Expérimentation haut-débit Science ou loterie? David FARRUSSENG
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1 Expérimentation haut-débit Science ou loterie? David FARRUSSENG
2 10 years of HT Catalysis Pharma Fine Chemicals Polymers Chemicals Refining Green chemistry 1970s 1980s 1990s Symyx hte Avantium Novodynamics Thales UOP/Sintef Dow + Exxon 370 M$ BASF The Catalytic Group Resources, JJ Murphy, Combicat2002 Europe, Lisbon, April 11-12, /20
3 Why HT experimentations? To shrink time-to-market To increase discovery rates Discovery Development Pilot plant Market Yield HTE 15 years Time variable 1 variable 2 3/20
4 Discovery of NH 3 synthesis catalyst in catalysts and experiments within 5 years Systematic investigation of the periodic table Reconstitution of A. Mittash laboratory in BASF in 1905 Highly complex formulation (ICI 35-4) Fe 3 O 4, 0.8% K 2 O, 2% CaO, 0.3% MgO, 2.5%Al 2 O 3, 0.4%SiO 2, traces of TiO 2, ZrO 2, V 2 O 5 Rapid dissemination of this empirical oriented approach 4/20
5 Rational approach temperature, solvent, composition, pressure, composition activity Design Model Make % Pd Test 5/20
6 HT & multivariate approach temperature, solvent, composition, 0.1 wt% 2.1 wt% 1 wt% 5 wt% Au Cu Pt Design Mo Nb V Model Make CeO 2 TiO 2 ZrO C 250 C 300 C Test 6/20
7 The combinatorial approach Primary Screening Hit discovery Secondary Screening Lead optimization Cocatalyst Pilot Cocatalyst 2 Ce Cu Mn Zn Ti Fe Co Sn Ir Ru Rh Zr Sb Ni Yb Eu Cr Pb Ce Cu Mn Zn Ti Fe Co Sn Ir Ru Rh Zr Sb Ni Yb Eu Cr Cocatalyst 2 7/20
8 The evolutionary approach Combining discovery & optimization Design Exploration & exploitation Test Synthesis Population Selection Mating Cross-over Mutation Testing Synthesis G. Grubert et al Appl. Catal. A-Gen., 2006, 306, 17 8/20
9 How can HTE generate Knowledge? Quantification of the variable effects on performances Maximising knowledge gain while minimizing trials DoE : Selox case study M 1 M 2 M 3 M 4 M 5 O1 O2 O3 O4 O5 O6 D1 D2 D3 S1 S2 S3 S4 S Li Cs Ca Al Ce Zr Zn C dopants supports 3 alkalins 5 supports 6 oxides 10 metalic binaries Cr Co Mn La Sm Mo metal oxides Pt-Pd Pt-Ru Pd-Ru Pt-Au Pd-Au Ru-Au Pt-Rh Pd-Rh Ru-Rh Au-Rh a b noble metals /20
10 Issues of library design in Catalysis FAQs Which is the best algorithm? How reliable is the methodology? How many experiments shall be performed to solve my problem? How to handle experimental errors? How to get clear information although all parameters are varied? What is the most relevant 101 th experiments to perform? F. Clerc et all Review of Scientifict Instrument, 2005, 76, D. Farrusseng et all, Appl. Surf. Sci., 2007, 254, /20
11 Success stories D. Farrusseng, Surface Sciences Reports, 2008, in press. IRCELYON: exhaust car applications HT discoveries -> pilot tests Microkinetic investigations DeNOx Soot combustion NOx conversion % CataRef IRCELYON T=50 C No. of obs T=80 C PhD thesis: P. Gravegeat Temperature / C Category Boundary / C PhD thesis: B. Bassou 11/20
12 Rational selection of samples How? samples 5-10 samples Bank of catalyst Uncompleted characterization Inconsistent methods Missing data Scale 2 How to quantify diversity in a library of diverse catalysts? Scale 1 12/20
13 Hydrogenation properties of bifunctional catalysts Hydrogenation of o-xylene Activity: highly sensitive to metallic composition Catalysts Hydrogenation rate (10-3 mol.h-1.g-1) Pt H 2 Pt 0.5 Pd Pt 0.5 Ge Pd 4 cis-dmch trans-dmch Guillon et al. Cat. Today 65(2001) Selectivity : sensitive to electrophilic features Selectivity correlated to calorific capacity of cond. e Electronic density of Fermi level D(εF) 13/20 Del Angel, G., et al., New Journal of Chemistry, (8-9): p
14 «Semi-empirical» model Langmuir based model r i = H 2 dissociate adsorption Competitive adsorption Fast product desorption A e i Ei RT Where i = cis or trans K ox p ox ( K p ) ( + K p + K p ) 2 1 ox ox H H H 2 H 2 2 n i 2 Conversion / - Reference catalyst 0.3%Pd/Al 2 O 3 16% 12% 8% 4% 0% p H Température / C 10 parameters 8 «physico-chemical» (Ea, A, H ads, S ads ) 2 semi-empirical (n cis, n trans ) G. Morra et al Cata. Today, 2008, in press 14/20
15 Hydrogenation profile visulalization Pd Ni Pt Rh 15/20
16 Catalyst mapping 2D activity plot 2D selectivity plot PC2 1 0 PC Factor 1 PC1 Distance = diversity quantification High effects of doping and supports Rational selection Factor 1 PC1 Ni Pd Pt Rh δ-al 2 O 3 αθ-al 2 O 3 16/20
17 Conclusions To Maximize information by mastering sample diversity To capture information To generate knowledge Virtual screening Design Statistics Kinetic Modeling Test Synthesis C. Klanner et al Angew. Chem.-Int. Edit., 2004, 43, 5347 L. Baumes, et al QSAR Comb. Sci., 2004, 23, 767. S. Pereira et al QSAR Comb. Sci., 2005, 24, 45 G. Morra et al Chem. Eng. J., 2008, 379 Qualitative information 17/20
18 Conclusions Concept development Diversity management for material optimization Knowledge discovery by modeling (kinetic & QSAR) Tool development SWITCH-16 for HT transient characterization and screening OptiCat, e-library design platform New paradigm in HT Catalysis? INTEGRATION OF: Molecular modeling (DFT,QM, MM ) Quantitative screening & characterization Kinetic modeling Statistical modeling (QSAR) AMTEC GmbH 18/20
19 Perspectives Screening unexplored domains MOF : New metal-organic molecular sieves ter-bucl OH U. Ravon et al NJC, 2008, in press D. Farrusseng, Handbook of Catalyst Design, Wiley, 2008, in press 19/20
20 THANKS F. Clerc, M. Lengliz, L. Baumes, D. Zediar, E. Burello Y. Vauthey, D. Tibiletti, C. Hoffmann, C. Klanner, U. Ravon,. A. Desmartin- Chomel, G. Morra, P. Gravegeat, B. Bassou, E. Iojoiu, S. Pereira Dr.R. Rocomatalala Dr. G. Rothenberg Prof. F. Schüth Dr. van der Waal Dr. S. Morin, Dr. N. Bats Dr. C. Mirodatos Engineering Team 20/20
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