CN107069055A - The preparation method of the fuel-cell catalyst of tin oxide composite diatomite load - Google Patents
The preparation method of the fuel-cell catalyst of tin oxide composite diatomite load Download PDFInfo
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- CN107069055A CN107069055A CN201710459411.0A CN201710459411A CN107069055A CN 107069055 A CN107069055 A CN 107069055A CN 201710459411 A CN201710459411 A CN 201710459411A CN 107069055 A CN107069055 A CN 107069055A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/925—Metals of platinum group supported on carriers, e.g. powder carriers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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Abstract
The invention discloses a kind of preparation method of the fuel-cell catalyst of tin oxide composite diatomite load, belong to fuel cell catalyst technical field of material, it is with SnCl3·5H2O, diatomite, chlorine palladium acid and reducing agent be primary raw material, first by after diatomite modified with SnCl3·5H2O together fully dispersed, stirrings soluble in water, again tin oxide composite diatomite carrier is obtained through drying, calcining, then gained complex carrier is added and is sufficiently stirred in chlorine palladium acid solution, by liquid phase reduction in supported palladium nano-catalyst particles thereon, so that the fuel-cell catalyst is made.The present invention is loaded using tin oxide composite diatomite carrier, the dispersiveness of palladium particle can be significantly improved, so as to improve catalytic activity and stability of the catalyst to alcohols.Raw material of the present invention is simple and easy to get, stable preparation process, with industrialization prospect.
Description
Technical field
The invention belongs to fuel cell catalyst technical field of material, and in particular to a kind of tin oxide-composite diatomite
Load the preparation method of fuel-cell catalyst.
Background technology
Catalyst is one of critical material of fuel cell, and the cost of catalyst accounts for the 1/3 of fuel cell cost, because
This, the research of larger catalyst, the commercialization for this following clean energy resource of fuel cell has very important significance.Platinum
It is proved to be the optimum catalyst active component for low-temperature fuel cell, but uses platinum to exist such as fuel-cell catalyst
Lower serious problems：（1）Platinum scarcity of resources；（2）It is expensive；（3）Poison resistance is poor.Therefore, seek cheap and have good steady
The catalyst of qualitative energy has turned into the main target that electrode catalyst is studied.In order to reduce the cost of fuel cell, it is necessary to reduce
Platinum carrying capacity, that is, develop low platinum or even non-platinum elctro-catalyst.It is main to use palladium base or ruthenium base at present for the research of non-platinum catalyst
Other metals are adulterated to prepare catalyst.In recent years, researcher is prepared for various active components with a variety of methods and highly divided
Scattered Pd catalyst.Pd catalyst is cheaper than Pt, and resource reserve enriches, but it still haves the shortcomings that serious, such as Pd conducts
During catalyst, because the intermediate product CO that fuel incomplete oxidation is produced easily makes catalyst poisoning during electro-catalysis, from
And reduce catalytic activity.
Transition metal oxide has stronger chemical stability and electrochemical stability, organic small in formic acid, methanol etc.
Among the oxidizing process of molecule, the resistance to overturning of catalyst material can be lifted, the loss of electrochemical surface area is reduced.Receive
Rice tin oxide has excellent catalytic activity, good heat endurance and chemical stability and electronics, Lacking oxygen transmission capacity,
And there is complicated interaction between noble metal, this interaction has important shadow to the catalytic performance of composite catalyst
Ring.
A kind of new material that natural diatomaceous earth belongs in silicon materials, it has the big advantage of widely distributed, natural reserves, and
The silicone hydroxyl on its surface is evenly distributed, surface it is mesoporous more regular.And the side for passing through chemical load on natural diatomaceous earth surface
Method supported palladium, can make the palladium catalyst after load more firm, and particle diameter distribution is more uniform, suitable, size mainly in nanoscale,
And its load capacity is easier to regulation and control so that the catalytic efficiency of this new heterogeneous catalysis is obtained with recycling ability
Larger raising and guarantee.
The content of the invention
In order to overcome the problem of easy CO poisonings of traditional catalyst and activity reduction, the invention provides a kind of tin oxide-silicon
The preparation method of the fuel-cell catalyst of diatomaceous earth composite load, its by the synergy of tin oxide-composite diatomite carrier,
Dispersiveness and particle diameter of the palladium nano-catalyst particles in carrier surface are significantly improved, and then improves its catalytic performance.
To achieve the above object, the present invention is adopted the following technical scheme that：
A kind of preparation method of the fuel-cell catalyst of tin oxide-composite diatomite load, it comprises the following steps：
1）Diatomite and surfactant are dissolved in ethanol, after ultrasonically treated 1 hour makes its dispersed, through centrifugation, dried
Obtain modification infusorial earth；
2）By SnCl3·5H2O and step 1）The modification infusorial earth of acquisition is soluble in water, makes its abundant within ultrasonically treated 0.5 ~ 5 hour
It is scattered, with after magnetic agitation 0.5 ~ 8 hour under room temperature or 90 DEG C of oil baths, then through centrifuge washing, drying, obtain solid powder；
3）By step 2）Obtained solid powder is positioned in tube furnace, and 300 ~ 500 DEG C, guarantor are warming up in protective gas atmosphere
Temperature 0.5 ~ 8 hour, obtains tin oxide-composite diatomite carrier；
4）By step 3）Gained tin oxide-composite diatomite carrier is added to ultrasonic agitation 0.5 ~ 6 hour in chlorine palladium acid solution；
5）Reductant solution is slowly added dropwise step 4）In gained mixed solution, room temperature magnetic agitation is after 1 ~ 10 hour, then
Through centrifuge washing, drying, the palladium base fuel-cell catalyst of tin oxide-composite diatomite load is obtained.
Step 1）The mol ratio of middle diatomite and surfactant is 1:1~10:1；The surfactant is CTAB（Ten
Six alkyl trimethyl ammonium bromides）、CTAC（Hexadecyltrimethylammonium chloride）、P123（PEO-PPOX-poly-
Oxirane triblock copolymer）、F127（Polyoxyethylene poly-oxygen propylene aether block copolymer）In one or more.
Step 2）Middle SnCl3·5H2The mass ratio of O and modification infusorial earth is 1:5~5:1.
Step 3）Described in protective gas be nitrogen, argon gas, hydrogen in one or more.
Step 4）The consumption of middle tin oxide-composite diatomite carrier and chlorine palladium acid is by the mol ratio of tin element and palladium element
1:3~3:1 is converted；The concentration of the chlorine palladium acid solution is 10 ~ 50 mmol/L.
Step 5）The volume ratio of middle reductant solution and mixed solution is 1:1；The reductant solution is NaBH4It is water-soluble
Liquid, its concentration is 0.1 ~ 0.5 mol/L.
The solvent of centrifuge washing described in step is absolute ethyl alcohol or water.
The remarkable advantage of the present invention is：
The present invention prepares complex carrier with tin oxide and diatomite material, and palladium nano-catalyst particles are entered with reference to liquid phase reduction
Row load, can obtain the palladium nano-particles of size uniform, and can significantly improve dispersiveness of the palladium nano-particles on carrier, so that
There is higher catalytic activity to Aalcohols fuels such as ethanol, methanol.Raw material of the present invention is simple and easy to get, and stable preparation process has
Industrialization prospect.
Brief description of the drawings
The TEM patterns of the palladium base fuel-cell catalyst of the tin oxide that Fig. 1 is prepared for the present invention-composite diatomite load
Figure.
Fig. 2 loads for single modification infusorial earth（There is no tin oxide in carrier）Palladium-based catalyst TEM patterns.
Embodiment
The present invention provides a kind of preparation method of the fuel-cell catalyst of tin oxide-composite diatomite load, to make this
The purpose of invention, technical scheme and effect are clearer, clear and definite, and with reference to specific embodiment, the present invention is expanded on further.Should
Understand, these embodiments are only illustrative of the invention and is not intended to limit the scope of the invention.In addition, it is to be understood that reading this
Invent after the content lectured, those skilled in the art can make various changes or modifications to the present invention, and these equivalent form of values are same
Sample falls within the application appended claims limited range.
Embodiment 1：
1）By diatomite and surfactant CTAC in molar ratio 3:1 is dissolved in ethanol, makes its dispersed within ultrasonically treated 1 hour
Afterwards, through centrifuging, being dried to obtain modification infusorial earth；
2）By SnCl3·5H2O and step 1）The modification infusorial earth of acquisition in mass ratio 5:1 is soluble in water, ultrasonically treated 1 hour
Make its fully dispersed, then magnetic agitation 6 hours at room temperature, then through washing centrifuge washing, drying, obtain solid powder；
3）By step 2）Obtained solid powder is positioned in tube furnace, and 350 DEG C are warming up in argon gas atmosphere, is incubated 6 hours,
Obtain tin oxide-composite diatomite carrier；
4）Mol ratio according to tin element and palladium element is 3:1, by step 3）Gained tin oxide-composite diatomite carrier is added to
In 20 mmol/L chlorine palladium acid solution, ultrasonic agitation 2 hours；
5）By reducing agent NaBH4It is dissolved in the NaBH for obtaining that concentration is 0.2 mol/L after water4Solution, by volume 1:1 is slow by its
Step 4 is added dropwise）In gained mixed solution, magnetic agitation 2 hours at room temperature, then through washing centrifugal drying, obtain tin oxide-
The palladium base fuel-cell catalyst of composite diatomite load.
Embodiment 2：
1）By diatomite and surfactant P123 in molar ratio 5:1 is dissolved in ethanol, makes its dispersed within ultrasonically treated 1 hour
Afterwards, through centrifuging, being dried to obtain modification infusorial earth；
2）By SnCl3·5H2O and step 1）The modification infusorial earth of acquisition in mass ratio 2:3 is soluble in water, ultrasonically treated 3 hours
Make its fully dispersed, then magnetic agitation 4 hours at room temperature, then through ethanol centrifuge washing, drying, obtain solid powder；
3）By step 2）Obtained solid powder is positioned in tube furnace, and 400 DEG C are warming up in argon gas atmosphere, is incubated 6 hours,
Obtain tin oxide-composite diatomite carrier；
4）Mol ratio according to tin element and palladium element is 1:1, by step 3）Gained tin oxide-composite diatomite carrier is added to
In 30 mmol/L chlorine palladium acid solution, ultrasonic agitation 3 hours；
5）By reducing agent NaBH4It is dissolved in the NaBH for obtaining that concentration is 0.3 mol/L after water4Solution, by volume 1:1 is slow by its
Step 4 is added dropwise）In gained mixed solution, magnetic agitation 4 hours, then clean centrifugal drying through ethanol at room temperature obtain oxygen
Change the palladium base fuel-cell catalyst of tin-composite diatomite load.
Embodiment 3：
1）By diatomite and surfactant F127 in molar ratio 7:1 is dissolved in ethanol, makes its dispersed within ultrasonically treated 1 hour
Afterwards, through centrifuging, being dried to obtain modification infusorial earth；
2）By SnCl3·5H2O and step 1）The modification infusorial earth of acquisition in mass ratio 3:2 is soluble in water, ultrasonically treated 4 hours
Make its fully dispersed, then magnetic agitation 2 hours at room temperature, then through ethanol centrifuge washing, drying, obtain solid powder；
3）By step 2）Obtained solid powder is positioned in tube furnace, and 450 DEG C are warming up in argon gas atmosphere, is incubated 2 hours,
Obtain tin oxide-composite diatomite carrier；
4）Mol ratio according to tin element and palladium element is 1:1, by step 3）Gained tin oxide-composite diatomite carrier is added to
In 40 mmol/L chlorine palladium acid solution, ultrasonic agitation 4 hours；
5）By reducing agent NaBH4It is dissolved in the NaBH for obtaining that concentration is 0.4 mol/L after water4Solution, by volume 1:1 is slow by its
Step 4 is added dropwise）In gained mixed solution, magnetic agitation 8 hours, then clean centrifugal drying through ethanol at room temperature obtain oxygen
Change the palladium base fuel-cell catalyst of tin-composite diatomite load.
Embodiment 4：
1）By diatomite and Surfactant CTAB in molar ratio 10:1 is dissolved in ethanol, it is uniformly divided within ultrasonically treated 1 hour
After dissipating, through centrifuging, being dried to obtain modification infusorial earth；
2）By SnCl3·5H2O and step 1）The modification infusorial earth of acquisition in mass ratio 4:1 is soluble in water, ultrasonically treated 5 hours
Make its fully dispersed, then magnetic agitation 0.5 hour at room temperature, then through washing centrifuge washing, drying, obtain solid powder；
3）By step 2）Obtained solid powder is positioned in tube furnace, 500 DEG C is warming up in hydrogen atmosphere, insulation 0.5 is small
When, obtain tin oxide-composite diatomite carrier；
4）Mol ratio according to tin element and palladium element is 1:1, by step 3）Gained tin oxide-composite diatomite carrier is added to
In 50 mmol/L chlorine palladium acid solution, ultrasonic agitation 6 hours；
5）By reducing agent NaBH4It is dissolved in the NaBH for obtaining that concentration is 0.5 mol/L after water4Solution, by volume 1:1 is slow by its
Step 4 is added dropwise）In gained mixed solution, magnetic agitation 10 hours, then clean centrifugal drying through ethanol at room temperature obtain oxygen
Change the palladium base fuel-cell catalyst of tin-composite diatomite load.
Embodiment 5：
1）By diatomite and Surfactant CTAB in molar ratio 1:1 is dissolved in ethanol, makes its dispersed within ultrasonically treated 1 hour
Afterwards, through centrifuging, being dried to obtain modification infusorial earth；
2）By SnCl3·5H2O and step 1）The modification infusorial earth of acquisition in mass ratio 1:5 is soluble in water, and ultrasonically treated 0.5 is small
When make its fully dispersed, then magnetic agitation 8 hours at room temperature, then through washing centrifuge washing, drying, obtain solid powder；
3）By step 2）Obtained solid powder is positioned in tube furnace, and 300 DEG C are warming up in nitrogen atmosphere, is incubated 8 hours,
Obtain tin oxide-composite diatomite carrier；
4）Mol ratio according to tin element and palladium element is 1:3, by step 3）Gained tin oxide-composite diatomite carrier is added to
In 10 mmol/L chlorine palladium acid solution, ultrasonic agitation 0.5 hour；
5）By reducing agent NaBH4It is dissolved in the NaBH for obtaining that concentration is 0.1 mol/L after water4Solution, then by volume 1:1 by its
It is slowly added dropwise step 4）In gained mixed solution, room temperature magnetic agitation is obtained after 1 hour, then through washing centrifuge washing, drying
To the palladium base fuel-cell catalyst of tin oxide-composite diatomite load.
Fig. 1 is the TEM shape appearance figures of the palladium-based catalyst of tin oxide manufactured in the present embodiment-composite diatomite load.By Fig. 1
It can be seen that, using catalyst of the tin oxide-modification infusorial earth as complex carrier, palladium particle is well dispersed, does not almost reunite existing
As, while the granularity of palladium is smaller, the nm of average grain diameter about 3.2.
Fig. 2 loads for the single modification infusorial earth prepared under the present embodiment condition of similarity（There is no tin oxide in carrier）'s
The TEM shape appearance figures of palladium-based catalyst.From Figure 2 it can be seen that using catalyst of the single modification infusorial earth as carrier, palladium particle has portion
Divide and reunite, and its average grain diameter is about 5.6 nm.
From Fig. 1,2 contrasts as can be seen that compared to catalyst of the single modification infusorial earth as carrier, by tin oxide and
The compound action of modification infusorial earth, can further improve the dispersiveness and particle diameter of palladium base fuel-cell catalyst, this is conducive to
Improve the catalytic activity of catalyst.
Using ethanol as raw material, the palladium-based catalyst of the tin oxide-composite diatomite load prepared respectively to embodiment 1-5 with
The palladium-based catalyst of single modification infusorial earth load carries out catalytic performance experiment, and it the results are shown in Table 1.
The performance test results of table 1
From the result of table 1, the palladium-based catalyst loaded compared to single modification infusorial earth, using tin oxide-composite diatomite
The palladium-based catalyst of load has higher catalytic activity and stability.
The foregoing is only presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, should all belong to the covering scope of the present invention.
Claims (8)
1. a kind of preparation method of the fuel-cell catalyst of tin oxide-composite diatomite load, it is characterised in that：Including following
Step：
1）Diatomite and surfactant are dissolved in ethanol, after ultrasonically treated 1 hour makes its dispersed, through centrifugation, dried
Obtain modification infusorial earth；
2）By SnCl3·5H2O and step 1）The modification infusorial earth of acquisition is soluble in water, makes its abundant within ultrasonically treated 0.5 ~ 5 hour
It is scattered, subsequent magnetic agitation 0.5 ~ 8 hour, then through centrifuge washing, drying, obtain solid powder；
3）By step 2）Obtained solid powder is positioned in tube furnace, and 300 ~ 500 DEG C, guarantor are warming up in protective gas atmosphere
Temperature 0.5 ~ 8 hour, obtains tin oxide-composite diatomite carrier；
4）By step 3）Gained tin oxide-composite diatomite carrier is added to ultrasonic agitation 0.5 ~ 6 hour in chlorine palladium acid solution；
5）Reductant solution is slowly added dropwise step 4）In gained mixed solution, room temperature magnetic agitation is after 1 ~ 10 hour, then
Through centrifuge washing, drying, the palladium base fuel-cell catalyst of tin oxide-composite diatomite load is obtained.
2. the preparation method of the fuel-cell catalyst of tin oxide according to claim 1-composite diatomite load, it is special
Levy and be：Step 1）The mol ratio of middle diatomite and surfactant is 1:1~10:1；
Wherein described surfactant is the one or more in CTAB, CTAC, P123, F127.
3. the preparation method of the fuel-cell catalyst of tin oxide according to claim 1-composite diatomite load, it is special
Levy and be：Step 2）Middle SnCl3·5H2The mass ratio of O and modification infusorial earth is 1:5~5:1.
4. the preparation method of the fuel-cell catalyst of tin oxide according to claim 1-composite diatomite load, it is special
Levy and be：Step 2）Described in magnetic agitation be under room temperature or 90 DEG C of oil baths carry out.
5. the preparation method of the fuel-cell catalyst of tin oxide according to claim 1-composite diatomite load, it is special
Levy and be：Step 3）Described in protective gas be nitrogen, argon gas, hydrogen in one or more.
6. the preparation method of the fuel-cell catalyst of tin oxide according to claim 1-composite diatomite load, it is special
Levy and be：Step 4）The consumption of middle tin oxide-composite diatomite carrier and chlorine palladium acid is by the mol ratio of tin element and palladium element
1:3~3:1 is converted；
The concentration of the chlorine palladium acid solution is 10 ~ 50 mmol/L.
7. the preparation method of the fuel-cell catalyst of tin oxide according to claim 1-composite diatomite load, it is special
Levy and be：Step 5）The volume ratio of middle reductant solution and mixed solution is 1:1；
The reductant solution is NaBH4The aqueous solution, its concentration be 0.1 ~ 0.5 mol/L.
8. the preparation method of the fuel-cell catalyst of tin oxide according to claim 1-composite diatomite load, it is special
Levy and be：The solvent of centrifuge washing described in step is absolute ethyl alcohol or water.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101711980A (en) * | 2009-11-30 | 2010-05-26 | 赵杰 | Novel attapulgite supported palladium hydrogenation catalyst and preparation method thereof |
| CN101944620A (en) * | 2010-08-02 | 2011-01-12 | 北京交通大学 | Fuel cell catalyst taking multi-element compound as carrier and preparation method thereof |
| CN102306810A (en) * | 2011-07-21 | 2012-01-04 | 华南理工大学 | Composite catalyst of self-humidifying fuel cell and manufacturing method and application thereof |
-
2017
- 2017-06-16 CN CN201710459411.0A patent/CN107069055A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101711980A (en) * | 2009-11-30 | 2010-05-26 | 赵杰 | Novel attapulgite supported palladium hydrogenation catalyst and preparation method thereof |
| CN101944620A (en) * | 2010-08-02 | 2011-01-12 | 北京交通大学 | Fuel cell catalyst taking multi-element compound as carrier and preparation method thereof |
| CN102306810A (en) * | 2011-07-21 | 2012-01-04 | 华南理工大学 | Composite catalyst of self-humidifying fuel cell and manufacturing method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 朱清玮: ""硅藻土、海泡石负载氧化亚铜光催化剂及TNT非水处理"", 《中国博士学位论文全文数据库》 * |
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Application publication date: 20170818 |