CN103191757B - PdNiW/C ternary alloy nano catalyst and preparation method thereof - Google Patents
PdNiW/C ternary alloy nano catalyst and preparation method thereof Download PDFInfo
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Abstract
本发明公开一种PdNiW/C三元合金纳米催化剂及其制备方法，所述PdNiW/C三元合金纳米催化剂以Pd、Ni和W为活性中心，以活性炭为载体，按摩尔比计算，Pd：Ni：W为7：2：1，按质量比计算，即活性炭的质量：Pd,Ni和W的总质量为4：1。其制备方法即将PdCl2,NiCl2·6H2O,Na2WO4的乙二醇溶液混合后调节pH值至9，升温至80℃反应1h后加入活性炭继续搅拌反应30min，加柠檬酸钠水溶液超声30min，再加NaBH4水溶液于50℃下搅拌反应3h，冷至室温后进行真空抽滤、洗涤、干燥，即得分散性良好，对碱性环境中乙醇催化氧化性能较好的PdNiW三元合金纳米催化剂。
The invention discloses a PdNiW/C ternary alloy nanocatalyst and a preparation method thereof. The PdNiW/C ternary alloy nanocatalyst uses Pd, Ni and W as active centers and activated carbon as a carrier. Calculated by molar ratio, Pd: Ni: W is 7:2:1, calculated by mass ratio, that is, the mass of activated carbon: the total mass of Pd, Ni and W is 4:1. The preparation method is to mix the ethylene glycol solutions of PdCl 2 , NiCl 2 6H 2 O, and Na 2 WO 4 , adjust the pH value to 9, raise the temperature to 80°C for 1 hour, add activated carbon and continue stirring for 30 minutes, add sodium citrate aqueous solution Ultrasound for 30 minutes, then add NaBH 4 aqueous solution and stir at 50°C for 3 hours. After cooling to room temperature, carry out vacuum filtration, washing and drying to obtain a PdNiW ternary compound with good dispersion and good catalytic oxidation performance for ethanol in alkaline environment. alloy nanocatalysts.
Description
Technical field
The invention belongs to nano-catalyst material preparing technical field, be specifically related to one, to ethanol, there is high catalytic activity PdNiW/C ternary alloy nano catalyst and preparation method thereof.
Background technology
Catalyst plays vital effect in a fuel cell.Fuel cell catalyst used no matter cathod catalyst or anode catalyst is all based on the noble metal catalyst of Pt system metal.Pt system metal expensive, in cost, occupy very large proportion, this kind of catalyst is subject to the reasons such as the restriction of resource in addition, develops highly active new catalyst, improves its utilization rate and reduces consumption, is the direction that fuel cell studies personnel make great efforts always.In recent years, it is found that and adopt Pd as fuel-cell catalyst successful, research achieved certain achievement.
Pd catalyst is catalyst emerging in fuel cell in recent years, remarkable to the catalytic oxidation effect of fuel cell
[1,2], cause the attention of people gradually.Fuel cell Pd catalyst is mainly at direct alcohol fuel cell (DAFC)
[3], direct methanoic acid fuel cell (DFAFC)
[4,5]and Proton Exchange Membrane Fuel Cells (PEMFC)
[6,7]etc. the wider model of application study of aspect, in alcohol fuel battery, application prospect is comparatively wide.
It has been recognized that Pd metallic catalyst has great commercial value in a fuel cell.Although the catalytic mechanism of Pd metallic catalyst and mechanism of poisoning aspect are not also completely understood at present, along with people go deep into the research of Pd metallic catalyst, Pd metal will probably replace in future the new catalyst that Pt becomes fuel cell.
The present invention adopts sodium borohydride and ethylene glycol to make reducing agent, prepares PdNiW/C ternary nanocatalyst by liquid phase reduction, mainly studies it to the catalytic oxidation activity of ethanol.Because current Direct Ethanol Fuel Cell research is limited, and the not equal reason of each experimental system, there is no similar report of the present invention.
bibliography
[1] Ruban, B. Hammer, P. Stoltze, H. L. et al. Surface electronic structure and reactivity of transition and noble metals [J]. Journal of Molecular Catalysis A: Chemical, 1997, 115(7):421-429
[2] B. Hammer, J.K. Norskov. Electronic factors determining the reactivity of metal surfaces [J]. Surface Science, 1995, 343(3):211-220
[3] J. Greeley, J.K. Norskov, M. Maurikakis, Annu. A general scheme for the estimation of oxygen binding energies on binary transition metal surface alloys [J]. Surface Science, 2005, 592(1~3):104-111
[4] Grgur B N; Markovic N M; Ross P N. Electrooxidation of H2, CO and H2/CO mixtures on a well-characterized Pt-Re bulk alloy electrode and comparison with other Pt binary alloys [J]. Electrochimica Acta, 1998, 43(24):3631-3635
[5] Zhang, Z.H; Huang, Y.J; Ge, J.J; et al. WO3/C hybrid material as a highly active catalyst support for formic acid electrooxidation [J]. Electrochemistry Communications. 2008, 10(8):1113-1116.
[6] Lee, E.P; Peng, Z.M; Chen, W; et al. Electrocatalytic properties of Pt nanowires supported on Pt and W Gauzes [J]. ACS Nano. 2008, 2(10):2167-2173.
[7] Meza, D; Morales, U; Roquero, P; et al. Oxygen reduction on carbon supported Pt-W electrocatalysts [J]. International Journal of hydrogen energy. 2010, 35(21):12111-12114
[8] Wang Z.B; Zuo, P.J; Yin, G.P. Effect of W on activity of Pt-Ru/C catalyst for methanol electrooxidation in acidic medium [J]. Journal of Alloys and Compounds. 2009, 479(1-2):395-400.
[9] Feng, L.G; Yan, L; Cui, Z.M; et al. High activity of Pd-WO3/C catalyst as anodic catalyst for direct formic acid fuel cell [J]. Journal of Power Sources. 2011, 196(5):2469-2474.
[10] Li W Z , Liang C H , Qiu J S , et al. Carbon nanotubes as support for cathode catalyst of a direct methanol fuel cell [J]. Carbon , 2002 , 40(5):791-794
[11] Li W Z , Liang C H , Zhou WJ , et al. Preparation and characterization of multiwalled carbon nanotube2supported platinum for cathode catalysts of direct methanol fuel cells [J]. J. Phys. Chem. B, 2003, 107: 6292-6299.
[12] Li W Z, Liang C H , Zhou WJ , et al. Homogeneous and control lable Pt particles deposited on multiwall carbon nanotubes as cath2 ode catalyst for direct methanol fuel cells [J]. Carbon, 2004, 42:423
[13] Gao H L, Liao S J, Liang Z X, et al. Anodic oxidation of ethanol on core-shell structured Ru@PtPd/C catalyst in alkaline media[J]. Journal of Power Sources, 2011, 196(15): 6138-6143.
Summary of the invention
An object of the present invention is to provide a kind of PdNiW/C ternary alloy nano catalyst.
Two of object of the present invention is to provide the preparation method of above-mentioned a kind of PdNiW/C ternary alloy nano catalyst.
Know-why of the present invention
The present invention adopts sodium borohydride and ethylene glycol co-reducing process, and wherein ethylene glycol not only makes reducing agent but also make dispersant, has prepared the PdNiW/C nanocatalyst of good dispersion property.The rate of reduction of ethylene glycol is comparatively slow, efficiently avoid the concentrated growth of nano-metal particle, thus avoids the generation of agglomeration.Adding sodium borohydride is because the reproducibility of ethylene glycol is more weak, makes up shortcoming metal ion thoroughly can not reduced.
Technical scheme of the present invention
A kind of PdNiW/C ternary alloy nano catalyst, being with Pd, Ni, W for activated centre, take active carbon as the PdNiW/C ternary alloy nano catalyst that carrier is formed;
The described activated centre of PdNiW/C ternary alloy nano catalyst and the amount of carrier active carbon, calculate in mass ratio, i.e. the quality of active carbon: the gross mass of Pd, Ni and W is preferably 4:1;
In the activated centre of described PdNiW/C ternary alloy nano catalyst, calculate in molar ratio, Pd:Ni:W is preferably 7:2:1;
Described absorbent charcoal carrier is preferably XC-72 active carbon.
The preparation method of above-mentioned a kind of PdNiW/C ternary alloy nano catalyst, specifically comprises the steps:
(1), by PdCl
2be dissolved in ethylene glycol solution, ultrasonic formation solution 1;
(2) successively NiCl is dripped in the solution 1, formed to step (1)
2ethylene glycol solution, Na
2wO
4ethylene glycol solution, then use the NaOH ethylene glycol solution adjust ph to 9 of 1mol/L, in 80 DEG C reaction 1h after mixed liquor 2;
(3), in active carbon ethylene glycol is added, ultrasonic formation suspension 1;
Control to drip suspension 1 in the mixed liquor 2 that drop rate formed for 2-2.5ml/min in step (2), drip rear continuation stirring reaction 30min, then adding mass percent concentration is 1 g L
-1sodium citrate aqueous solution, ultrasonic 30min, then to add mass percent concentration be 1 g L
-1naBH
4the aqueous solution, at 50 DEG C, stirring reaction 3h obtains suspension 2;
The amount of active carbon used and ethylene glycol in described suspension 1, in active carbon: ethylene glycol is that the ratio of 1mg:1.25ml calculates;
The natrium citricum added and NaBH
4amount calculate in molar ratio relative to the total amount of Pd, Ni and W, the molal quantity of namely total Pd, Ni and W: natrium citricum molal quantity: NaBH
4molal quantity=1:1:1;
(4), the suspension 2 of step (3) gained is cooled to room temperature final vacuum suction filtration, preferred controlled pressure is-0.1MPa, and the filter cake tap water of gained is washed till without chlorion in solution, then vacuum drying, preferred control temperature is 90 DEG C, obtains PdNiW/C ternary alloy nano catalyst.
Above-mentioned a kind of PdNiW/C ternary alloy nano catalyst is to Catalytic oxidation of ethanol better performances in alkaline environment.
Beneficial effect of the present invention
The preparation method of a kind of PdNiW/C ternary alloy nano catalyst of the present invention, owing to adopting sodium borohydride and ethylene glycol as reducing agent, wherein ethylene glycol not only makes reducing agent but also make dispersant, the rate of reduction of ethylene glycol is slower, efficiently avoid the concentrated growth of nano-metal particle, thus avoid the generation of agglomeration, the therefore PdNiW/C nanocatalyst favorable dispersibility of final gained.
A kind of PdNiW/C ternary alloy nano catalyst of the present invention, due to adding containing Ni element, NiO is formed in preparation process, NiO can increase the active sites of Pd, improve the utilization rate of Pd, thus raising catalyst resists poisoning ability, in addition, due to adding containing W element, in preparation process, form WO
3, WO
3the active sites of Pd can be increased, improve the utilization rate of Pd, thus improve the activity of PdNiW/C ternary alloy nano catalyst.
In addition, a kind of PdNiW/C ternary alloy nano catalyst of the present invention to Catalytic oxidation of ethanol better performances in alkaline environment, with PdNiW(7:2:1 in one embodiment of the invention) PdNiW(7:2:1 that formed of/C nano catalyst)/C catalysis electrode is that current density that-0.12V is corresponding is up to 51.93 mAcm at spike potential
-2.
Accompanying drawing explanation
The TEM figure of the PdNiW/C ternary alloy nano catalyst of Fig. 1, embodiment 1 gained;
The XRD figure of the PdNiW/C ternary alloy nano catalyst of Fig. 2, embodiment 1 gained;
Fig. 3, PdNiW(7:2:1)/C catalysis electrode and Pd/C(JM) catalysis electrode is at 1molL
-1c
2h
5oH+1molL
-1chronoa mperometric plot in KOH solution;
Fig. 4, PdNiW/C catalysis electrode is at 1molL
-1stripping Voltammetry curve in KOH solution.
Detailed description of the invention
Also by reference to the accompanying drawings the present invention is set forth further below by specific embodiment, but do not limit the present invention.
The model of various equipment used in the embodiment of the present invention and the information of manufacturer as follows:
Transmission electron microscope, model JEM-2100F, Japanese JEOL company produces;
X-ray powder diffraction instrument is German Bruker D8-ADVANCE type, and radiation source is Cu K
(
=0.15418nm), step-length 0.0167 °, often step stops 1s, and sweep limits is 20 ~ 90 °;
CHI660C electrochemical workstation, Shanghai Chen Hua instrument company.
Active carbon used is XC-72 active carbon, and manufacturer is Cabot company of the U.S.;
The specification of various raw materials used in the embodiment of the present invention and the information of manufacturer as follows:
Palladium bichloride PdCl
2, analyze pure, Shanghai fine chemistry industry Materials Research Laboratories;
Sodium borohydride, analyzes pure, Chemical Reagent Co., Ltd., Sinopharm Group
Ethylene glycol, analyzes pure, Chemical Reagent Co., Ltd., Sinopharm Group;
NaOH, analyzes pure, Solution on Chemical Reagents in Shanghai Co., Ltd;
NiCl
26H
2o, Na
2wO
4, analyze pure, Chemical Reagent Co., Ltd., Sinopharm Group.
embodiment 1
A kind of PdNiW/C ternary alloy nano catalyst is with Pd, Ni and W for activated centre, with XC-72 active carbon for carrier and the PdNiW/C ternary alloy nano catalyst that formed;
The activated centre of described PdNiW/C ternary alloy nano catalyst and the amount of carrier XC-72 active carbon calculate in mass ratio, i.e. the quality of XC-72 active carbon: the gross mass of Pd, Ni and W is 4:1;
In the activated centre of described PdNiW/C ternary alloy nano catalyst, calculate in molar ratio, Pd:Ni:W is 7:2:1.
The preparation method of above-mentioned a kind of PdNiW/C ternary alloy nano catalyst, concrete steps are as follows:
(1), by 11.86mgPdCl
2be dissolved in 50ml ethylene glycol solution, ultrasonic 1h, form solution 1;
(2) successively 0.5g L is dripped in the solution 1, formed to step (1)
-1niCl
26H
2the ethylene glycol solution 9.1ml of O, 1g L
-1na
2wO
4ethylene glycol solution 2.8ml, by the ethylene glycol solution adjust ph to 9 of 1MNaOH, 80 DEG C reaction 1h after mixed liquor 2;
(3), take the XC-72 active carbon of 40mg, add 50ml ethylene glycol, after ultrasonic 30min, form suspension 1;
Control to drip suspension 1 in the mixed liquor 2 that drop rate formed for 2ml/min in step (2), after ultrasonic 30min, then add 1 g L
-1sodium citrate aqueous solution 28.1ml, ultrasonic 30min, continue to add 1 g L
-1naBH
4aqueous solution 21.7ml, continues stirring reaction 3h and obtains suspension 2 at 50 DEG C;
(4) vacuum filtration is carried out after, the suspension 2 of step (3) gained being cooled to room temperature, suction filtration process control pressure is-0.1MPa, the filter cake tap water of gained is washed till without chlorion in solution, then 90 DEG C of vacuum drying 12h, obtains PdNiW/C ternary alloy nano catalyst.
The PdNiW/C ternary alloy nano catalyst of transmission electron microscope to above-mentioned gained is utilized to scan, the TEM figure of gained as shown in Figure 1, Pd nano particle can be clearly found out from Fig. 1, be evenly distributed, obtaining the average nanometer particle size of PdNiW/C ternary alloy nano catalyst through statistical computation is 4.2nm.
The XRD analysis result utilizing X-ray diffraction to scan to draw as shown in Figure 2, with the standard card (JCPDS of Pd, No.65-6174) compare, it is the crystal face diffraction of (111), (200), (220) and (311) of 40.14 °, 46.69 °, 68.17 ° and the 82.17 ° corresponding metal Pds of difference at the angle of diffraction 2 θ, the characteristic diffraction peak can also observing C from Fig. 2 disappears and without any other impurity peaks, shows that metal Pd successfully loads on XC-72 absorbent charcoal carrier thus.
application Example 1
By the PdNiW/C ternary alloy nano catalyst of embodiment 1 gained and PdNiW(7:2:1) 20%Pd/C catalyst (hereinafter the adopting Pd/C(JM) catalyst produced of/C ternary alloy nano catalyst and Johnson Matthey company of the U.S. represents) being made into catalysis electrode respectively, step is as follows:
Working electrode is glass carbon (GC) electrode (d=3mm), with 0.3 before using
the Al of m
2o
3powder is milled to minute surface on chamois leather, then uses deionized water and absolute ethyl alcohol supersound washing respectively.
Take the PdNiW(7:2:1 of 5mg embodiment 1 gained respectively)/C ternary alloy nano catalyst, Pd/C(JM) catalyst is dissolved in the 1mL absolute ethyl alcohol aqueous solution (absolute ethyl alcohol: the volume ratio of water is 1:4) respectively, adds 120 respectively
l 5%Nafion solution, respectively ultrasonic vibration 30min, distribution gets 4
l dispersant liquid drop, on glass-carbon electrode, dries respectively, obtains PdNiW(7:2:1)/C catalysis electrode and Pd/C(JM) catalysis electrode.
The PdNiW(7:2:1 will prepared respectively)/C catalysis electrode and Pd/C(JM) catalysis electrode is as working electrode, all with saturated calomel electrode (SCE) for reference electrode, Pt sheet is that auxiliary electrode forms three electrode test systems, CHI660C electrochemical workstation carries out chronoa mperometric plot test, result as shown in Figure 3, 1-PdNiW in Fig. 3 is PdNiW(7:2:1)/C catalysis electrode, 2-PdC (JM) is Pd/C(JM) catalysis electrode, as can be seen from Figure 3 PdNiW(7:2:1) PdNiW(7:2:1 that formed of/C ternary alloy nano catalyst)/C catalysis electrode is that the current density that-0.12V is corresponding reaches maximum 51.93 mAcm at spike potential
-2, than Pd/C(JM) and the Pd/C(JM that formed of catalyst) 48.70 mAcm of catalysis electrode
-2also high, PdNiW(7:2:1 is described)/C ternary alloy nano catalyst to the catalytic activity of ethanol than Pd/C(JM) catalyst is good.
PdNiW(7:2:1 using preparing)/C catalysis electrode is as working electrode, and with saturated calomel electrode (SCE) for reference electrode, Pt sheet is that auxiliary electrode forms three electrode test systems, CHI660C electrochemical workstation is tested it at 1molL
-1cyclic voltammetry curve in KOH solution, result as shown in Figure 4, extrapolates PdNiW(7:2:1 according to the adsorption desorption peak of " H " in Fig. 4) active surface area of/C catalyst is 27.5m
2/ g, shows that Pd metal is reducing loaded on XC-72 absorbent charcoal carrier, and has high electrochemical activity surface area.
A kind of PdNiW/C ternary alloy nano catalyst of the present invention can be found out in sum, to the catalytic oxidation of ethanol in alkaline environment, there is excellent effect, if for having great practical significance and value in Direct Ethanol Fuel Cell, by the development of the Fashion of Future new forms of energy.
The above is only the citing of embodiments of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvement and modification, these improve and modification also should be considered as protection scope of the present invention.
Claims (4)
1. the preparation method of a PdNiW/C ternary alloy nano catalyst, described PdNiW/C ternary alloy nano catalyst is for activated centre with Pd, Ni and W, take active carbon as the PdNiW/C ternary alloy nano catalyst that carrier is formed, calculate in mass ratio, the i.e. quality of active carbon: Pd, the gross mass of Ni and W is 4:1, described activated centre calculates in molar ratio, Pd:Ni:W is wherein 7:2:1, described active carbon is XC-72 active carbon, it is characterized in that its preparation process specifically comprises the steps:
(1), by PdCl
2be dissolved in ethylene glycol solution, ultrasonic formation solution 1;
(2) NiCl is dripped in the solution 1, formed to step (1)
2, Na
2wO
4ethylene glycol solution, then use the ethylene glycol solution adjust ph to 9 of NaOH, in 80 DEG C reaction 1h after mixed liquor 2;
(3), in active carbon ethylene glycol is added, ultrasonic formation suspension 1;
Control to drip suspension 1 in the mixed liquor 2 that drop rate formed for 2-2.5ml/min in step (2), continue stirring reaction 30min, then add sodium citrate aqueous solution, ultrasonic 30min, then add NaBH
4the aqueous solution, at 50 DEG C, stirring reaction 3h obtains suspension 2;
The natrium citricum added and NaBH
4amount by its mol ratio relative to the total amount of Pd, Ni and W calculate, the molal quantity of namely total Pd, Ni and W: natrium citricum molal quantity: NaBH
4molal quantity=1:1:1;
(4), by the suspension 2 of step (3) gained be cooled to room temperature final vacuum suction filtration, the filter cake tap water of gained is washed till without chlorion in solution, and vacuum drying obtains PdNiW/C ternary alloy nano catalyst.
2. the preparation method of a kind of PdNiW/C ternary alloy nano catalyst as claimed in claim 1, it is characterized in that the amount of active carbon used and ethylene glycol in the suspension 1 described in step (3), in active carbon: ethylene glycol is that the ratio of 1mg:1.25ml calculates.
3. the preparation method of a kind of PdNiW/C ternary alloy nano catalyst as claimed in claim 2, is characterized in that the vacuum filtration controlled pressure described in step (4) is-0.1MPa.
4. the preparation method of a kind of PdNiW/C ternary alloy nano catalyst as claimed in claim 3, is characterized in that the process of vacuum drying control temperature described in step (4) is 90 DEG C.
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| US9761884B2 (en) | 2014-06-19 | 2017-09-12 | GM Global Technology Operations LLC | Synthesis of alloy nanoparticles as a stable core for core-shell electrocatalysts |
| JP6741545B2 (en) * | 2016-10-10 | 2020-08-19 | 田中貴金属工業株式会社 | Catalyst for polymer electrolyte fuel cell and method for producing the same |
| 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 |
| CN110858653A (en) * | 2018-08-22 | 2020-03-03 | 中国石油天然气股份有限公司 | Carbon-supported palladium-nickel binary alloy nano catalyst and preparation method and application thereof |
| CN111834642B (en) * | 2019-04-15 | 2021-12-17 | 武汉氢阳能源有限公司 | Organic matter electrocatalytic oxidation catalyst and preparation method and application thereof |
| CN112054222B (en) * | 2020-09-04 | 2021-12-28 | 西安交通大学 | Carbon-supported palladium nickel tantalum nitride nano-electrocatalyst for direct methanol fuel cell and preparation method thereof |
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| CN102203034A (en) * | 2008-08-27 | 2011-09-28 | 维仁特能源系统公司 | Synthesis of liquid fuels from biomass |
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