Electrochemical Promotion of CO 2 hydrogenation on Ru deposited on YSZ (O 2- ), β"-al 2 O 3 (Na + ) and BZY-NiO (H + ) conductors
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1 Laboratory of Chemical & Electrochemical Processes Department of Chemical Engineering University of Patras, Greece Electrochemical Promotion of CO 2 hydrogenation on Ru deposited on YSZ (O 2- ), β"-al 2 O 3 (Na + ) and BZY-NiO (H + ) conductors 10 th European Symposium on Electrochemical Engineering D. Theleritis, M. Makri, I. Kalaitzidou A. Katsaounis and C. G. Vayenas
2 Outline CO 2 Hydrogenation Introduction Electrochemical Promotion of Catalysis preparation and characterization of the catalysts Experimental Procedure Experimental setup - Reactor Electrochemical Promotion of CO 2 Hydrogenation Ru/BZY, Ru/YSZ, Ru/β -Al 2 O 3 electrochemical cell Comparative Results Discussion - Conclusions
3 CO 2 Hydrogenation
4 Electrochemical Promotion of Catalysis EPOC M. Stoukides and C.G. Vayenas, J. Catal., 70 (1981) 137.
5 Electrochemical Promotion of Catalysis EPOC 0< 0>
6 Electrochemical Promotion of Catalysis EPOC C 2 H 4 oxidation on Pt Faradaic Efficiency Δr r r 0 r, r 0 rate of production / consumption(g-mol/s) I/nF under closed and open (Ι=0) circuit ion transfer rate Rate Enhancement Ratio ǀ Λ ǀ > 1 Non Faradaic Electrochemical Modification of Catalytic Activity (ΝΕMCA) Electrochemical Activation of Catalysis: Promotion, Electrochemical Promotion and Metal-Support Interactions C.G. Vayenas, S. Bebelis, C. Pliangos, S. Brosda, D. Tsiplakides, Kluwer Academic/Plenum Publishers (2001).
7 r / mol CO 2 /s U WR / mv Electrochemical Promotion of Catalysis EPOC CO oxidation with labeled oxygen 18 O 2 on Pt r / mol CO2/s I= +1 =1.3 =11.4 o.c. I= -1 =0.8 =9.6 o.c. 16O mol O 2 /s Faradaic Efficiency I/2F r C 16 O 18 O r C 16 O C P=8x10-6 mbar 1% 18 O % C 16 O time / s C 16 O 18 O C 16 O 2 CO + 18 O C 16 O 18 O (mass 46) CO + 16 O C 16 O 16 O (mass 44) 0 open circuit catalytic reaction time / s A. Katsaounis, Z. Nikopoulou, X.E. Verykios, C.G. Vayenas, J. Catal. 222 (2004) 192 and J. Catalysis 226 (2004) 197.
8 Preparation of electrochemical Cells Catalyst (Ru) Working electrode Wet impregnation of RuCl 3 solution (150mM) Calcination at 650 o C for 1 h 2 mm Solid electrolyte 18 mm Reference electrode Au Counter electrode Au Deposition with Au paste (Metalor A1118) Calcination at 650 o C for 1 h Electrochemical Activation of Catalysis: Promotion, Electrochemical Promotion and Metal-Support Interactions C.G. Vayenas, S. Bebelis, C. Pliangos, S. Brosda, D. Tsiplakides, Kluwer Academic/Plenum Publishers, (2001).
9 Characterization of the catalyst SEM Ru/BZY(H + ) fresh catalyst used catalyst Uniform Porous nm Uniform Porous nm I. Kalaitzidou, A. Katsaounis, T. Norby, C.G. Vayenas, J. Catal. (2015), submitted.
10 Characterization of the catalyst XRD Ru/BZY(H + ) Scherrer equation 20.6 ± 2 nm I. Kalaitzidou, A. Katsaounis, T. Norby, C.G. Vayenas, J. Catal. (2015), submitted.
11 Experimental setup 1. Gas bottles 2. Flow meters 3. Three way valves 4. Reactor 5. Furnace 6. Temperature controller 7. Voltage transformer 8. Galvanostat/ Potentiostat 9. Mass Spectrometer 10. IR analyzer 11. Gas chromatographer 12. Bubble meter
12 Electrochemical reactor Single chamber BaZr 0.85 Y 0.15 O w% NiO I. Kalaitzidou, A. Katsaounis, T. Norby, C.G. Vayenas, J. Catal. (2015), submitted Electrochemical Activation of Catalysis: Promotion, Electrochemical Promotion and Metal-Support Interactions C.G. Vayenas, S. Bebelis, C. Pliangos, S. Brosda, D. Tsiplakides, Kluwer Academic/Plenum Publishers, (2001).
13 Preparation of electrochemical cells using BZY NorECs Norwegian Electro Ceramics AS calcination of the nominal amounts of BaCO 3, 8YSZ (TOSOH) and 1 wt % NiO at 1500 o C for 12 hr BaZr 0.8 5Y 0.15 O 3 T.S. Bjørheim, A. Kuwabara, T. Norby, J. Phys. Chem. C 117 (2013) S. Erdal, C. Kongshaug, T.S. Bjørheim, N. Jalarvo, R. Haugsrud, T. Norby, J. Phys. Chem. C, 114 (2010) T. Norby, Solid State Ionics 125 (1999) 1-11.
14 Effect of potential on r CH4 and r CO Ru/BZY(H + ) Proton removal Proton supply I. Kalaitzidou, A. Katsaounis, T. Norby, C.G. Vayenas, J. Catal. (2015), submitted.
15 Effect of potential on r CH4, r CO, Λ, ρ Ru/BZY(H + ) I. Kalaitzidou, A. Katsaounis, T. Norby, C.G. Vayenas, J. Catal. (2015), submitted.
16 Effect of potential on selectivity Ru/BZY(H + ) I. Kalaitzidou, A. Katsaounis, T. Norby, C.G. Vayenas, J. Catal. (2015), submitted.
17 Mechanistic model Ru/BZY(H + ) open circuit + e - - H + U > 0 I. Kalaitzidou, A. Katsaounis, T. Norby, C.G. Vayenas, J. Catal. (2015) submitted. P. Panagiotopoulou, D.I. Kontarides, X.E. Verykios, Catalysis Today 181 (2012)
18 Effect of potential on r CH4 and r CO Ru/YSZ(O 2- ) Positive potential application CH 4 CO CO 2 D. Theleritis, S. Souentie, A. Siokou, A. Katsaounis, C.G. Vayenas, ACS Catalysis 2 (2012) 770.
19 Effect of potential on r CH4 and r CO Ru/β -Al 2 O 3 β -Al 2 O 3 (Na + ) β -Al 2 O 3 (K + ) D. Theleritis, M. Makri, S. Souentie, A. Caravaca, A. Katsaounis, C.G. Vayenas, ChemElectroChem 1 (2014) 254. M. Makri, A. Katsaounis, C.G. Vayenas (2015), in preparation.
20 Rules of Electrochemical & Chemical Promotion RULES OF PROMOTION IN TERMS OF REACTION ORDERS (LEFT) OR IN TERMS OF ADSORPTION COEFFICIENTS (RIGHT) S. Brosda, C.G. Vayenas and J. Wei, Appl. Catal. B 68 (2006) 109.
21 Kinetic behaviour - predictions based on EPOC rules reaction (r CH4 and r CO ) order with respect to the electron donor, H 2 CH 4 CO BZY β - Al 2 O 3 YSZ D. Theleritis, M. Makri, S. Souentie, A. Caravaca, A. Katsaounis, C.G. Vayenas, ChemElectroChem 1 (2014) 254. M. Makri, A. Katsaounis, C.G. Vayenas, (2015), in preparation.
22 Kinetic behaviour - predictions based on EPOC rules reaction (r CH4 and r CO ) order with respect to the electron acceptor, CO 2 CH 4 CO BZY β - Al 2 O 3 YSZ D. Theleritis, M. Makri, S. Souentie, A. Caravaca, A. Katsaounis, C.G. Vayenas, ChemElectroChem 1 (2014) 254. M. Makri, A. Katsaounis, C.G. Vayenas, (2015), in preparation.
23 Kinetic behaviour - predictions based on EPOC rules reaction (r CH4 and r CO ) order with respect to the electron acceptor, CO 2 CH 4 CO BZY β - Al 2 O 3 YSZ D. Theleritis, M. Makri, S. Souentie, A. Caravaca, A. Katsaounis, C.G. Vayenas, ChemElectroChem 1 (2014) 254. M. Makri, A. Katsaounis, C.G. Vayenas, (2015), in preparation.
24 Kinetic behaviour - predictions based on EPOC rules Ru/YSZ Ru/BZY D. Theleritis, M. Makri, S. Souentie, A. Caravaca, A. Katsaounis, C.G. Vayenas, ChemElectroChem 1 (2014) 254. M. Makri, A. Katsaounis, C.G. Vayenas, (2015), in preparation.
25 Conclusions Electrochemical promotion of CO 2 hydrogenation was explored on Ru supported catalysts using electronegative and electropositive promoters. Methane and carbon monoxide were the only measurable products under the investigated conditions. In all cases methane production followed electrophobic behaviour while CO formation followed electrophilic one. Rate enhancement ratios, ρ, up to 5 and Faradaic efficiency values, Λ, up to 250 were observed.
26 Acknowledgements Work supported by the ARISTEIA Action of the Operational programme of education and lifelong learning (ELECTROFUELS/467)which is cofunded by the European Social Fund (ESF) and National Resources (ESPA ).
27 Laboratory of Chemical & Electrochemical Processes Department of Chemical Engineering University of Patras, Greece Dimitris Theleritis Ioanna Kalaitzidou Eftychia Martino Alexandros Katsaounis Marialena Makri Dimitris Grigoriou Alexandros Similides
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