Propylene: key building block for the production of important petrochemicals

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1 Propylene production from 11-butene and ethylene catalytic cracking: Study of the performance of HZSMHZSM-5 zeolites and silicoaluminophosphates SAPO--34 and SAPOSAPO SAPO-18 E. Epelde Epelde*, *, A.G. Gayubo Gayubo,, M. Gamero, A.T. Aguayo, J. Bilbao Departamento de Ingeniería Química, Universidad del País Vasco, Apartado 644, 488 Bilbao, Spain

2 Propylene: key building block for the production of important petrochemicals RESULTS CONCLUSIONS C-C double bond Adjacent methyl group J.S. Plotkin,Catalysis Today,16 (25) Propylene worlwide demand has been increasing at an annual average of 5.7% and by year 215, demand will grow to 15 million tonnes T. Mokrani and M. Scurrell Scurrell, Catalysis Reviews,, 51 (29),1

3 CONCLUSIONS RESULTS Sustainability 18% Fluid Catalytic Cracking Steam Cracking Crude Oil Natural Gas Coal Biomass Wastes Refinery Coupled Methanol Hydrocarbons Cracking 7% Methane Oxidative Coupling Paraffins Oxidative Dehydrogenation 2 % On purpose technologies (paraffin dehydrogenation, metathesis) Steam Reforming Gasification Syngas Methanol Dimethil Ether Methanol To Olefins OLEFINS Propylene Intensification 1% Fermentation Bio-Ethanol Bio-Oil PROPYLENE Pyrolisis CO 2 D. Mier et al. Chemical Engineering Journal, 16 (21)

4 Catalytic Processes and Waste Valorization SPLITTER Propylene RESULTS MeOH MTO Paraffins Olefins (C 2=, C 4= ) PROPYLENE INTENSIFICATION Propylene CONCLUSIONS Paraffins

5 RESULTS C 2 -C 4 olefin interconversion Acid catalysts Mechanism of oligomerization-cracking Shape selectivity of the catalysts significant role in propylene yield and selectivity New catalyst development for C 2 -C 4 olefin catalytic cracking Modification of HZSM-5 by metal incorporation (P, P-La, Ni, K ) by dealumination methods (NaOH, steaming ) Silicoaluminophosphates (SAPO-34, SAPO-18) CONCLUSIONS Aim of this work: Study the role of the properties of the catalyst (acidity and shape selectivity) in the intensification fo propylene production from 1-butene and ethylene transformation Conversion-propylene yield selectivity-stability X. Zhu, S. Liu, Y. Song, L. Xu, Catal. Lett., 13 (25) G. Zhao, J. Teng, Z. Xie, W. Jin, W. Jang, Q. Chen, Y. Tang, J. Catal., 248 (27) A.T. Aguayo, D. Mier, A.G. Gayubo, M. Gamero, J. Bilbao,Ind. Eng. Chem. Res., 49 (21)

6 CONCLUSIONS RESULTS Catalyst preparation Zeolite HZSM-5 or SAPOs (25 %) Wet extrusion, dry, calcination (55 ºC, 2h) Bentonite Alumina (3 %) (45 %) HZ-3 (SiO 2 /Al 2 O 3 =3) HZ-8 (SiO 2 /Al 2 O 3 =8) HZ-28 (SiO 2 /Al 2 O 3 =28) SAPO-18 SAPO-34 Confer suitable size and mechanical resistance to the catalytic particles in fixed and fluidized bed reactors A matrix with meso- and macroporous structure is formed reducing deactivation by coke increasing hydrothermal stability A.T. Aguayo, A.G. Gayubo, R. Vivanco, M. Olazar, J. Bilbao, Appl. Catal. A.: Gen. 283 (25) 197

7 CONCLUSIONS RESULTS Catalyst characterization N 2 adsorption-desorption (77 K) Active phase S BET (m 2 /g) V mesopore (cm 3 /g) V micropore (cm 3 /g) HZ HZ HZ SAPO SAPO Catalyst S BET (m 2 /g) V mesopore (cm 3 /g) V micropore (cm 3 /g) HZ HZ HZ SAPO SAPO ) V ads (cm 3 g Catalyst (agglomerated) Active phase P/P

8 CONCLUSIONS RESULTS Catalyst characterization DSC (15 ºC)- TPD of NH 3 (up to 55 ºC) Active Total acidity T peak(ºc) in the TPD phase (mmol NH 3 g -1 ) 1st 2nd peak peak HZ HZ HZ SAPO SAPO TPD NH 3 (mmol NH3 3/s g catalyst ) HZ-3 HZ T (ºC) These acid properties remain after agglomeration HZ-28

9 Reactor setup Fixed bed reactor Microactivity (316-L SS,D i = 9 mm) Feed: 35 cm 3 min - 1 of 1-butene or ethylene diluted (1%) in He 5 ºC Mass of catalyst:.55 g t= 5 h RESULTS CONCLUSIONS MS5A PPQ Alumina OV1

10 CONCLUSIONS RESULTS Evaluation criteria used for catalytic performance Conversion (X): F F X = F Yield of i lump: Y i F i = F Selectivity of i lump: Molar flowrates: F = reactant in the feed F= reactant in the outlet stream F i = i-lump in the product stream F Y i (% %) CH4 C2H4 C3H6 C2-C3 C4H1 C5+ BTX X S = i i F -F. Terms expressed as CH 2 equivalent units, corresponding to zero time on stream t (min) HZ-3 catalyst 5 º C, W/F A =24.5 g catalyst h (mol CH 2 ) -1 X

11 CONCLUSIONS RESULTS Transformation of 1-butene Effect of SiO 2 /Al 2 O 3 in HZM-5 zeolites Y S i,x i (%) CH4 C2H4 C3H6 C2-C3 C4H1X C5+ BTX YC2H4 YC3H SiO SiO 2 /Al 2 3 ratio 2 /Al 2 O 3 ratio HZ-28 SiO 2 /Al 2 O 3 ratio Butene conversion C 2 H 4 and C 3 H 6 yield C 2 H 4, C 3 H 6 and C 5+ selectivities Hydrogen transfer reactions (catalyzed by strong acid sites) C 2 -C 4 and BTX selectivities

12 X, Y i (%) Transformation of 1-butene Shape selectivity catalysts HZ-28 SAPO-18 SAPO-34 S i (%) HZ-28 SAPO-18 SAPO-34 CONCLUSIONS RESULTS 2 X YC3H6 YC2H4 2 C2H4 C3H6 C2-C3 C4H1 C5+ BTX Severity of shape selectivity is higher for SAPOs (steric limitations) SC 3 H 6 SAPO-34 is more active than SAPO-18 HIGHER TOTAL ACIDITY AND ACID STRENGTH OF SAPO-34

13 CONCLUSIONS RESULTS X Transformation of 1-butene Deactivation by coke SAPO-34 (4.7 wt%)> SAPO-18 (3.3 wt%) >HZ-28 (2.7 wt%) HZ-28 SAPO-18 SAPO t (min) cat) -1 Mass variation µg (s g c HZ-28 SAPO-34 SAPO-18 (537 ºC) t (min) (569 ºC) (563 ºC) T (ºC)

14 CONCLUSIONS RESULTS Transformation of ethylene Effect of SiO 2 /Al 2 O 3 in HZM-5 zeolites Y i,x (% %) X 4 YC4H8 YC3H SiO 2 /Al 2 O 3 ratio S i (%) CH4 C3H6 C4H8 C2-C3 C4H1 C5+ BTX SiO 2 /Al 2 O 3 ratio Ethylene conversion requires low values of SiO 2 /Al 2 O 3 ratio HZ-28 SC 3 H 6, YC 3 H 6

15 X, Y i (%) Transformation of ethylene Shape selectivity catalysts HZ-28 SAPO-18 SAPO-34 S i (% %) HZ-28 SAPO-18 SAPO-34 CONCLUSIONS RESULTS X YC3H6 YC4H8 C3H6 C4H8 C2-C3 C4H1 C5+ SAPO-34 and SAPO-18 higher ethylene conversion and propylene yield SAPO-18 suitable for the Steric restrictions in selective SAPOs production SC 3 H 6 of Deactivation rate: SAPO-34>>SAPO-18 propylene BTX

16 CONCLUSIONS RESULTS CONCLUSIONS The moderation of total acidity and acid strength is an appropriate way to modify HZSM-5 zeolites in order to enhance propylene production SAPO-18 shows higher propylene selectivities using both feeds, although the deactivation by coke is slightly faster than for HZ- 28 catalyst The use of SAPO-34 is conditioned by the fast deactivation by coke Operating conditions may have a great influence; the study should be extended to higher temperatures (up to 55 ºC) and feed composed of ethylene/propylene mixtures

17 ACKNOWLEDGMENTS This work was carried out with the financial support of the Ministry of Science and Innovation of the Spanish Government (Project CTQ ) and of the Department of Education Universities and Research of the Basque Government (Project GIC7/24-IT-22-7). E. Epelde is grateful for the Ph.D. grant from the Department of Education, University and Research of the Basque country (BFI8.122).

18 THANK YOU

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