 | 2020-03-27 | 一汽解放汽车有限公司 | Platinum alloy catalyst, preparation method thereof and application thereof in fuel cell cathode catalyst |
| CN111408369A (en) * | 2020-04-16 | 2020-07-14 | 桂林理工大学 | Nano gold-platinum bimetallic @ carbon material oxygen reaction catalyst and preparation method thereof |
| CN113097509A (en) * | 2021-03-22 | 2021-07-09 | 中自环保科技股份有限公司 | Hydrogen fuel cell platinum-carbon catalyst and preparation method thereof |
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| CN102903537B (en) * | 2012-10-17 | 2015-04-15 | 东南大学 | Preparation method of multi-walled carbon nanotube loaded high-density high-dispersion nano platinum counter electrode |
| CN103928691A (en) * | 2014-04-10 | 2014-07-16 | 哈尔滨工业大学 | Platinum-based catalyst carrier of direct methanol fuel cell and preparation method thereof |
| CN103928691B (en) * | 2014-04-10 | 2016-07-06 | 哈尔滨工业大学 | DMFC platinum based catalyst carrier and preparation method thereof |
| CN110931805A (en) * | 2019-11-19 | 2020-03-27 | 一汽解放汽车有限公司 | Platinum alloy catalyst, preparation method thereof and application thereof in fuel cell cathode catalyst |
| CN111408369A (en) * | 2020-04-16 | 2020-07-14 | 桂林理工大学 | Nano gold-platinum bimetallic @ carbon material oxygen reaction catalyst and preparation method thereof |
| CN114497587A (en) * | 2020-10-23 | 2022-05-13 | 中国石油化工股份有限公司 | Catalyst in proton exchange membrane fuel cell and preparation method thereof |
| CN114512687A (en) * | 2020-10-23 | 2022-05-17 | 中国石油化工股份有限公司 | Carbon-supported noble metal nano catalyst and preparation method and application thereof |
| CN114512687B (en) * | 2020-10-23 | 2023-11-28 | 中国石油化工股份有限公司 | Carbon-supported noble metal nano catalyst and preparation method and application thereof |
| CN114497587B (en) * | 2020-10-23 | 2024-03-26 | 中国石油化工股份有限公司 | Catalyst in proton exchange membrane fuel cell and preparation method thereof |
| CN113097509A (en) * | 2021-03-22 | 2021-07-09 | 中自环保科技股份有限公司 | Hydrogen fuel cell platinum-carbon catalyst and preparation method thereof |
| CN113097509B (en) * | 2021-03-22 | 2022-03-11 | 中自环保科技股份有限公司 | Hydrogen fuel cell platinum-carbon catalyst and preparation method thereof |
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