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Redox-Based Electrochemical Separations

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Redox-Based Electrochemical Separations Separations Consortium Redox-based Electrochemical Separations March 11, 2021 Technology Area Session: Performance-Advantaged Bioproducts, Bioprocessing Separations, and Plastics Lauren Valentino, Edward Barry, Yupo Lin, Philip Laible, Eric Tan, Bill Kubic, Jennifer Dunn ANL, NREL, LANL This presentation does not contain any proprietary, confidential, or otherwise restricted information Project Overview Context Fuel Biomass Pretreatment Enzymatic Purification & Biological Product product • Separations account for up to 70% of & conditioning hydrolysis concentration conversion* upgrading processing costs for biofuels and Lignin, solids *includes separation bioproducts1 Liquor • BETO design case: Anaerobic production Lignin Chemical upgrading of carboxylic acids that are upgraded to co-product BETO design case hydrocarbon fuel • Separation of organic species in biomass conversion processes is energy-intensive2 Goal: Develop redox-based electrochemical separations to selectively separate and recover aqueous organic acid compounds, specifically butyric acid from fermentation broth streams to enable cost-effective and sustainable renewable biodiesel production State of technology and limitations: Simulated moving bed is limited to A/B separations; Pertraction and electrodeionization have been investigated by the Separations Consortium (slide 9) Importance: Efficient separation processes are needed meet the BETO cost target of $2.5/GGE Risks: Capacitive deionization is used at the industrial scale for water treatment but has not been demonstrated for organic acid separation. Redox-active materials will enable selective separations. [1]: BETO 2016 strategic plan; [2] BETO 2019 SOT report 2 Management • Weekly meetings to coordinate and discuss experimental progress • Weekly analysis meetings to evaluate economic and sustainability measures • Collaboration with inCTRL Solutions via weekly meetings to estimate material and separation process costs • Monthly Consortium meetings • Bi-annual meeting with Industrial Advisory Board for progress updates and feedback • SmartSheets tool used to monitor interdependencies and progress towards go/no-go and internal project milestones Process Process modeling – modeling – Materials + Biochem Alternative Experimental process modeling design case applications R&D / cost estimation Life cycle assessment 3 Approach Conventional capacitive deionization (CDI) principles Carbon-based materials • Porous conductive electrodes are charged by Cation applying an electrical potential Non-specific / Non-selective Anion Adsorption / charging – Electrode material cost, capacity, durability, and lifetime are key considerations Cathode (-) e- • Adsorption: Under applied potential, ion transport is driven towards electrodes where the ions are Anode (+) stored – Charging time is a key operational parameter Desorption / discharging • Desorption: Ions are stored until the electric potential is reversed or removed resulting in the release of ions – Discharging time is a key operational parameter Redox chemistry will enable selective separation of organic species (carboxylates) 4 Approach Sensitivity analysis for CDI system performance Separation cost ($/kg butyrate) $0.50 $1.50 $2.50 $3.50 Electrode capacity (kg butyrate/m²/cycle) 0.2 0.05 Charge time (d) 0.05 0.2 Increasing the electrode Discharge time (d) 0.05 0.2 capacity by a factor of 4 (from 0.05 to 0.2 kg/m2) decreases Carbon lifetime (yr) 2 0.5 separation cost by a factor of 3. O&M (% ISBL) 0.025 0.1 Future work: incorporate into Up time (%) 0.99 0.75 biorefinery-level TEA to assess Energy requirement (kWh/kg butyrate) 0.5 2 impacts on MFSP TEA identifies research and development priorities and guides experimental work Capacity and cycle time (charge + discharge time) are key cost drivers and are the focus of experimental work 5 Approach Technical approach: parallel development of CDI process and redox-active materials in conjunction with TEA / LCA • Challenges • Economic and technical metrics (GNG on slide 8) – Redox-active material fabrication cost and – Energy consumption, recovery, and purity scalability – Electrode capacity – Fouling potential and clean-in-place strategies – MFSP and GHG emissions for TEA and LCA CDI process development Redox-based electrode fabrication Develop with Measure Modify Screen for activated performance operating Functionalize Scale up butyrate carbon indicators conditions material synthesis (capacity, energy, (charge/discharge selectivity electrodes recovery) time, flow rate) Redox-based CDI for butyrate separation Measure Adapt redox Integrate redox- performance material to form based electrode indicators electrodes into CDI (capacity, energy, recovery, purity) 6 Approach Conventional CDI Redox-based CDI Carbon-based materials Redox active electrodes Cation Butyrate Non-specific / Non-selective Anion Specific / selective Anion impurity Adsorption / charging Adsorption / extraction Cation Cathode (-) Cathode (-) e- e- Redox anode (+) Anode (+) Desorption complete Adsorption complete e- Desorption / discharging Redox anode (+) Desorption / recovery Redox chemistry will enable selective separation of carboxylic acids and greater electrode capacity 7 Approach Go/no-go decision point (occurs in FY21) Name Description Criteria Date B.2 [ANL]: RECS Evaluate whether RECS Determine whether the selectivity, separation, and 6/30/2021 performance compared exhibits improvements over capture ratio for RECS exceeds those of (i) CDI by to CDI and consortium baseline CDI technology and at least 100% for C2-C4 carboxylates, and (ii) EDI technologies for butyric EDI and ISPR as evaluated and ISPR targets with respect to energy acid (C4) separation within the Consortium. consumption (≤1.2kWh/lb) and recovery (≥70% at purity ≥80%). Electrodeionization (EDI) Membrane pertraction R&D within the Separations Consortium showed that economics and sustainability of EDI and pertraction outperform simulated moving bed at the biorefinery level. RECS performance will be evaluated against these technologies. RECS: Redox-based electrochemical separations 8 Impact Relevance to industry and BETO • RECS will provide an alternative to simulated moving bed (SMB), EDI, and pertraction – SMB: limited to A/B separations only, expensive stationary phase, solvent recycling is complicated in reverse phase – EDI: more cost-intensive and greater GHG emissions than pertraction – Pertraction: limited to pH<5.5, titers>10 g/L, and acids with boiling point<240°C • CDI has been demonstrated at industrial scale but not for bioprocessing separations • If successful, CDI and/or RECS could be tailored for other applications including homogeneous catalyst recycling, by-product recovery, and impurity removal SOT: Simulated Moving Bed1 • Integration with biomass conversion processes at NREL and analysis (NREL, LANL, ANL) • Supports BETO mission to develop sustainable bioenergy technologies Commercialization partnerships • Ongoing collaboration with Atlantis Technologies will enable technology transfer Dissemination of materials fabrication, process design, and techno- economic and sustainability analysis results CDI at commercial scale2 • Presentation at scientific conferences and publication in peer-reviewed journals (60,000 m3/d) [1]: AZoM 2017 (https://www.azom.com); [2]: Suss et al. 2015 9 Approach Technical approach: parallel development of CDI process and redox-active materials in conjunction with TEA / LCA • Challenges • Economic and technical metrics (GNG on slide 8) – Redox-active material fabrication cost and – Energy consumption scalability – Butyric acid recovery and purity – Fouling potential and clean-in-place strategies – MFSP and GHG emissions for TEA and LCA CDI process development Redox-based electrode fabrication Develop with Measure Modify Screen for activated performance operating Functionalize Scale up butyrate carbon indicators conditions material synthesis (capacity, energy, (charge/discharge selectivity electrodes recovery) time, flow rate) Redox-based CDI for butyrate separation Measure Adapt redox Integrate redox- performance material to form based electrode indicators electrodes into CDI (capacity, energy, recovery, purity) 10 Progress and Outcomes Lab-scale CDI system with LabVIEW-based control and data logging software • Power supply, peristaltic pump, in-line conductivity probe, valves, and a laptop with LabVIEW • User-specified operational parameters for adsorption/removal and desorption/recovery • Real-time monitoring of voltage, current, and conductivity • Valves at stack inlet and outlet will help to achieve recovery and purity targets for the GNG and provide framework for clean-in-place strategies (based on Industrial Advisory Board feedback) LabVIEW user interface Process flow diagram Program Conductivity Control meter Power supply Recovered Organic organic acid feed acid solution Valve Valve Pump De- CDI module ionized Cleaning solution agent LabVIEW module developed for data acquisition and instrument control 11 Progress and Outcomes 700 1.6 ) CDI with activated carbon electrodes L / g 1.4 Outlet Cycle 1 Cycle 2 Cycle 3 Cycle 4 Cycle 5 Cycle 6 Cycle 7 m 600 ( n o 1.2 i t 500 a Outermetal plate Outermetal plate r Current collector Current ) Current collector Current t Carbon Carbon electrode Carbon electrode Plastic block Plastic block 1 V Nylonmesh n (Cathode/ ( Gasket Gasket (Anode/+) Gasket spacer e 400 e c g n - 0.8 ) a o t l c 300 o e V t 0.6 a Inlet r y 200 t 0.4 u b Electrode capacity = ~30 mg/g at 1.2 V t 100 n 0.2 e u l f f 0 0 E
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