CN101773839A - PtRuCo/C ternary alloy nano catalyst and preparation method thereof - Google Patents
PtRuCo/C ternary alloy nano catalyst and preparation method thereof Download PDFInfo
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- CN101773839A CN101773839A CN201010100345A CN201010100345A CN101773839A CN 101773839 A CN101773839 A CN 101773839A CN 201010100345 A CN201010100345 A CN 201010100345A CN 201010100345 A CN201010100345 A CN 201010100345A CN 101773839 A CN101773839 A CN 101773839A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 229910002058 ternary alloy Inorganic materials 0.000 title claims abstract description 19
- 239000011943 nanocatalyst Substances 0.000 title claims abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 12
- 239000002002 slurry Substances 0.000 claims abstract description 10
- 239000001509 sodium citrate Substances 0.000 claims abstract description 10
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims abstract description 10
- 229940038773 trisodium citrate Drugs 0.000 claims abstract description 10
- 238000013019 agitation Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 4
- 239000002184 metal Substances 0.000 claims abstract description 4
- 229910052751 metal Inorganic materials 0.000 claims abstract description 4
- 238000001291 vacuum drying Methods 0.000 claims abstract description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 6
- 229910052707 ruthenium Inorganic materials 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 241000370738 Chlorion Species 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000003828 vacuum filtration Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract description 39
- 239000000446 fuel Substances 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 3
- 239000003223 protective agent Substances 0.000 abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract 1
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 abstract 1
- 229910002621 H2PtCl6 Inorganic materials 0.000 abstract 1
- 229910019891 RuCl3 Inorganic materials 0.000 abstract 1
- 230000001276 controlling effect Effects 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 abstract 1
- 239000012279 sodium borohydride Substances 0.000 abstract 1
- 229910000033 sodium borohydride Inorganic materials 0.000 abstract 1
- 238000002604 ultrasonography Methods 0.000 abstract 1
- 229910002849 PtRu Inorganic materials 0.000 description 7
- 239000000243 solution Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 231100000572 poisoning Toxicity 0.000 description 3
- 230000000607 poisoning effect Effects 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 2
- 239000013067 intermediate product Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000035772 mutation Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000004832 voltammetry Methods 0.000 description 1
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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 PtRuCo/C ternary alloy nano catalyst and a preparation method thereof, and the method comprises the following steps: dissolving activated carbon in water, boosting the temperature to 40 DEG C, stirring by magnetic force, controlling the stirring velocity at 500r/min to form carbon slurry, dropwise adding H2PtCl6, RuCl3 and CoCl2 solution successively and slowly, adding trisodium citrate as a metal protective agent, carrying out ultrasound agitation, regulating the pH value of the solution to be 8 by NaOH, dropwise adding NaBH4 as a reducing agent slowly, reacting for 3h, vacuum filtering, rinsing until no chloride ion exists in the solution, and vacuum drying for 12h at the temperature of 70 DEG C to obtain the PtRuCo/C ternary alloy nano catalyst in the invention. The PtRuCo/C ternary alloy nano catalyst in the invention can greatly improve the ability of catalyzing methanol in fuel cells.
Description
Technical field
The present invention relates to a kind of PtRuCo/C ternary alloy nano catalyst and preparation method thereof, belong to the material field.
Background technology
Because the energy conversion efficiency height, pollute for a short time, help reducing the environment that excessively uses and preserve our planet of fossil fuel, fuel cell now has been subjected to various countries researcher's common concern.DMFC is a kind of mutation of hydrogen Proton Exchange Membrane Fuel Cells, methyl alcohol is equivalent to store hydrogen carrier, methyl alcohol is the simplest liquid organic compound of a kind of structure at normal temperatures and pressures, store simply convenient sources, low price, it is a kind of desirable recyclable fuel, and in methanol molecules, not having the constraint of C-C key, the electro-chemical activity height can keep higher energy conversion efficiency.
Pt has very high catalytic activity to methanol oxidation, but oxidization of methanol intermediate product (similar CO) is easy to occupy the active sites on Pt surface, and Pt is poisoned.And the key that improves catalyst activity is the intermediate product of the similar CO of oxidation under electronegative potential, thereby discharges the active sites of Pt.Present Pt
50Ru
50It is the effective bianry alloy of commercialization of generally acknowledging.Adding that it is generally acknowledged Ru has the effect of two aspects: the affiliation that adds of (1) Ru influences the d electronic state of Pt, thereby has weakened the interaction between Pt and the CO; (2) Ru is than easily forming active oxygenated species under the electronegative potential, and it can promote methyl alcohol to dissociate the intermediate of absorption at its surface oxidation, thereby has improved anti-CO poisoning capability.Though the PtRu/C bianry alloy can improve anti-CO poisoning capability, according to the Norskov theory,, can greatly improve ability of catalyzing methanol if can synthesize the PtRuCo/C ternary alloy three-partalloy, the present invention is with head it off.
Summary of the invention
In order to strengthen the catalytic activity of anti-CO poisoning capability of catalyst and raising catalysis methanol, the present invention proposes a kind of PtRuCo/C ternary alloy nano catalyst and preparation method thereof.
Technical scheme of the present invention
A kind of preparation method of PtRuCo/C ternary alloy nano catalyst comprises being prepared as follows step:
(1), the preparation of carbon slurry
Is active carbon to be dissolved in the water in 3: 2 active carbon by the mass ratio of itself and water, is warming up to 40 ℃, magnetic agitation, and control stir speed (S.S.) 500r/min forms the carbon slurry behind the 30min;
(2), the preparation of the hydrosol
In the carbon slurry of step (1) gained, slowly drip H successively
2PtCl
6, RuCl
3, CoCl
2The mole that promptly adds Pt, Ru, Co metallics is 6: 3: 1 than by Pt: Ru: Co, add trisodium citrate again as the metal coating agent, the addition of trisodium citrate is by its integral molar quantity ratio with metallics Pt, Ru and Co, be trisodium citrate: metallics Pt, Ru and Co=1: 1, ultrasonic agitation, the control supersonic frequency is 40KHz, mixing time is 30min, gets the hydrosol;
(3), the preparation of PtRuCo/C
With the pH to 8 of step (2) the gained hydrosol, under 40 ℃, slowly drip NaBH with 0.1M NaOH regulator solution
4As reducing agent, reaction 3h, vacuum filtration, being washed to does not have chlorion in the solution, and 70 ℃ of vacuum drying 12h promptly get a kind of PtRuCo/C ternary alloy nano catalyst of the present invention.
Beneficial effect of the present invention
A kind of PtRuCo/C ternary alloy nano catalyst of the present invention can greatly improve ability of catalyzing methanol in fuel cells.Use trisodium citrate as protective agent in its preparation process, can prepare finely dispersed nanocatalyst, nano particle is difficult for agglomeration takes place, and trisodium citrate is water-soluble protective agent, can the water flush away, and preparation process is simple.
Description of drawings
The TEM figure of Fig. 1, PtRuCo/C
The XRD figure of Fig. 2, PtRuCo/C and PtRu/C (commercialization)
Fig. 3, PtRuCo/C and PtRu/C are at the HClO of pre-absorption monolayer CO
4Stripping volt-ampere curve in the solution
Fig. 4, PtRuCo/C and PtRu/C (commercialization) are respectively at 0.1M HClO
4+ 0.5M CH
3Catalysis methanol cyclic voltammetry curve in the OH solution
The specific embodiment
Below in conjunction with accompanying drawing and instantiation PtRuCo/C Catalysts and its preparation method of the present invention is further specified.
A kind of preparation method of PtRuCo/C ternary alloy nano catalyst comprises being prepared as follows step:
(1), the preparation of carbon slurry
30.6mg active carbon be dissolved in the aqueous solution of 20ml, be warming up to 40 ℃, magnetic agitation, control stir speed (S.S.) 500r/min forms the carbon slurry behind the 30min;
(2), the preparation of the hydrosol
In the carbon slurry of step (1) gained, slowly drip 6ml 0.03mM H successively
2PtCl
6, 7.5ml 0.015mM RuCl
3, 2.5ml 0.005mM CoCl
2, add the 15mg trisodium citrate again as the metal coating agent, ultrasonic agitation, the control supersonic frequency is 40KHz, mixing time is 30min, gets the hydrosol;
(3), the preparation of PtRuCo/C
Step (2) gained is got the pH to 8 of the hydrosol with 0.1M NaOH regulator solution, under 40 ℃, slowly drip 10ml 0.1M NaBH
4As reducing agent, reaction 3h, vacuum filtration, being washed to does not have chlorion in the solution, and 70 ℃ of vacuum drying 12h promptly get a kind of PtRuCo/C ternary alloy nano catalyst of the present invention.
With the PtRuCo/C ternary alloy nano catalyst of gained of the present invention, use transmission electron microscope observation, observed result is seen Fig. 1.As can be seen from Figure 1, suitable little of PtRuCo/C ternary alloy nano particle, the about 4nm of particle diameter, and be dispersed in the surface of active carbon.
Fig. 2 as can be seen, the XRD diffraction maximum of PtRuCo/C obtains by the X-ray diffraction method, and is main because the size ratio Pt of Co is little with respect to the PtRu/C skew that hoists, skew hoists after in the lattice of infiltration Pt.
By current potential such as Fig. 3 of cyclic voltammetric method mensuration PtRuCo/C, as can be seen from Figure 3, PtRuCo/C just can oxidation CO under lower current potential.
Measure the activity of PtRuCo/C and PtRu/C catalysis methanol by pre-absorption monolayer CO method and see Fig. 4, as can be seen from Figure 4, the activity of PtRuCo/C catalysis methanol is far above business-like PtRu/C.
Above said content only is the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.
Claims (2)
1. the preparation method of a PtRuCo/C ternary alloy nano catalyst is characterized in that comprising being prepared as follows step:
(1), the preparation of carbon slurry
Is active carbon to be dissolved in the water in 3: 2 active carbon by the mass ratio of itself and water, is warming up to 40 ℃, magnetic agitation, and control stir speed (S.S.) 500r/min forms the carbon slurry behind the 30min;
(2), the preparation of the hydrosol
In the carbon slurry of step (1) gained, slowly drip H successively
2PtCl
6, RuCl
3, CoCl
2The mole that promptly adds Pt, Ru, Co metallics is 6: 3: 1 than by Pt: Ru: Co, add trisodium citrate again as the metal coating agent, the addition of trisodium citrate is by its integral molar quantity ratio with metallics Pt, Ru and Co, be trisodium citrate: metallics Pt, Ru and Co=1: 1, ultrasonic agitation, the control supersonic frequency is 40KHz, mixing time is 30min, gets the hydrosol;
(3), the preparation of PtRuCo/C
With the pH to 8 of step (2) the gained hydrosol, under 40 ℃, slowly drip NaBH with 0.1M NaOH regulator solution
4As reducing agent, reaction 3h, vacuum filtration, being washed to does not have chlorion in the solution, and 70 ℃ of vacuum drying 12h promptly get a kind of PtRuCo/C ternary alloy nano catalyst of the present invention.
2. the PtRuCo/C ternary alloy nano catalyst of preparation method's gained of an a kind of PtRuCo/C ternary alloy nano catalyst as claimed in claim 1, particle diameter is 3～5nm.
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|---|---|---|---|
| CN2010101003456A CN101773839B (en) | 2010-01-25 | 2010-01-25 | PtRuCo/C ternary alloy nano catalyst and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101003456A CN101773839B (en) | 2010-01-25 | 2010-01-25 | PtRuCo/C ternary alloy nano catalyst and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN101773839A true CN101773839A (en) | 2010-07-14 |
| CN101773839B CN101773839B (en) | 2012-07-25 |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102125865A (en) * | 2011-01-25 | 2011-07-20 | 上海电力学院 | Mesoporous carbon supported Pt nano catalyst and preparation method thereof |
| CN103413951A (en) * | 2013-08-28 | 2013-11-27 | 武汉科技大学 | Nitrogen-doped graphene-loaded Pt-based alloy nanometre electrocatalyst and preparation method thereof |
| CN104393312A (en) * | 2014-11-19 | 2015-03-04 | 中国科学院长春应用化学研究所 | Preparation method of ultralow platinum-loading capacity Pt-CoP/C anode electrocatalyst for high-activity high-stability direct methanol fuel cell |
| CN106910906A (en) * | 2017-02-28 | 2017-06-30 | 上海电力学院 | A kind of Pd Cu Co/C ternary fuel cell anode catalysts and preparation method and application |
| CN108786434A (en) * | 2018-06-21 | 2018-11-13 | 重庆文理学院 | A kind of efficient bioengineering tail gas treatment device and its processing method, fermentation tank |
| CN109065894A (en) * | 2018-07-04 | 2018-12-21 | 上海交通大学 | Without film anaerobic direct methanol fuel cell three-dimensional gradient structure anode and preparation method |
| CN110635146A (en) * | 2019-08-23 | 2019-12-31 | 同济大学 | High-performance Pt-based tri-alloy catalyst and preparation method thereof |
-
2010
- 2010-01-25 CN CN2010101003456A patent/CN101773839B/en active Active
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102125865A (en) * | 2011-01-25 | 2011-07-20 | 上海电力学院 | Mesoporous carbon supported Pt nano catalyst and preparation method thereof |
| CN102125865B (en) * | 2011-01-25 | 2012-10-17 | 上海电力学院 | Mesoporous carbon supported Pt nano catalyst and preparation method thereof |
| CN103413951A (en) * | 2013-08-28 | 2013-11-27 | 武汉科技大学 | Nitrogen-doped graphene-loaded Pt-based alloy nanometre electrocatalyst and preparation method thereof |
| CN104393312A (en) * | 2014-11-19 | 2015-03-04 | 中国科学院长春应用化学研究所 | Preparation method of ultralow platinum-loading capacity Pt-CoP/C anode electrocatalyst for high-activity high-stability direct methanol fuel cell |
| CN106910906A (en) * | 2017-02-28 | 2017-06-30 | 上海电力学院 | A kind of Pd Cu Co/C ternary fuel cell anode catalysts and preparation method and application |
| CN108786434A (en) * | 2018-06-21 | 2018-11-13 | 重庆文理学院 | A kind of efficient bioengineering tail gas treatment device and its processing method, fermentation tank |
| CN108786434B (en) * | 2018-06-21 | 2021-02-26 | 重庆文理学院 | Efficient bioengineering tail gas treatment equipment and method and fermentation tank |
| CN109065894A (en) * | 2018-07-04 | 2018-12-21 | 上海交通大学 | Without film anaerobic direct methanol fuel cell three-dimensional gradient structure anode and preparation method |
| CN110635146A (en) * | 2019-08-23 | 2019-12-31 | 同济大学 | High-performance Pt-based tri-alloy catalyst and preparation method thereof |
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| CN101773839B (en) | 2012-07-25 |
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Effective date of registration: 20141217 Address after: 200090 Pingliang Road, Shanghai, No. 2103, No. Patentee after: Shanghai University of Electric Power Patentee after: State Grid Shanghai Municipal Electric Power Company Address before: 200090 Pingliang Road, Shanghai, No. 2103, No. Patentee before: Shanghai University of Electric Power |