CN105789648A - Three-dimensional ordered bimodal mesoporous carbon supported Pt catalyst and preparation method thereof - Google Patents
Three-dimensional ordered bimodal mesoporous carbon supported Pt catalyst and preparation method thereof Download PDFInfo
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- CN105789648A CN105789648A CN201610319242.6A CN201610319242A CN105789648A CN 105789648 A CN105789648 A CN 105789648A CN 201610319242 A CN201610319242 A CN 201610319242A CN 105789648 A CN105789648 A CN 105789648A
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- 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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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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Abstract
The invention relates to a three-dimensional ordered bimodal mesoporous carbon supported Pt catalyst and a preparation method thereof. The catalyst comprises carbon support materials and, by weight, 20 percent-50 percent of supported Pt particles, wherein the carbon support materials have bimodal mesoporous structures, namely containing three-dimensional ordered macro mesoporous structures with pore size of 10-50nm and micro mesoporous structures with pore size of 2-6nm on the wall of the macro mesoporous structures. The three-dimensional ordered bimodal mesoporous carbon supported Pt catalyst has high catalytic activity and poison resistance. Compared with commercialized Pt/C catalysts, the catalytic activity is increased by 5.6 times, and the poison resistance is increased by 1.5 times. In addition, according to the preparation method, the process is simple and the pore size of macro mesoporous can be adjusted.
Description
Technical field
The present invention relates to the preparation method of the double mesoporous carbon-loaded Pt nanoparticle catalyst of a kind of three-dimensional order, belong to Pt catalyst
Technical field.
Background technology
In the world, energy crisis is on the rise, today that ecological environment goes from bad to worse, the most fully development and utilization cleaning new energy,
Realize low-carbon emission reduction, it has also become the topic that the mankind pay close attention to jointly.DMFC (Direct Methanol Fuel Cells,
DMFC), big with its energy density, transformation efficiency is high, the advantage such as pollution-free, becomes the heat of new energy field R and D
Point.Recent decades, the research of DMFC achieves significantly progress, but real commercialization, universalness are the most unrealized.
Realizing one of key technology being converted into electric energy efficient for the chemical energy of methanol fuel, continual is to develop more effectively
Eelctro-catalyst.At present, most widely used catalyst is platinum C catalyst.But in the long-time course of reaction of fuel cell,
Pt nano-particle easily combines CO and is poisoned, it also occur that migrate, reunite, even spin off from carrier, and impact
The activity of catalyst and life-span；In addition Pt metal fancy price is also the restriction business-like key factor of DMFC.Therefore,
How to improve Pt utilization rate, maintain catalyst activity, selectivity and long service life that catalyst is high to be always DMFC simultaneously
The key problem of catalyst preparation.
For improving Pt utilization rate, research worker is devoted to develop novel, and the nanostructured carbon material of high-specific surface area is urged as Pt
The backing material of agent.Wherein meso-porous carbon material receives significant attention due to its higher specific surface area.But, have Xiao Jie
The material with carbon element in hole (2-3nm), although there is higher specific surface area, but actual catalytic reaction medium and small mesoporous be unfavorable for anti-
Answer thing quickly to arrive reactivity position, the most do not utilize the quick diffusion of product.When mesopore size is the biggest, carbon material can be reduced again
The specific surface area of material, affects catalyst dispersion on the carbon material.
Double meso-hole structure material with carbon elements of little mesoporous formation bimodal distribution, phase to a certain extent is added on the basis of big meso-hole structure
Methanol fuel cell can be preferably applied for for the most mesoporous or little meso-porous carbon material.The the most mesoporous of this material with carbon element can be effectively
Reduce resistance to mass tranfer, contribute to the diffusion of reactant and product, molecule can be made to be accessible to active sites, and little mesoporous be provided that
Higher specific surface area and bigger pore volume, thus this pair of meso-hole structure material with carbon element catalyst can be made to have as carrier higher
Catalytic efficiency.
In view of the material with carbon element of double meso-hole structures has huge prospect in terms of catalysis, the present invention provides a kind of new synthetic method,
Utilizing silica nanosphere for hard template, one-step synthesis goes out to have the double meso-porous carbon material of three-dimensional order of high-specific surface area, load
Prepare after Pt nano-particle and there are good stability, catalysis activity and double mesoporous carbon-loaded Pt catalyst of mithridatism.
Summary of the invention
Present invention aims to commercial methanol fuel cell catalyst Pt/C catalyst and there is the shortcomings such as low, the easy poisoning of activity,
Double mesoporous carbon-loaded Pt catalyst materials that a kind of activity performance high, antitoxin is good and preparation method thereof are provided.This material exists simultaneously
Two kinds of meso-hole structures, the little meso-hole structure on the big meso-hole structure of three-dimensional order and big mesoporous wall.Little meso-hole structure can improve
Specific surface area, the dispersibility of enhancing Pt nano-particle, the reunion in the growth of restriction Pt nano-particle and catalytic process, three
Tieing up orderly big meso-hole structure can be with mass transfer enhancement.Silica nanosphere can be used as the most mesoporous pore creating material, again can be in calcining
Hindering the contraction of carbon matrix precursor during carbon matrix precursor (phenolic resin), the microcellular structure making original carbon granules pile up expands into
Little meso-hole structure.
The technical solution used in the present invention is:
The double mesoporous carbon-loaded Pt catalyst of a kind of three-dimensional order, it is characterised in that the composition of this catalyst includes carrier carbon material and bears
The Pt nano-particle carried, the load quality percentage ratio of Pt is 20%-50%；Wherein, described carrier carbon material has double mesoporous
Structure, i.e. containing aperture on the big meso-hole structure of three-dimensional order and big mesoporous wall that aperture is 10-50nm is that 2-6nm is little mesoporous
Structure.
The particle diameter of described Pt nano-particle is less than 2.5nm；It is preferably 1.5～2.3nm.
Described material with carbon element is amorphous carbon.
The preparation method of the double mesoporous carbon-loaded Pt catalyst of described three-dimensional order, comprises the following steps:
(1) silica template of silica nanosphere composition is prepared: monodispersed silica nanosphere colloidal sol is at 45-60 DEG C
Lower standing 2-4 days, obtains the bulk silicon dioxide template of the silica nanosphere array of three-dimensional order；
(2) prepare the double mesoporous carbon of three-dimensional order: the bulk silicon dioxide template that upper step is obtained be immersed in containing 50wt% can
In the ethanol solution of dissolubility phenolic resin；When, after ethanol volatilization completely, calcining 1-3h after template being taken out at 700-1000 DEG C,
Calcined product is soaked in HF solution 24h again, through over cleaning, obtains material with carbon element；
Wherein, the ethanol solution of the resol resin that every 20mL contains 50wt% adds 1-2g silica template；
(3) the double mesoporous carbon-loaded Pt catalyst of three-dimensional order is prepared: be immersed in platinum acid chloride solution by the material with carbon element that upper step prepares；
After ultrasonic disperse 10-15min, at room temperature dry；Then chloroplatinic acid reduction obtains the double mesoporous carbon-loaded Pt of three-dimensional order urge
Agent；
Wherein, mass ratio is material with carbon element: Pt=1-4:1；The concentration of described platinum acid chloride solution is 45～55wt%.
In described monodispersed silica nanosphere colloidal sol, the sphere diameter of nanosphere is 10～50nm；Nanosphere is in colloidal sol
Mass percent is 5～20%.
The concentration of described HF solution is 5wt%.
The invention have the benefit that
Double mesoporous carbon-loaded Pt catalyst prepared by the present invention are carried out electrocatalysis characteristic research, and research shows, three-dimensional order is double
Mesoporous carbon-loaded Pt catalyst shows as higher catalytic activity and good antitoxin performance.Compared with business Pt/C catalyst, urge
Changing increased activity 5.6 times, antitoxin performance enhances 1.5 times.
The preparation method using the present invention utilizes a step list template can complete two kinds of mesoporous preparations, not only technique simple and
And by supporting Pt nano-particle can prepare have high electrocatalytic active carbon carry Pt catalyst.Can be by controlling dioxy
The sphere diameter of SiClx nanosphere, the big mesoporous pore size of the double meso-porous carbon material of regulation three-dimensional order.
Accompanying drawing explanation
The adsorption/desorption isotherms of the double mesoporous carbon of three-dimensional order of Fig. 1 embodiment 1 preparation and graph of pore diameter distribution (illustration)；
The SEM figure of the double mesoporous carbon of three-dimensional order of Fig. 2 embodiment 2 preparation；
The TEM figure of the double mesoporous carbon-loaded Pt catalyst (Pt load capacity is 50wt%) of three-dimensional order of Fig. 3 embodiment 2 preparation；
The double mesoporous carbon-loaded Pt catalyst of three-dimensional order of Fig. 4 embodiment 3 preparation and the XRD figure of business Pt/C catalyst；
The double mesoporous carbon-loaded Pt catalyst of three-dimensional order of Fig. 5 embodiment 3 preparation and business Pt/C catalyst are at 0.5M H2SO4+1
M CH3Cyclic voltammetry curve in OH solution；Sweep speed is 50mv s-1。
Detailed description of the invention
Below in conjunction with example, the method for the present invention is further described.These examples have further described and demonstrated model of the present invention
Enclose interior embodiment.The purpose that the example be given is merely to illustrate, but it is not limited to this, the present invention should not constituted any limit
Fixed, it can be carried out various change without departing from the spirit and scope of the present invention.
It is known material that the present invention sends out the silica nanosphere colloidal sol related to, and its preparation may refer to (Fan, W.et al.
Hierarchical nanofabrication of microporous crystals with ordered mesoporosity.Nature Mater.7,
984-991)。
Embodiment 1
The preparation method of the double mesoporous carbon-loaded Pt catalyst of three-dimensional order, step is as follows:
1) the Stober method improved is used to prepare the silica nanosphere colloidal sol of monodispersed 10nm sphere diameter: to weigh certain successively
The deionized water of quality, ethanol and lysine pour there-necked flask, magnetic agitation 500rpm into, are warming up to 70 DEG C.After Wen Ding,
Weigh and have been heated to the tetraethyl orthosilicate (TEOS) of 70 DEG C and be mixed with.Lysine, ethanol, deionized water and TEOS
Mol ratio be that 1.23:246:9500:61.5x (x=1) 24 hours reaction terminates, obtain the silica nanometer of 10nm sphere diameter
Ball colloidal sol, nanosphere quality is the 7% of colloidal sol quality.
2) by step 1) silica nanosphere prepared stands 3 days at 45 DEG C, and now solution evaporation is complete, obtains from group
Dress up the bulk silicon dioxide template of three-dimensional order silica nanosphere array.
3) 2.0g phenol is melted at 50 DEG C, is subsequently adding the NaOH aqueous solution stirring 10min of 0.425g 20wt.%,
The formalin instilling 3.45g 37wt% continues stirring 10min, is finally to slowly warm up to 75 DEG C of reaction 1h.Reaction knot
Being cooled to room temperature after bundle, regulating the pH value of solution with the HCl solution of 0.1M be～7.0 that decompression distills 1～2h at 45 DEG C
Reduce water content.The product obtained is dissolved in ethanol stir and be centrifuged off the sodium chloride separated out.Finally join to obtain solubility
Phenolic resin (M < 500) ethanol solution, its mass concentration is 50wt.%.
4) by step 1) the silica template 1.5g that obtains is immersed in 20mL step 3) in the mixed solution that obtains, room temperature
Lower volatilization ethanol, takes out sample, obtains the composite of silicon dioxide and carbon matrix precursor.
5) complex of silicon dioxide and carbon matrix precursor is placed in porcelain boat, under nitrogen protection, with the heating rate of 5 DEG C/min
It is warmed up to 900 DEG C, is incubated 2h, obtains the complex of silicon dioxide and material with carbon element.
6) by 5) complex that obtains of step soaks 24h in the HF solution of 5wt% and removes silica template, then use
Ethanol and deionized water are cleaned multiple times product, finally obtain the double meso-porous carbon material of three-dimensional order (now material with carbon element is amorphous carbon,
Following example are same.).
7) by the step 6 of certain mass) the double mesoporous carbon of the three-dimensional order three-dimensional order that obtains immerses in chloroplatinic acid ethanol solution (50
Wt%), wherein, the mass ratio of material with carbon element and Pt is 1:1, then ultrasonic disperse 10-15min, and at room temperature dries.
8) by 7) step is dried after sample 4% hydrogen and 96% nitrogen mixed gas in, reduce at 150 DEG C
Just the double mesoporous carbon-loaded Pt catalyst of three-dimensional order has been obtained after 2h.
Fig. 1 show the adsorption/desorption isothermal curve of the double mesoporous carbon of three-dimensional order that this example prepares, and pore size distribution curve
(PSD) (illustration).The BET specific surface area being calculated the double mesoporous carbon of three-dimensional order from adsorption/desorption isothermal curve is 1320
m2g-1, illustrate that the double mesoporous carbon of three-dimensional order has bigger specific surface area.Can be seen that prepared by this example from PSD figure
Material with carbon element has the meso-hole structure of bimodal distribution, the most mesoporous for silica nanosphere in 10nm, with silica template
Sphere diameter consistent, little mesoporous for 3.6nm on big mesoporous wall.From the foregoing, it will be observed that the material with carbon element that the present embodiment prepares is really double
Mesoporous material.
Embodiment 2
The preparation method of the double mesoporous carbon-loaded Pt catalyst of three-dimensional order, step, with embodiment 1, is a difference in that, step 1) in
Silicon dioxide sphere diameter be 30nm.The silicon dioxide using the Stober method improved to prepare particle diameter monodispersed 30nm sphere diameter is received
Rice ball colloidal sol: weigh the deionized water of certain mass, ethanol and lysine successively and pour there-necked flask into, magnetic agitation 500rpm,
It is warming up to 90 DEG C.After Wen Ding, weigh and have been heated to the TEOS of 90 DEG C and be mixed with.Lysine, ethanol, deionized water and
The mol ratio of TEOS is 1.23:246:9500:61.5x (x=1), continuously adds TEOS and reacts 24h again, obtain after 24h
The silica nanosphere of 30nm.The mol ratio of final lysine, ethanol, deionized water and TEOS is 1.23:246:9500:
61.5x (x=4).
Fig. 2 show the SEM picture of the double mesoporous carbon of three-dimensional order that this example prepares, and as can be seen from the figure sample has very well
Meso-hole structure, and present large-area three-dimensional ordered arrangement.The big mesoporous pore size of sample is 30nm, pore size and silicon dioxide
In template, the sphere diameter (30nm) of silica nanosphere is consistent.Fig. 3 is that the double mesoporous carbon of three-dimensional order that the present embodiment prepares is born
Carry the TEM picture of Pt catalyst, as can be seen from the figure material with carbon element the most mesoporous the most high-visible after supporting Pt nano-particle,
This is conducive to catalyst reactant and quick diffusion of product in catalytic process.
Embodiment 3
The preparation method of the double mesoporous carbon-loaded Pt catalyst of three-dimensional order, step, with embodiment 1, is a difference in that, step 1) in
Silicon dioxide sphere diameter be 50nm.The silicon dioxide using the Stober method improved to prepare particle diameter monodispersed 50nm sphere diameter is received
Rice ball colloidal sol: weigh the deionized water of certain mass, ethanol and lysine successively and pour there-necked flask into, magnetic agitation 500rpm,
It is warming up to 90 DEG C.After Wen Ding, weigh and have been heated to the TEOS of 90 DEG C and be mixed with.Lysine, ethanol, deionized water and
The mol ratio of TEOS is 1.23:246:9500:61.5x (x=1), continuously adds TEOS and reacts 24h again, obtain after 24h
The silica nanosphere of 50nm.The mol ratio of final lysine, ethanol, deionized water and TEOS is 1.23:246:9500:
61.5x (x=8).
Fig. 4 is that the X of the double mesoporous carbon-loaded Pt catalyst (Pt load capacity is 50wt%) of three-dimensional order that the present embodiment prepares penetrates
Ray diffraction diagram spectrum (XRD) and business Pt/C catalyst (JM company, model is: HiSPEC 8000).Pt from figure
(220) half-peak breadth in face can calculate the Pt grain a size of 2.0nm of the double mesoporous carbon-loaded Pt catalyst of three-dimensional order,
Less than the crystallite dimension (2.9nm) of business Pt/C catalyst, little crystal grain be formed as the mesoporous growth limiting Pt granule.
Fig. 5 be the catalyst prepared of the present embodiment with business Pt/C catalyst at 0.5M H2SO4+1M CH3Circulation in OH solution
Volt-ampere curve；Sweep speed is 50mv s-1.As can be seen from Figure 5 the peak current density at 0.86V is 624mAmg-1,
It is peak current density (the 111mA mg of business Pt/C catalyst-1) 5.6 times, the double mesoporous carbon of the three-dimensional order prepared by explanation
Loaded Pt catalyst has relatively high methanol catalytic oxidation activity.Further, the peak current density I of forward potential scanningfWith negative sense current potential
The peak current density I of scanningbRatio be 1.37, (this numerical value represent in methanol oxidation process produce intermediate product CO by oxygen
The degree changed, i.e. the performance of numerical value the highest explanation CO tolerance catalysts is the best) show prepared catalyst and business Pt/C catalyst
(If/Ib=0.89) ratio, has higher antitoxin performance.
Embodiment 4
The preparation method of the double mesoporous carbon-loaded Pt catalyst of three-dimensional order, step, with embodiment 1, is a difference in that, step 5) in
Holding temperature is 700 DEG C.
Embodiment 5
The preparation method of the double mesoporous carbon-loaded Pt catalyst of three-dimensional order, step, with embodiment 1, is a difference in that, step 5) in
Holding temperature is 800 DEG C.
Embodiment 6
The preparation method of the double mesoporous carbon-loaded Pt catalyst of three-dimensional order, step, with embodiment 1, is a difference in that, step 7) in
Material with carbon element and Pt mass ratio are 2:1.
Embodiment 7
The preparation method of the double mesoporous carbon-loaded Pt catalyst of three-dimensional order, step, with embodiment 1, is a difference in that, step 7) in
Material with carbon element and Pt mass ratio are 3:1.
Embodiment 8
The preparation method of the double mesoporous carbon-loaded Pt catalyst of three-dimensional order, step, with embodiment 1, is a difference in that, step 7) in
Material with carbon element and Pt mass ratio are 4:1.
Unaccomplished matter of the present invention is known technology.
Claims (7)
1. the double mesoporous carbon-loaded Pt catalyst of three-dimensional order, it is characterised in that the composition of this catalyst includes the Pt nano-particle of carrier carbon material and load, and the load quality percentage ratio of Pt is 20%-50%；Wherein, described carrier carbon material has double meso-hole structure, and i.e. containing aperture on the big meso-hole structure of three-dimensional order and big mesoporous wall that aperture is 10-50 nm is the little meso-hole structure of 2-6 nm.
2. the double mesoporous carbon-loaded Pt catalyst of three-dimensional order as claimed in claim 1, it is characterised in that the particle diameter of described Pt nano-particle is less than 2.5 nm.
3. the double mesoporous carbon-loaded Pt catalyst of three-dimensional order as claimed in claim 1, it is characterised in that the particle diameter of described Pt nano-particle is preferably 1.5 ~ 2.3nm.
4. the double mesoporous carbon-loaded Pt catalyst of three-dimensional order as claimed in claim 1, it is characterised in that described material with carbon element is amorphous carbon.
5. the preparation method of the double mesoporous carbon-loaded Pt catalyst of three-dimensional order as claimed in claim 1, is characterized by comprise the following steps:
(1) silica template of silica nanosphere composition is prepared: monodispersed silica nanosphere colloidal sol stands 2-4 days at 45-60 DEG C, obtains the bulk silicon dioxide template of the silica nanosphere array of three-dimensional order；
(2) the double mesoporous carbon of three-dimensional order is prepared: the bulk silicon dioxide template upper step obtained is immersed in containing 50 wt
In the ethanol solution of the resol resin of %；When, after ethanol volatilization completely, calcining 1-3 h after template being taken out at 700-1000 DEG C, then calcined product is soaked in HF solution 24 h, through over cleaning, obtain material with carbon element；
Wherein, the ethanol solution of the resol resin that every 20 mL contain 50 wt % adds 1-2 g silica template；
(3) the double mesoporous carbon-loaded Pt catalyst of three-dimensional order is prepared: be immersed in platinum acid chloride solution by the material with carbon element that upper step prepares；After ultrasonic disperse 10-15 min, at room temperature dry；Then chloroplatinic acid reduction is obtained the double mesoporous carbon-loaded Pt catalyst of three-dimensional order；
Wherein, mass ratio is material with carbon element: Pt=1-4:
1；The concentration of described platinum acid chloride solution is 45 ~ 55
wt % 。
6. the preparation method of the double mesoporous carbon-loaded Pt catalyst of three-dimensional order as claimed in claim 5, is characterized by that in described monodispersed silica nanosphere colloidal sol, the sphere diameter of nanosphere is 10 ~ 50nm；Nanosphere mass percent in colloidal sol is 5 ~ 20%.
7. the preparation method of the double mesoporous carbon-loaded Pt catalyst of three-dimensional order as claimed in claim 5, is characterized by that the concentration of described HF solution is 5 wt %.
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Cited By (5)
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| CN107069049A (en) * | 2017-04-10 | 2017-08-18 | 河北工业大学 | A kind of mesoporous polypyrrole nano-rings loaded Pt catalyst and preparation method thereof |
| CN110665496A (en) * | 2019-10-10 | 2020-01-10 | 四川大学 | Preparation method of ordered mesoporous carbon-supported platinum-based catalyst with controllable pore length |
| CN111342062A (en) * | 2019-10-23 | 2020-06-26 | 广东道氏云杉氢能科技有限公司 | Supported fuel cell catalyst and application thereof |
| CN113908836A (en) * | 2021-09-30 | 2022-01-11 | 广州市佳境水处理技术工程有限公司 | Neutral advanced oxidation catalyst and preparation method thereof |
| CN115020724A (en) * | 2021-03-04 | 2022-09-06 | 丰田自动车株式会社 | Electrode catalyst |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107069049A (en) * | 2017-04-10 | 2017-08-18 | 河北工业大学 | A kind of mesoporous polypyrrole nano-rings loaded Pt catalyst and preparation method thereof |
| CN107069049B (en) * | 2017-04-10 | 2019-07-02 | 河北工业大学 | A kind of mesoporous polypyrrole nano-rings loaded Pt catalyst and preparation method thereof |
| CN110665496A (en) * | 2019-10-10 | 2020-01-10 | 四川大学 | Preparation method of ordered mesoporous carbon-supported platinum-based catalyst with controllable pore length |
| CN111342062A (en) * | 2019-10-23 | 2020-06-26 | 广东道氏云杉氢能科技有限公司 | Supported fuel cell catalyst and application thereof |
| CN115020724A (en) * | 2021-03-04 | 2022-09-06 | 丰田自动车株式会社 | Electrode catalyst |
| CN113908836A (en) * | 2021-09-30 | 2022-01-11 | 广州市佳境水处理技术工程有限公司 | Neutral advanced oxidation catalyst and preparation method thereof |
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