Non-oxidative methane aromatization in a catalytic membrane reactor

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1 Non-oxidative methane aromatization in a catalytic membrane reactor Olivier RIVAL, Bernard GRANDJEAN, Abdelhamid SAYARI, Faïçal LARACHI Department of Chemical Engineering and CERPIC Université Laval, Ste-Foy, Québec and Christophe GUY Department of Chemical Engineering, Ecole Polytechnique de Montreal Environmentally Friendly Gas Technologies 2 nd Canadian-Korean joint WORKSHOP Feb. 28 to Mar. 2, 2000 Montreal / Boucherville / Varennes / Bells Corners Canada 1 Production of H 2 : growing interests Demand in ecofriendly fuels and processes Fuel-cell technology development F ideal energy carrier 2

2 Major source of H 2 Natural gas - Abundance of methane reserves - Canada is the 3 rd world largest producer the 2 nd world exporter F Economic significance of CH 4 conversion into H 2 3 H 2 production from CH 4 Main industrial processes : Gas steam reforming Catalytic methane decomposition Methane pyrolysis Disadvantages : energy intensive and costly low H 2 purity greenhouse gas emissions F non-oxidative process 4

3 Non-oxidative methane conversion into H 2 and hydrocarbons x CH 4 y H 2 + z C n H m C n H m = alkanes, alcenes (C 2 to C 8 ) 1- or 2- step processes : Garnier et al.,1997, Smith et al.,1995, Cheikhi et al.,1994 C n H m = aromatics (benzene, toluene,...) 1- or 2-step processes: Iglesia et al., 1999, Shu et al., 1999, Weckhuysen et al.,1998 F low yield, complexity 5 Aromatization: Equilibrium-limited conversion 6 CH 4 9 H 2 + C 6 H 6 CH4 CONVERSION % mol TEMPERATURE (K) F Limitation: 11.3% at 973K 6

4 Shift of the thermodynamic equilibrium using permselective membrane k 1 6 CH 4 9 H 2 + C 6 H 6 k 2 Permselective membrane H 2 withdrawal F lower temperature, higher yield separation in situ 7 Objective of this study Investigation of methane aromatization in a catalytic membrane reactor 8

5 Experimental set-up Membrane reactor REB Research (with Palladium-Coated Tantalum and/or Niobium membrane GC permselective Membrane CH 4, Ar, H 2, C 6 H 6 (reaction side) CH 4, Ar (feed in) H 2 (permeation side) under vacuum (10-2 Pa) T Catalyst fixed bed Ru~Mo-HZSM5 prepared by wet impregnation Furnace 9 Test on H 2 permeation through REB- Research Membrane H 2 permeation rate (mlstp min -1 ) Sievert s type permeation equation J = J o e (-Ep / RT) (P H2,r -P H2,p ) K 599 K 686 K 870 K J o = 10-5 m.s -1.Pa - E p = 18 kj.mol P reaction - P permeation (Pa )

6 Test on catalytic activity without hydrogen permeation Formation of molybden carbides which are the actives species for aromatization ) Catalyst is 100% selective in benzene 2) Catalyst activity: complex pattern CH4 CONVERSION TO C6H6 [CH4]o=100% FCH4 o =12,2mL.mIn -1 T=600C) CH4 to C6H6 ( %mol) quasi steady state reactivity Time (min) methane adsorption and decomposition and catalyst reduction and slight occurrence of catalyst deactivation 11 Residence time effect on methane conversion (without hydrogen permeation) CH 4 conversion into C 6 H 6 ( % mol) 3 2,5 2 1,5 1 0,5 Experimental Conditions No permeation P reaction side = 101 kpa Temperature = 873K CH4 feed conc. = 100% GHSV = 400 h-1 GHSV = 710 h-1 GHSV = 1100 h TIME (min) F still under kinetics control 12

7 Effect of hydrogen permeation on conversion CH 4 conversion into C 6 H 6 ( % mol) ) hydrogen permeation increases conversion No permeation With permeation after 360min on stream Time on stream (min) 2)..but it promotes coke-laydown catalyst deactivation T = 873K [CH4]o = 100% GHSV = 710h-1 13 Results on CH 4 conversion: H 2 withdrawal (permeation) Temperature K CH 4 feed dilution % mol G.H.S. V. h -1 CH 4 conversion b,c % mol Thermodynamic CH 4 conversion % mol No Yes a No No Yes a No Yes a No No No a = P TOTAL permeation = 0.2 Pa b = calculated on a benzene basis c without permeation, quasi steady state conversion is reported with permeation, initial conversion is reported 14

8 Permeation effect on methane conversion CH 4 conversion into C 6 H 6 ( % mol) 6,0 5,0 4,0 3,0 2,0 1,0 Experimental Conditions P permeation side = 0,2 Pa P reaction side = 101 kpa G.H.S.V. = h -1 CH4 feed conc. = 100% x 1.8 Thermodynamic equilibrium Permeation No permeation 0,36 0,2 0, TEMPERATURE (K) 5,8 2,5 x Literature comparison Best yield in C 6 H 6 at 873K: 2.6 %mol (G.H.S.V.= 50h -1, Pt-HZSM-5, Marczewski et al., 1994) Permeation effect : Conversion of propane into aromatics is increased by a factor 2 in a membrane reactor (Uemiya et al., 1990) 16

9 Membrane Reactor Modelling: Schematic of the membrane reactor (plug-flow) Reaction side H F i,r Fi,r + F i,r Permeation side F i,p F i,p + F i,p Membrane H F i,r F i,r + F i,r Shell Simplified reaction rate r CH4 = k 1 P CH4 R.T α - k 2 P C6 H 6 R.T β P H2,r R.T γ 17 Membrane Reactor Modelling: CH 4 balance: Permeation rate: d F H2,p = J da H 2 balance: d X CH4 r CH4 = d W F CH4 J = J o e (-Ep / RT) (P H2,r -P H2,p ) P H2,r = P t,r 3 /2 X CH4 F CH4 - F H2,p (1+ 2 / 3 ) X CH4 F CH4 + F o Ar - F H 2,p Fitting of kinetic parameters using Powell algorithm: α = 0.41 β = 0.41 γ = 0.31 k 1 = k 2 =

10 Modelling results (at 873 K) EXPERIMENTAL or equilibrium CH 4 conversion ( % mol) 0,10 0,09 0,08 0,07 0,06 0,05 0,04 0,03 0,02 0,01 Experimental Conditions: P permeation side = 0,2 and 101 kpa P reaction side = 101 kpa CH4 feed conc. = % Temperature = 873 K G.H.S.V. = h -1 Active reactor lentgh = m E: Equilibrium conversion simulation with an hypothetical 1m-length reactor 0,00 0 0,01 0,02 0,03 0,04 0,05 0,06 0,07 0,08 0,09 0,1 E E E PREDICTED CH 4 conversion ( % mol) 19 Conclusions Ru~Mo-HZSM5 catalyst was prepared Methane aromatization with 100% benzene selectivity was observed REB-Research membrane reactor has been tested: Hydrogen permeation: J improves the conversion rate (by a factor 2) at 600 o C, conversion of 5.8 % vs 2.5% without permeation L contributes to catalyst deactivation Membrane reactor model has been proposed and validated Future work Enhancement of catalyst performances: Æ X CH4, coking, Æ stability adding small amounts of CO, CO 2 (Ichikawa et al.,1999) 20

11 Boudouart: CO [C] active + CO 2 carbide species formation (promoting effect) [C] actif + x / 2 H 2 CH x «Decokefaction» and regeneration (stabilizing effect) [C] inert + CO 2 CO (coke) ex: {+1.8% CO during 100h} 2x 4% = 8% conv. of CH 4 with a selectivity in C 6 H 6 alm. cste (# 67%) (Ichikawa et al., 1999) 21

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