CN102836707A - Photochemical preparation method for Pd core @Pt shell nanometer catalyst - Google Patents
Photochemical preparation method for Pd core @Pt shell nanometer catalyst Download PDFInfo
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- CN102836707A CN102836707A CN2012103630297A CN201210363029A CN102836707A CN 102836707 A CN102836707 A CN 102836707A CN 2012103630297 A CN2012103630297 A CN 2012103630297A CN 201210363029 A CN201210363029 A CN 201210363029A CN 102836707 A CN102836707 A CN 102836707A
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- solution
- nuclear
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- preparation
- mixed solution
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- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000003054 catalyst Substances 0.000 title claims abstract description 19
- 239000000243 solution Substances 0.000 claims abstract description 35
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000011259 mixed solution Substances 0.000 claims abstract description 20
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 14
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 12
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 5
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 5
- 239000000460 chlorine Substances 0.000 claims abstract description 5
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 26
- 239000011943 nanocatalyst Substances 0.000 claims description 22
- 239000000203 mixture Substances 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 11
- 238000002835 absorbance Methods 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 239000002105 nanoparticle Substances 0.000 claims description 8
- 230000003287 optical effect Effects 0.000 claims description 8
- 238000001228 spectrum Methods 0.000 claims description 8
- 239000006229 carbon black Substances 0.000 claims description 7
- 101150003085 Pdcl gene Proteins 0.000 claims description 4
- 238000011068 loading method Methods 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims description 4
- 150000002739 metals Chemical class 0.000 claims description 2
- 230000004048 modification Effects 0.000 claims description 2
- 238000012986 modification Methods 0.000 claims description 2
- 230000005855 radiation Effects 0.000 claims description 2
- 238000002156 mixing Methods 0.000 abstract description 7
- 239000000446 fuel Substances 0.000 abstract description 4
- 238000003756 stirring Methods 0.000 abstract description 4
- 230000001678 irradiating effect Effects 0.000 abstract 2
- 229910002621 H2PtCl6 Inorganic materials 0.000 abstract 1
- 229910002666 PdCl2 Inorganic materials 0.000 abstract 1
- 150000001875 compounds Chemical group 0.000 abstract 1
- 239000011258 core-shell material Substances 0.000 abstract 1
- 238000002386 leaching Methods 0.000 abstract 1
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000002131 composite material Substances 0.000 description 5
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 description 4
- 239000000084 colloidal system Substances 0.000 description 4
- JLFNLZLINWHATN-UHFFFAOYSA-N pentaethylene glycol Chemical compound OCCOCCOCCOCCOCCO JLFNLZLINWHATN-UHFFFAOYSA-N 0.000 description 4
- 239000010453 quartz Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 229910002849 PtRu Inorganic materials 0.000 description 1
- 229910018879 Pt—Pd Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000004900 laundering Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 238000007540 photo-reduction reaction Methods 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004758 underpotential deposition Methods 0.000 description 1
Classifications
-
- 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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- Catalysts (AREA)
Abstract
The invention provides a photochemical preparation method for a Pd core @Pt shell nanometer catalyst and relates to a preparation method for a catalyst. The preparation method comprises the following steps: taking and mixing PdCl2 aqueous solution, polyethylene glycol and acetone aqueous solution, thereby obtaining a mixed solution a; taking and mixing H2PtCl6 aqueous solution, polyethylene glycol and acetone aqueous solution, thereby obtaining a mixed solution b; irradiating the mixed solution a by adopting ultraviolet rays, thereby obtaining a nanometer Pd colloidal solution c; mixing the solution c with the mixed solution b, thereby obtaining a mixed solution d; irradiating the mixed solution d by adopting the ultraviolet rays, thereby obtaining a Pd core @Pt shell nanometer colloidal solution e; and under the condition of the colloidal solution e obtained through stirring, immersing a carbon carrier for 2-24h, leaching and washing with de-ionized water till no chlorine exists, thereby obtaining the Pd core @Pt shell nanometer catalyst. The catalyst nanometer grain obtained according to the technology has a core-shell compound structure; the size of the grain is easily controlled and the monodispersity is excellent; and the preparation method is widely applied to the field of low-temperature fuel cells.
Description
Technical field
The present invention relates to a kind of Preparation of catalysts method, particularly relate to a kind of photochemical method for preparation of Pd nuclear Pt shell nanocatalyst.
Background technology
The low-temperature fuel cell catalyst is one of main direction of this art development at present cheaply.Commercial catalyst is mainly Pt/C and PtRu/C catalyst at present.Because the price that Pd is cheaper with respect to Pt reaches catalytic activity widely, Pd has caused researcher's concern in recent years.Pd nuclear Pt shell nanostructured can make the Pt that price is higher, catalytic performance is good mainly be distributed in the catalyst pellets sub-surface, helps improving the utilization rate of Pt, reduces the catalyst cost.Patent CN 102107137A proposes a kind of precursor solution impregnated carrier, heat chemistry reduction preparation Pt-Pd catalyst method.This method can not obtain Pd nuclear Pt shell structure.K. Sasaki etc. is at Pd particle surface deposited monolayers Cu atom; And then with Pt atomic substitutions Cu atom (underpotential deposition method); Synthesized Pd nuclear Pt core/shell nanoparticles with monoatomic layer Pt shell (Electrochimica Acta, 2010,55:2645-2652.).This method complex process, have relatively high expectations and the reaction time longer, be difficult for to amplify.The method of utilizing photoreduction to prepare Pd nuclear Pt shell nanocatalyst then has the advantage of a series of uniquenesses.For example, the Pd of acquisition nuclear Pt shell nanometer material is pure, compares with the chemical reagent reducing process, does not have excessive chemical reducing agent or reducing agent product the absorption that particle produces is polluted; Preparation technology is simple, and cost is low; The catalyst nanoparticles that obtains has nuclear-shell composite structure; It is good or the like to be easy to control size, the monodispersity of particle.
Summary of the invention
The object of the present invention is to provide a kind of photochemical method for preparation of Pd nuclear Pt shell nanocatalyst, this method technology is simple, and cost is low; The catalyst nanoparticles that obtains has nuclear-shell composite structure; The size, the monodispersity that are easy to control particle are good; Be adapted at the extensive use of low-temperature fuel cell field.
The objective of the invention is to realize through following technical scheme:
A kind of photochemical method for preparation of Pd nuclear Pt shell nanocatalyst, said method comprises following preparation process:
1. get PdCl
2The aqueous solution, polyethylene glycol, aqueous acetone solution mix, and obtain mixed solution a, get H
2PtCl
6The aqueous solution, polyethylene glycol, aqueous acetone solution mix, and obtain mixed solution b;
2. the ultraviolet irradiation step of using at least a wavelength between wavelength 200 ~ 360 nm is gained mixed solution a 1.; Till the surface plasma resonance optical spectrum absorbance of solution system Pd particle no longer changes, stop irradiation, promptly obtain nanometer Pd colloidal solution c; With solution c and step 1. gained mixed solution b arbitrary proportion mix; Obtain mixed solution d, with 2. gained mixed solution d of the ultraviolet irradiation step of at least a wavelength between wavelength 200 ~ 360 nm, till the surface plasma resonance optical spectrum absorbance of solution system no longer changes; Stop irradiation, obtain Pd nuclear Pt shell nano-sized colloidal solution e;
3. 2. obtain under the condition of colloidal solution e at whipping step, carbon carrier is immersed 2 ~ 24h, suction filtration also spends deionised water to there not being chlorine, promptly obtains Pd nuclear Pt shell nanocatalyst.
The photochemical method for preparation of described a kind of Pd nuclear Pt shell nanocatalyst, the nano particle structure of said acquisition is a nucleocapsid structure, and Pd nuclear Pt shell.
The photochemical method for preparation of described a kind of Pd nuclear Pt shell nanocatalyst, the said step 2. total radiation intensity of ultraviolet light is 0.5 ~ 1 x 10
6Cal/m
2S.
The photochemical method for preparation of described a kind of Pd nuclear Pt shell nanocatalyst; Said each mixed solution metal total concentration scope is: 40 ~ 250mg/L; Said polyethylene glycol (polyethylene glycol; PEG) molecular weight can be from 400-6000, and polyethylene glycol is 10 ~ 1000: 1 with the metal quality ratio, and acetone is 200 ~ 2000: 1 with the metal quality ratio.
The photochemical method for preparation of described a kind of Pd nuclear Pt shell nanocatalyst, said step 3. carbon carrier be the carbon black of carbon black, CNT or modification, one or more mixtures in the CNT, the specific area of carrier is 100 ~ 2000m
2/ g.
The photochemical method for preparation of described a kind of Pd nuclear Pt shell nanocatalyst, the total loading of said catalyst metals is 10 ~ 60%.
Advantage of the present invention and effect are:
Preparation technology of the present invention is simple, and cost is low; The catalyst nanoparticles that obtains has nuclear-shell composite structure; The size, the monodispersity that are easy to control particle are good; Be adapted at the extensive use of low-temperature fuel cell field.
Description of drawings
Fig. 1 is the CV curve of the Pd nuclear Pt shell nanocatalyst of embodiment 1 preparation.
The specific embodiment
Below in conjunction with embodiment the present invention is elaborated.
Embodiment 1
1) gets the PdCl that 2 ml contain Pd (II) 300 mg/L
2Solution adds PEG400 2.5 g behind the dilute with water, 2 ml acetone are settled to 25 ml, mixing with water.
2) mixture solution is transferred in the quartz reactor, (48W) irradiation 15 min under 254 nm uviol lamps are till the surface plasma resonance optical spectrum absorbance of solution system Pd particle no longer changes.
3) get the H that 2 ml contain Pt (IV) 600 mg/L
2PtCl
6Solution adds PEG400 2.5 g, 2 ml acetone and steps 2 behind the dilute with water) gained nanometer Pd colloidal solution, be settled to 50 ml, mixing with water.
4) mixture solution is transferred in the quartz reactor; (48W) irradiation 20 min under 254 nm uviol lamps; Till the surface plasma resonance optical spectrum absorbance of solution system metallic no longer changes, promptly obtain the Pd nuclear Pt shell nano-colloid of Pd:Pt mass ratio 1:2.Ratio in catalyst loadings 20%; (carbon black: sodium borohydride: quality compares 1:1:100 with the above-mentioned Pd nuclear Pt shell composite nanometer particle colloid for preparing with through pretreated XC-72 carbon black; Stir 8 h, filtration is also clean with massive laundering, oven dry 36 h under 105 ℃ of conditions.) mix, stirring 12h, suction filtration also spends deionised water to there not being chlorine, promptly obtains Pd nuclear Pt shell nanocatalyst.Fig. 1 is the CV curve of the Pd nuclear Pt shell nanocatalyst for preparing of embodiment.
1) gets the PdCl that 3.2 ml contain Pd (II) 300 mg/L
2Solution adds PEG400 4 g behind the dilute with water, 3.2 ml acetone are settled to 40 ml, mixing with water.
2) mixture solution is transferred in the quartz reactor, (48W) irradiation 15 min under 254 nm uviol lamps are till the surface plasma resonance optical spectrum absorbance of solution system gold particle no longer changes.
3) get the H that 0.8 ml contains Pt (IV) 600 mg/L
2PtCl
6Solution adds PEG400 1 g, 0.8 ml acetone and step 2 behind the dilute with water) gained nanometer Pd colloidal solution, be settled to 50 ml, mixing with water.
4) mixture solution is transferred in the quartz reactor; (48W) irradiation 15 min under 254 nm uviol lamps; Till the surface plasma resonance optical spectrum absorbance of solution system metallic no longer changes, promptly obtain the Pd nuclear Pt shell nano-colloid of Pd:Pt mass ratio 2:1.Ratio in catalyst loadings 20%; Mix with the above-mentioned Pd nuclear Pt shell composite nanometer particle colloid for preparing with through pretreated XC-72 carbon black (with embodiment 1); Stir 12h, suction filtration also spends deionised water to there not being chlorine, promptly obtains Pd nuclear Pt shell nanocatalyst.
Claims (6)
1. the photochemical method for preparation of Pd nuclear Pt shell nanocatalyst is characterized in that said method comprises following preparation process:
1. get PdCl
2The aqueous solution, polyethylene glycol, aqueous acetone solution mix, and obtain mixed solution a, get H
2PtCl
6The aqueous solution, polyethylene glycol, aqueous acetone solution mix, and obtain mixed solution b;
2. the ultraviolet irradiation step of using at least a wavelength between wavelength 200 ~ 360 nm is gained mixed solution a 1.; Till the surface plasma resonance optical spectrum absorbance of solution system Pd particle no longer changes, stop irradiation, promptly obtain nanometer Pd colloidal solution c; With solution c and step 1. gained mixed solution b arbitrary proportion mix; Obtain mixed solution d, with 2. gained mixed solution d of the ultraviolet irradiation step of at least a wavelength between wavelength 200 ~ 360 nm, till the surface plasma resonance optical spectrum absorbance of solution system no longer changes; Stop irradiation, obtain Pd nuclear Pt shell nano-sized colloidal solution e;
3. 2. obtain under the condition of colloidal solution e at whipping step, carbon carrier is immersed 2 ~ 24h, suction filtration also spends deionised water to there not being chlorine, promptly obtains Pd nuclear Pt shell nanocatalyst.
2. the photochemical method for preparation of a kind of Pd nuclear Pt shell nanocatalyst according to claim 1 is characterized in that the nano particle structure of said acquisition is a nucleocapsid structure, and Pd nuclear Pt shell.
3. the photochemical method for preparation of a kind of Pd nuclear Pt shell nanocatalyst according to claim 1 is characterized in that the said step 2. total radiation intensity of ultraviolet light is 0.5 ~ 1 x 10
6Cal/m
2S.
4. the photochemical method for preparation of a kind of Pd nuclear Pt shell nanocatalyst according to claim 1; It is characterized in that; Said each mixed solution metal total concentration scope is: 40 ~ 250mg/L, said polyethylene glycol (polyethylene glycol, PEG) molecular weight can be from 400-6000; Polyethylene glycol is 10 ~ 1000: 1 with the metal quality ratio, and acetone is 200 ~ 2000: 1 with the metal quality ratio.
5. the photochemical method for preparation of a kind of Pd nuclear Pt shell nanocatalyst according to claim 1; It is characterized in that; Said step 3. carbon carrier be the carbon black of carbon black, CNT or modification, one or more mixtures in the CNT, the specific area of carrier is 100 ~ 2000m
2/ g.
6. the photochemical method for preparation of a kind of Pd nuclear Pt shell nanocatalyst according to claim 1 is characterized in that the total loading of said catalyst metals is 10 ~ 60%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015156027A1 (en) * | 2014-04-11 | 2015-10-15 | トヨタ自動車株式会社 | Methods for manufacturing catalyst particles and carbon-supported catalysts |
| CN105449235A (en) * | 2015-11-10 | 2016-03-30 | 武汉理工大学 | Optical auxiliary preparation method for Au@Pt-Au core-shell nanoparticles with controllable surface components |
| WO2016051960A1 (en) * | 2014-10-02 | 2016-04-07 | トヨタ自動車株式会社 | Method for producing core-shell catalyst |
| CN115386897A (en) * | 2022-08-22 | 2022-11-25 | 华南理工大学 | High-exposure platinum nanocluster HER electrocatalyst and preparation method and application thereof |
-
2012
- 2012-09-26 CN CN2012103630297A patent/CN102836707A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 《中国优秀硕士学位论文全文数据库 工程科技I辑》 20120515 赵恩格 "贵金属核壳结构纳米催化剂的光化学合成及其甲醇阳极氧化催化特性研究" 第14页1.3第2段，第19-20页 1-6 , 第05期 * |
| 赵恩格: ""贵金属核壳结构纳米催化剂的光化学合成及其甲醇阳极氧化催化特性研究"", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015156027A1 (en) * | 2014-04-11 | 2015-10-15 | トヨタ自動車株式会社 | Methods for manufacturing catalyst particles and carbon-supported catalysts |
| JP2015202434A (en) * | 2014-04-11 | 2015-11-16 | トヨタ自動車株式会社 | Method for producing catalyst particulate and carbon carrying catalyst |
| WO2016051960A1 (en) * | 2014-10-02 | 2016-04-07 | トヨタ自動車株式会社 | Method for producing core-shell catalyst |
| JP2016073895A (en) * | 2014-10-02 | 2016-05-12 | トヨタ自動車株式会社 | Method for producing core-shell catalyst |
| CN105449235A (en) * | 2015-11-10 | 2016-03-30 | 武汉理工大学 | Optical auxiliary preparation method for Au@Pt-Au core-shell nanoparticles with controllable surface components |
| CN105449235B (en) * | 2015-11-10 | 2017-11-17 | 武汉理工大学 | A kind of light assistant preparation method of the controllable Au@Pt Au core-shell nanos of surface composition |
| CN115386897A (en) * | 2022-08-22 | 2022-11-25 | 华南理工大学 | High-exposure platinum nanocluster HER electrocatalyst and preparation method and application thereof |
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Application publication date: 20121226 |