Chemical Looping Reforming with Packed Bed Technology: Experimental Study and Modelling

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1 Chemical Looping Reforming with Packed Bed Technology: Experimental Study and Modelling V. Spallina, B. Marinello, M.C. Romano, F. Gallucci, M. van Sint Annaland

2 OUTLINE Motivation of the study Description of the concept Experimental study Conclusions Future works 2

3 Motivation of the study Chemical Looping Reforming has been studied only using interconnected Circulating Fluidized Beds but H 2 production (as well as CH 3 OH) is more convenient (techno-economic) at high pressure Packed Bed Reactor Fuel-to-chemicals conversion is less demanding in terms of heat management than fuel-to-heat: the overall heat of reaction is lower when compared to fuel combustion CLR vs CLC O 2 (from ASU) and H 2 O (from steam turbine extraction) are not for free auto-thermal reforming using oxygen carrier CCUS applied to chemical industry CO 2 capture convenient without subsides (e.g. carbon tax) Exploiting chemical looping technology in other industrially relevant processes chemical looping convenient without CO 2 capture policies 3

4 OXIDATION REDUCTION REFORMING the main concept Me (i.e. Ni) N 2 CO 2 +H 2 O Reformed syngas MeO (i.e. NiO) Air PSA offgas CH 4 (+H 2 O) 4

5 OXIDATION REDUCTION REFORMING the concept for H 2 production η ref = 75.4% HR= Gcal/kNm 3 H2 EE= kwh/kg H2 gas turbine H 2 Air N 2 Reformate (39.4%H 2, 29%H 2 O, 19.2%, CO, 11% CO 2, 1.1% CH 4 ) CO 2 + H 2 O steam HT-WGS PSA SH steam at (500 C, 100 bar) Export steam (180 C, 6 bar) steam H 2 O natural gas des HP-pure CO 2 to CPU H 2 O PSA offgas (CH 4 2.5%, CO 13.7%, H %, CO %) 5

6 units FTR-SMR FTR-SMR CLR-PBR CO 2 capture NO MDEA H 2 O cond reforming efficiency (LHV basis) % Heat Rate (no steam export) Gcal fuel /knm 3 H Heat Rate (with steam) Gcal/kNm 3 H Electricity (prod/cons) GWh/kg H Advantages: The system is convenient also when CO 2 capture is considered Compared to FTR-SMR there are less conversion/separation steps Steam to process is significantly lower: S/C for FTR is 3.4; in this process is 1.9 (comb. ATR/FTR) Conventional turbomachines are considered The technology is flexible to different applications (i.e. Methanol, Fischer-Tropsch, etc..) 6

7 the model 1D adiabatic axially dispersed packed bed reactor model: details are in Spallina (2013, 2015), Gallucci (2015), Hamers (2013, 2014) The reactor model has been validated for CLC using Cu, Ni, Fe and Mn oxygen carriers The model has been used for design and optimization of dynamically operated PBR Pseudo-homogeneous model Radial temperature or concentration gradients are neglected Heat losses through the reactor wall are neglected (not true for lab-scale experimental validation) Kinetics of Ni/CaAl 2 O 4 G-S reactions and heterogeneous reactions are based on Medrano(2015) 1. Spallina V, Gallucci F, Romano MC, Chiesa P, Lozza G, van Sint Annaland M. Investigation of heat management for CLC of syngas in packed bed reactors. Chem Eng J 2013;225: Hamers HP, Gallucci F, Cobden PD, Kimball E, van Sint Annaland M. A novel reactor configuration for packed bed chemical-looping combustion of syngas. Int J Greenh Gas Control 2013;16: Gallucci F, Hamers HP, van Zanten M, van Sint Annaland M, Experimental demonstration of chemical-looping combustion of syngas in packed bed reactors with ilmenite, Chem Eng J 2015;274: Medrano JA, Hamers HP, Williams G, van Sint Annaland M, Gallucci F, NiO/CaAl 2 O 4 as active oxygen carrier for low temperature chemical looping applications, accepted for publication (Applied Energy) 7

8 REDUCTION REFORMING OXIDATION Temperature [ C] gas fraction [vol.] the model REDUCTION REFORMING OXIDATION CO Temperature H 2 O H 2 H 2 O CO time cycle [s] CO 2 +H 2 O Reformed syngas N 2 CH 4 PSA offgas (CH 4, H 2 O: S/C 2) Air Reduction with PSA off-gas leads to full gas conversion and the gas is delivered at high temperature The reforming step is providing H 2 -rich gas at the equilibrium conditions. Due to the lower temperature, the CH 4 conversion decreases at the end of reforming. During Oxidation the Gas temperature is in the range of C 8

9 Temperature [ C] the model CO 2 +H 2 O Reformed syngas REDUCTION REFORMING OXIDATION PSA offgas (CH 4, H 2 O: S/C 2) N 2 Air The OXIDATION step heats up the bed ( C) The REDUCTION with PSA-offgas moves the heat front to the reactor outlet (cooling less than 30% of the bed) The REFORMING acts as heat removal: the heat front cools down the reactor from left to right the reaction front cools down the reactor from top to down Solid Temperature Profile After OX After RED After REF Reactor Inlet reactor length [m] Reactor Outlet 9

10 the experiments small size PBR (heated) (about 500 g of OC/catalyst) L/min flow rate (1 bar up to 1100 C) medium size PBR (semi-adiabatic) (about 5 kg of OC/catalyst) L/min flow rate (7 bar up to 1100 C) 10

11 the experiments Air N 2 H 2 CO CO 2 Steam p T 1 Packed bed reactor oven oven oven Insulation material T 48 p Water condenser H 2 O PC Mass spectrometer Vent REACTIONS: RED: H 2 + NiO H 2 O + Ni (ΔH R = -15 kj/mol i ) CO + NiO CO 2 + Ni (ΔH R = -47 kj/mol i ) CH 4 + 4NiO 2H 2 O + CO 2 + 4Ni (ΔH R = 134 kj/mol i ) REF: CH 4 + H 2 O CO + 3H 2 ΔH R = 206 kj/mol i ) CH 4 + CO 2 2CO + 3H 2 ΔH R = 247 kj/mol i ) CO + H 2 O CO 2 + H 2 ΔH R = -41 kj/mol i ) small size PBR (heated) 10 L/min flow rate (1 bar up to 1100 C) OX: ½ O 2 + Ni NiO (ΔH R = -468 kj/mol i ) Reactor Length 0.5 m Ni-CaAl 2 O 4 as catalyst/oxygen carrier 11

12 gas mol fraction, dry H 2 mol fraction, dry REDUCTION The stability of the OC has been tested for more than 200h of operation by checking the breakthrough of the H 2 using 10 l/min (20 H 2 / 20 H 2 O / 60 N 2 ) H2_red#1 H2_ref#2 H2_ref#4 The experiments H 2 breakthrough H2_ref#1 H2_ref#3 H2_aug24th 1 st test (OC not completely activated) 0 0:00:00 0:04:19 0:08:38 0:12:58 0:17:17 0:21:36 time [ hh:mm:ss] syngas breakthrough 10L/min (H 2 /H 2 O/CO 2 /N 2 20/10/20/50) Different breakthroughs occur in presence of syngas (H 2 /CO 2 /H 2 O 20/20/10) Reverse WGS after the OC reduction has been completed CO 2 Reverse WGS CO H 2 0:00:00 0:01:44 0:03:27 0:05:11 0:06:55 0:08:38 time [hh:mm:ss] 12

13 T [ C] Reformate mol fraction, dry Reformate mol fraction, dry The experiments REFORMING Different industrially relevant compositions (combination of CH 4 /H 2 O/CO 2 ) diluted with N 2 have been tested The experiments have been done at 900 C, the same tests will be carried at 800 C The CH 4 full conversion has been achieved in both cases (working with high H 2 O or CO 2 dilution) The methane reforming (both steam and dry) reduces the temperature carbon deposition control has to be taken into account Bed Temperature profile (Reforming) REF_start REF 33% REF 66% REF_end Reactor length [m[ Reformate composition 10 L/min CH 4 /H 2 O/N 2 10/50/40) Steam Reforming H CO CH CO :00:00 0:01:26 0:02:53 0:04:19 0:05:46 0:07:12 time [ hh:mm:ss] Reformate composition 10 L/min (CH /CO 2 /N 2 10/60/30) 0.45 Dry Reforming CO CO H CH :00:00 0:00:43 0:01:26 0:02:10 0:02:53 0:03:36 0:04:19 time [hh:mm:ss] 13

14 Temperature [ C] O 2 vol. fraction [%] Experiments and Preliminary validation OXIDATION the kinetic model is predicting the breakthrough of the oxygen with high accuracy results confirms the previous experiments by Kooiman et al. (2015) using the same OC and reactor experiment model :00:00 0:01:26 0:02:53 0:04:19 0:05:46 0:07:12 0:08:38 0:10:05 0:11:31 cycle time [hh:mm:ss] the temperature rise is almost 600 C) very close to the adiabatic value ( 700 C) The thermal model is not able to catch the temperature rise at the beginning of the reactor (heat losses model need to be refined and adjusted) exp_30s exp_60s exp_90s model_30s model_60s model_90s reactor length [m] 14

15 Conclusions Chemical Looping Reforming is a very promising way to combine H 2 production and CO 2 capture A preliminary assessment shows already the gain (+1.5 percentage points compared to benchmark technologies) Several industrial relevant processes can benefit from chemical looping Commercial Ni-based OC has been (is being) successfully tested in a labscale reactor (more than 200 h) The first lab tests confirm the proof-of-principle (at 900 C and 1 bar for 10 L/min of syngas using different composition) Carbon deposition play an important role due to the temperature variation (high syngas dilution) Reformate composition is different than conventional plant (is that a problem in case of plant retrofitting?) but the way is long 15

16 Future research Experiments Mapping the operating conditions of the reactors: composition, temperature, dilution (i.e. S/C), flow rate Oxygen carrier characterization and stability test (under multiple cycles) Scale-up from 10 L/min (small PBR) to 100 L/min and 5 Modelling Design of the reactor Investigation with different reactor concepts Heat transfer modelling (i.e. heat losses, etc ) Heat management strategies Techno-economic assessment of full scale plant and comparison with conventional technologies for H 2 production Techno-economic assessment of the system for different process (CH 3 OH, Fischer-Tropsch, etc..) 16

17 THANK YOU FOR YOUR ATTENTION! CONTACT INFO: Vincenzo Spallina mail: 17

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