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1 Eletroni Supplementary Material (ESI) for Catalysis Siene & Tehnology. This journal is The Royal Soiety of Chemistry 2017 Eletroni Supplementary information Conversion of n-utane and produt seletivity was alulated from mole fration of produts in outflow as elow : Conversion of n utane (%) = ([C 4 H 10] in [C 4 H 10 ] out ) 100 [C 4 H 10 ] in (1) Conversion of oxidant (%) = ([oxidant] in [oxidant ] out ) 100 [oxidant] in (2) moles of the produt Seletivity (%) = total moles of the produt (3) 1. Mass and Heat Transfer Calulations for n-utane oxidation over Ni-Mo/Al 2 O 3 atalyst Mears Criterion for External Diffusion (Fogler, p841; Mears, 1971) n-utane ativation over oxygen: If ra ' Rn 0.15, then external mass transfer effets an e negleted. k C A r A ' = reation rate, kmol/kg-at s = 4.98 x 10-5 kmol-c 3 /kg-at. s n = reation order = 2 R = atalyst partile radius, m=3 x 10-5 m ρ = ulk density of atalyst ed, kg/m 3 =(1-ф) (ф= porosity or void fration of paked ed)= 1024 kg/m 3 ρ = solid atalyst density, kg/m 3 = 1.28 m/s C A = ulk gas onentration of A, kmol/m 3 = kmol/m 3
2 k = mass transfer oeffiient, m/s = 1.28 m/s ra ' Rn = 3.12 x 10-4 <0.15 {Mears for External Diffusion} k C A Similarly, for CO 2 = 2.85 x 10-4 and for N 2 O = 1.72 x Weisz-Prater Criterion for Internal Diffusion (Fogler, p839) If C WP r' A( os) D C e R As 2 1, then internal mass transfer effets an e negleted. -r A(os) = oserved reation rate, kmol/kg-at s = 5.05 x 10-5 kmol-c 3 /kg-at. s R = atalyst partile radius, m =3 x 10-5 m ρ = solid atalyst density, kg/m 3 = 3600 kg/m 3 D e = effetive gas-phase diffusivity, m 2 /s [Fogler, p815] D AB p = where D AB = gas-phase diffusivity m 2 /s; = pellet porosity; =onstrition fator; =tortuosity. p C As = gas onentration of A at the atalyst surfae, kmol-a/m 3 = kmol-c3/m 3 C WP r' A( os) D C e R As 2 = 4.9 x 10-4 < 1 {Weisz-Prater Criterion for Internal Diffusion} Similarly, for CO 2 = 4.07 x 10-4 and for N 2 O = 2.28 x Mears Criterion for Comined Interphase and Intrapartile Heat and Mass Transport (Mears, 1971) r' C A R D A e n n R E g T s E H r DeC A H r r' A R ; ; ; ; R T T h T g t r' A R k C A γ = Arrhenius numer; β = heat generation funtion;
3 λ = atalyst thermal ondutivity, W/m.K; χ = Damköhler numer for interphase heat transport ω = Damköhler numer for interphase mass transport r' C A A R D e 2 = 3.11 x10-5 < 3{Mears Criterion for Interphase and Intrapartile Heat and Mass Transport } Similarly, for CO 2 = 2.15 x 10-5 and for N 2 O = 1.72 x 10-5 Tale S1: The effet of metal oxide, support and promoter on the n-utane oxidative ativation Catalyst n-utane onversion Oxidant Temperature TOF (s -1 ) Referene (mol %) 7 % V 2 O 5 /SiO Air x 10-5 [1, 2] 17.5 % V 2 O 5 /Al 2 O Air x 10-5 [1, 2] 6 % V 2 O 5 /N 2 O Air x 10-5 [1, 2] 4 % V 2 O 5 /ZrO Air x 10-5 [1] 3 % V 2 O 5 /CeO Air x 10-5 [1] 5 % V 2 O 5 /TiO Air x 10-5 [1] 1 % V 2 O 5 / 5 % P 2 O 5 /TiO Air x 10-5 [1] 6 % WO 3 / 1 % V 2 O 5 /TiO Air x 10-5 [1] γ-bi 2 MoO Air+steam x 10-4 [3] β-bi 2 Mo 2 O Air+steam x 10-4 [3] BiMoZr x oxide 42.3 Air x 10-4 [4] BiMoFe x oxide 68.6 Air x 10-4 [5] ZrFe 2-x Al x O Air x 10-4 [6] ZnFe 2 O Air x 10-4 [3, 7] TiP 2 O 7 -M CO x 10-4 [8] TiP 2 O 7 -M CO x 10-4 [8] 1.2 % Cr 2.8 % 10.2 CO x 10-4 [9]
4 V/MCM % Cr 2.8 % V/ZSM % Cr 2.8 % V/ MCM % Cr 2.8 % V/ZSM- 5(Mesoporus) 8.3 CO x 10-4 [9] 7.2 CO x 10-4 [9] 6.1 CO x 10-5 [9] XPS analysis of fresh redued and reoxidised atalyst: Figure S1: X-ray photoeletron spetra (Mo 3d - S 2s region) of NiMo/Al 2 O 3 atalysts Redued and and reoxidised samples are inluded for omparison
5 4. Kinetis of redution and oxidation: The kinetis of redution and oxidation was alulated using Autohem 2920 Chemisorption analyser. A series of redution (TPR) and oxidation (TPO) experiments (as explained in Experimental setion) were done at different heating rates namely 2 C/min, 5 C/min, 7 C/min, 10 C/min, 14 C/min and 20 C/min. The data are plotted and the slope determined to alulate the rate, ativation energy for redution and oxidation [10]. Figure S2: First order kinetis of redution experiments of Ni-Mo/Al 2 O 3 atalyst
6 ln k /(TPR Peak temperature, K) Figure S3: Arrhenius relationship profile of redution (with H 2 ) of Ni-Mo/Al 2 O 3 atalyst -ln k /(TPO Peak temperature, K) Figure S4: Arrhenius relationship profile of oxidation (with O 2 ) of Ni-Mo/Al 2 O 3 atalyst
7 Ln K O2 CO2 N2O Linear (O2) Linear (CO2) Linear (N2O) 1/T ( x 10-3) Figure S5: Arrhenius relationship profile of n-utane ativation over different oxidants Referenes [1] I.E. Wahs, J.-M. Jehng, G. Deo, B.M. Wekhuysen, V.V. Guliants, J.B. Benziger, S. Sundaresan, Fundamental Studies of Butane Oxidation over Model-Supported Vanadium Oxide Catalysts: Moleular Struture-Reativity Relationships, J. Catal., 170 (1997) [2] I.E. Wahs, J.-M. Jehng, G. Deo, B.M. Wekhuysen, V.V. Guliants, J.B. Benziger, In situ Raman spetrosopy studies of ulk and surfae metal oxide phases during oxidation reations, Catal. Today, 32 (1996) [3] J.C. Jung, H. Kim, A.S. Choi, Y.-M. Chung, T.J. Kim, S.J. Lee, S.-H. Oh, I.K. Song, Effet of ph in the preparation of γ-bi2moo6 for oxidative dehydrogenation of n-utene to 1,3-utadiene: Correlation etween atalyti performane and oxygen moility of γ-bi2moo6, Catal. Commun., 8 (2007) [4] R. Grasselli, Fundamental Priniples of Seletive Heterogeneous Oxidation Catalysis, Top. Catal., 21 (2002) [5] J.-H. Park, C.-H. Shin, Oxidative dehydrogenation of utenes to utadiene over Bi Fe Me(Me = Ni, Co, Zn, Mn and Cu) Mo oxide atalysts, J Ind. Eng. Chem., 21 (2015) [6] J.A. Toledo, P. Bosh, M.A. Valenzuela, A. Montoya, N. Nava, Oxidative dehydrogenation of 1- utene over ZnAl ferrites, J. Mol. Catal. A: Chem., 125 (1997) [7] Y.-M. Chung, Y.-T. Kwon, T.J. Kim, S.J. Lee, S.-H. Oh, Prevention of Catalyst Deativation in the Oxidative Dehydrogenation of n-butene to 1,3-Butadiene over Zn-Ferrite Catalysts, Catal. Lett., 131 (2009) [8] I.-C. Maru, I. Sandulesu, J.-M.M. Millet, Oxidehydrogenation of n-utane over tetravalent metal phosphates ased atalysts, Appl. Catal., A,, 227 (2002) [9] B.R. Jermy, B.P. Ajayi, B.A. Aussaud, S. Asaoka, S. Al-Khattaf, Oxidative dehydrogenation of n- utane to utadiene over Bi Ni O/γ-alumina atalyst, J. Mol. Catal. A: Chem., 400 (2015)
8 [10] A. Gervasini, Temperature Programmed Redution/Oxidation (TPR/TPO) Methods, in: A. Auroux (Ed.) Calorimetry and Thermal Methods in Catalysis, Springer Berlin Heidelerg, Berlin, Heidelerg, 2013, pp
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