Novel Engineered Osmosis Technology: A Comprehensive Approach to the Treatment and Reuse of Produced Water and Drilling Wastewater

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Best of RPSEA 10 Years of Research - Ultra-Deepwater and Onshore Technology Conference

1 Novel Engineered Osmosis Technology: A Comprehensive Approach to the Treatment and Reuse of Produced Water and Drilling Wastewater Tzahi Cath Colorado School of Mines Best of RPSEA 10 Years of Research - Ultra-Deepwater and Onshore Technology Conference August 30-31, 2016 The San Luis Resort, Spa & Conference Center, Galveston, TX 1 rpsea.org

2 A few thoughts about desalination o Energy for reverse osmosis (SWRO) desalination close to the thermodynamic limit of separation o Reverse osmosis is limited to low salinity water Desalination of seawater (3.5%) is limited to ~60% water recovery o The cost of desalinated seawater is ~$1.7/m 3 (~27 /bbl) o For the same feedwater salinity (and even lower), the cost of produced water treatment is ~$1.7/bbl There are ~6.3 bbl in one m 3 >>>> ~$11/m 3 produced water o Common hurdles need thorough pretreatment (!) 2

3 Engineering Osmosis vs. Osmotic Dilution DP=Dp Brine Reconcentration Draw Solution Feed Brine (Draw Solution) Feed Osmosis (Osmotic Dilution) Forward Osmosis (Engineered Osmosis) 3

4 Forward Osmosis: Theory & Transport Phenomena o Engineered osmosis O&G wastewater pretreatment J w» A( Dp ) J S» B( DC ) Brine Reconcentration Draw Solution Feed Forward Osmosis engineered osmosis J w Water flux J s Solute transport A Pure water permeability B Solute permeability 4

5 Forward Osmosis: Theory & Transport Phenomena o Engineered osmosis O&G wastewater pretreatment J w» A( Dp ) J S» B( DC ) FO Membrane Brine Reconcentration Draw Solution Feed Draw Solution O&G WW Forward Osmosis engineered osmosis Contaminant Transport Permeate quality Reverse Salt Flux Loss of driving force J w Water flux J s Solute transport A Pure water permeability B Solute permeability 5

Forward Osmosis: Theory & Transport Phenomena o Engineered osmosis O&G wastewater pretreatment Woven Polyester Support S º tt e Brine Reconcentration Draw Solution Feed Forward

6 Forward Osmosis: Theory & Transport Phenomena o Engineered osmosis O&G wastewater pretreatment Woven Polyester Support S º tt e Brine Reconcentration Draw Solution Feed Forward Osmosis engineered osmosis Dense Polymer Active Layer Porous Support Layer S Structural parameter t Support layer thickness τ Tortuosity of porous layer ε Porosity of support layer 6

Desalination Technologies Specific Energy, kwh/m 3 30 20 10 0 Membrane Limited Recovery High Pressure

7 Desalination Technologies Specific Energy, kwh/m Membrane Limited Recovery High Pressure Simple/modular High FO/RO Efficiency RO SWRO Crystallizer Brine Concentrators MBC v1.0 Membrane Distillation MBC v2.0 Thermal High recovery Energy to boil water Exotic metals Membrane Brine Concentrator (MBC) High Recovery Modular No Boiling/Low Pressure 1% 2% 3% 4% 5% 10% 25% 50% 75% 7 Sources: Oasys Water % Total Dissolved Solids

8 The Water-Energy Nexus Water Management at the O&G Upstream Sector Internal Reuse Fracturing Flowback Produced Water 8

Research Objectives o Support forward osmosis (FO) membrane development for O&G wastewater treatment Bench-scale membrane performance evaluations Membrane and foulant characterization o Enhance

9 Research Objectives o Support forward osmosis (FO) membrane development for O&G wastewater treatment Bench-scale membrane performance evaluations Membrane and foulant characterization o Enhance innovative membrane surface characterization strategies Membrane zeta potential (surface charge) o FO system scale-up Design, build, and operate pilot system o Process modeling Life cycle impact assessment Economic evaluations FOROSA design package Systems Level Engineering Pilot-scale Development Membrane Surface Autopsy Process Modeling 9

10 Research Structure 1. Tech Assessment Development & Optimization of FO Processes FO Process Performance for O&G WW Treatment 2. Hydraulic TMP in FO 3. High Salinity Zeta Potential 4. Membrane Fouling & Rejection 5. Effects of PW on Membrane Performance 6. Pilot-scale Study 7. Life Cycle Assessment/Life Cycle Costing 10

11 Outputs: Publications o o o o o o o o o Regnery, J., Coday, B.D., Riley, S.M., Cath, T.Y., Solid-phase extraction followed by gas chromatography-mass spectrometry for the quantitative analysis of semi-volatile hydrocarbons in hydraulic fracturing wastewaters, Analytical Methods (RSC), 8 (2016) Coday, B.D., Hoppe-Jones, C., Wandera, D., Shethji, J., Herron, J., Lampi, K., Snyder, S.A., Cath, T.Y., Evaluation of the transport parameters and physiochemical properties of forward osmosis Membranes after treatment of produced water, Journal of Membrane Science, 499 (2016) Coday, B.D., Miller-Robbie, L., Beaudry, E.G., Munakata-Marr, J., Cath, T.Y., Life cycle and economic assessments of engineered osmosis and osmotic dilution for desalination of Haynesville shale pit water, Desalination, 369 (2015), Coday, B.D., Almaraz, N., Cath, T.Y., Forward osmosis desalination of oil and gas wastewater: Impacts of membrane selection and industrial operating conditions, Journal of Membrane Science, 488 (2015) Coday, B.D., Luxbacher, T., Childress, A.E., Almaraz, N., Xu, X., Cath, T.Y., Indirect determination of zeta potential at high ionic strength: Specific application to semipermeable polymeric membranes, Journal of Membrane Science, 478 (2015) Coday, B.D., Yaffe, B.G.M., Xu, P., Cath, T.Y., Rejection of trace organic compounds in forward osmosis: A literature review, Environmental Science & Technology, 48 (7), (2014) Coday, B.D., Cath, T.Y., Forward osmosis: Novel desalination of produced water and fracturing flowback, Journal AWWA, 106 (2) (2014) E55-E66. Coday, B.D., Xu, P., Beaudry, E.G., Herron, J., Lampi, K., Hancock, N.T., Cath, T.Y., The sweet spot of forward osmosis: treatment of produced water, drilling wastewater, and other complex and difficult liquid streams, Desalination, 333 (2014) Coday, B.D., Heil, D.M., Xu, P., Cath, T.Y., The effects of transmembrane hydraulic pressure on performance of forward osmosis membranes, Environmental Science & Technology, 47 (5) (2013)

12 Focus of the presentation today 1. Tech Assessment FO background Development & Optimization of FO Processes FO Process Performance for O&G WW Treatment 2. Hydraulic TMP in FO 3. High Salinity Zeta Potential 4. Membrane Fouling & Rejection 5. Effects of PW on Membrane Performance 6. Pilot-scale Study 7. Life Cycle Assessment/Life Cycle Costing 12

operate Employ specialized software Life cycle impact assessment software Custom designed software for FO-RO

13 Research Methodologies o Major methods and materials: Chemicals and analysis All chemicals used were ACS grade 1 M NaCl for FO draw solution Detection of trace contaminants in high TDS matrix System design, build, and operate Employ specialized software Life cycle impact assessment software Custom designed software for FO-RO system design (VBA Excel based) ~20 GPM Feed Flow ~6.3 m 2 Membrane Area 13 ~0.6 GPM Feed Flow ~0.02 m 2 Membrane Area

14 Research Methodologies TDS: 20,000 to 30,000 mg/l DOC: 200 mg/l to 2500 mg/l COD: 500 mg/l to 12,000 mg/l Alkalinity: >600 mg/l as CaCO 3 14

15 15 Effects of Transmembrane Hydraulic Pressure (TMP) on Performance of Forward Osmosis Membranes

16 Research Objectives & Relevance o Research objective: To explore FO membrane performance at increasing hydraulic TMP Water flux o Relevance: Reverse salt flux (RSF) Inorganic feed ion rejection Bi-directional solute flux Organic molecule rejection Hydraulic transmembrane pressure (TMP) in FO is common in industrial treatment but effects are never investigated Laboratory results under-predict true membrane performance Impact of membrane selection Impact on permeate water quality 16 TMP Transmembrane pressure

17 Water flux, L/m 2 -hr Water Flux at Increasing TMP CTA vs. Emerging TFC Membrane TFC1 CTA TFC2 CTA Transmembrane pressure, PSI FO Membrane 1M NaCl: DI Feed Solution 17 CTA Cellulose triacetate TFC Thin-film composite (polyamide) J w Water flux

18 Reverse salt flux, mmol/m 2 -hr 2 -hr RSF at Increasing TMP CTA vs. Emerging TFC Membrane TFC1 CTA TFC2 CTA Feed Solution FO Membrane Draw Solution Transmembrane pressure, PSI PSI 1M NaCl Draw Solution : DI water Feed Solution 18 CTA Cellulose triacetate TFC Thin-film composite (polyamide) J s Ion (solute) flux

19 Reverse Salt Flux, mmol/m 2 -hr Anion rejection, % Cation rejection, % CTA Membrane Cl Na Transmembrane pressure, PSI Mg Li K SO4 Br NO Transmembrane pressure, PSI 19 CTA Cellulose triacetate TFC Thin-film composite (polyamide)

20 Reverse Salt Flux, mmol/m 2 -hr Anion rejection, % Cation rejection, % TFC Membrane Na Cl Transmembrane pressure, PSI Mg Li 80 K SO4 70 Br 60 NO Transmembrane pressure, PSI 20 CTA Cellulose triacetate TFC Thin-film composite (polyamide)

21 21 Forward Osmosis Desalination of Oil and Gas Wastewater: Impacts of Membrane Selection and Operating Conditions on Process Performance

22 Research Objectives & Relevance o Research objectives: To assess FO treatment of raw produced water Membrane type (Cellulose triacetate vs. different polyamide surface chemistries) Industrial operating conditions FO module design (effects of feed spacer) To identify sustainable operating methods for pilot-scale and full-scale operations o Relevance: Understand fouling mechanisms of FO membranes in O&G WW treatment Chemically resistant to complex O&G WW feeds? Benchmark for future membrane designs Plate-and-frame membrane modules Novel hollow fiber CTA FO membranes 22

23 Engineered Osmosis vs. Osmotic Dilution o Osmotic Dilution o Engineered Osmosis 23

24 Experimental Research Stepwise Performance Evaluation Cellulose Triacetate (CTA) Polyamide TFC (TFC1) Polyamide TFC + Proprietary surface coating (TFC2) 24

25 Membrane Performance Results: Effects of Membrane Selection Normalized water flux, J w /J w OB OB OB OB CTA TFC1 TFC2 Test Set A Permeate volume, L o >2000 hrs of bench-scale fouling data o Initial membrane fouling Permeate drag forces Independent of membrane surface properties Formation of complex cake layer o Long term membrane fouling Foulant-foulant interactions Similar flux decline regardless of membrane permeability 25 OB Osmotic backwash

Operating Conditions: Membrane Spacers 100 90 80 70 60 50 40 30 20 10 0 Standardized Testing Methods [A] Chevron Feed Spacer Virgin Spiral Wound

26 0 Hr 6 Hr 12 Hr 18 Hr 24 Hr OB 30 Hr 36 Hr 42 Hr 48 Hr 0 Hr 6 Hr 12 Hr 18 Hr 24 Hr OB 30 Hr 36 Hr 42 Hr 48 Hr 0 Hr 6 Hr 12 Hr 18 Hr 24 Hr OB 30 Hr 36 Hr 42 Hr 48 Hr 0 Hr 6 Hr 12 Hr 18 Hr 24 Hr OB 30 Hr 36 Hr 42 Hr 48 Hr Normalized water flux, % Membrane Performance Results Effects of Operating Conditions: Membrane Spacers Standardized Testing Methods [A] Chevron Feed Spacer Virgin Spiral Wound Crossflow Chevron Velocities Spacer Fouled Increased Transmembrane Pressure Membrane Surface Test Set A Tast Set B Test Set C Test Set D Osmotic backwash 26

27 0 Hr 6 Hr 12 Hr 18 Hr 24 Hr OB 30 Hr 36 Hr 42 Hr 48 Hr 0 Hr 6 Hr 12 Hr 18 Hr 24 Hr OB 30 Hr 36 Hr 42 Hr 48 Hr 0 Hr 6 Hr 12 Hr 18 Hr 24 Hr OB 30 Hr 36 Hr 42 Hr 48 Hr 0 Hr 6 Hr 12 Hr 18 Hr 24 Hr OB 30 Hr 36 Hr 42 Hr 48 Hr Normalized water flux, % Membrane Performance Results Effects of Operating Conditions: Membrane Spacers Standardized Testing Methods [A] Chevron Feed Spacer Spiral Wound Crossflow Chevron Velocities Spacer Increased Transmembrane Pressure Membrane Surface Test Set A Tast Set B Test Set C Test Set D Osmotic backwash 27

Spacers 100 90 80 70 60 50 40 30 20 10 0 Standardized Testing Methods [A] 4000 Chevron Feed Spacer Virgin Membrane Fouled Membrane CaCO3+Oil Residues 3200 2400 1600

28 0 Hr 6 Hr 12 Hr 18 Hr 24 Hr OB 30 Hr 36 Hr 42 Hr 48 Hr 0 Hr 6 Hr 12 Hr 18 Hr 24 Hr OB 30 Hr 36 Hr 42 Hr 48 Hr 0 Hr 6 Hr 12 Hr 18 Hr 24 Hr OB 30 Hr 36 Hr 42 Hr 48 Hr 0 Hr 6 Hr 12 Hr 18 Hr 24 Hr OB 30 Hr 36 Hr 42 Hr 48 Hr Normalized water flux, % Transmittance Membrane Performance Results Effects of Operating Conditions: Membrane Spacers Standardized Testing Methods [A] 4000 Chevron Feed Spacer Virgin Membrane Fouled Membrane CaCO3+Oil Residues Wavenumber, cm -1 (e) 800 Spiral Wound Crossflow Velocities Increased Transmembrane Pressure Membrane Surface Test Set A Tast Set B Test Set C Test Set D Osmotic backwash 28

29 0 Hr 6 Hr 12 Hr 18 Hr 24 Hr OB 30 Hr 36 Hr 42 Hr 48 Hr 0 Hr 6 Hr 12 Hr 18 Hr 24 Hr OB 30 Hr 36 Hr 42 Hr 48 Hr 0 Hr 6 Hr 12 Hr 18 Hr 24 Hr OB 30 Hr 36 Hr 42 Hr 48 Hr 0 Hr 6 Hr 12 Hr 18 Hr 24 Hr OB 30 Hr 36 Hr 42 Hr 48 Hr Normalized water flux, % Membrane Performance Results Effects of Operating Conditions: Cross-flow Velocity Standardized Testing Methods [A] Chevron Feed Spacer Spiral Wound Crossflow Velocities Increased Transmembrane Pressure Test Set A Tast Set B Test Set C Test Set D Osmotic backwash 29

30 OD GW SM AP EP CP NCP RE EcP FFD Contribution to impact category Treatment Cost, $/bbl Membrane Performance Results Effects of Operating Conditions: Cross-flow Velocity 100% 90% 80% 70% 60% 50% Engineered Osmosis Transport & Disposal NF Energy NF Membranes NF Infrastructure NF Membrane CC RO Energy RO Membranes Fixed Capital Labor & Spares Energy Cleaning Chemicals 40% 30% 20% 10% 0% RO Infrastructure RO Membrane CC FO Energy FO Membranes FO Infrastructure FO Membrane CC NF Membrane Replacement RO Membrane Replacement FO Membrane Replacement TRACI 2.1 impact category RO < 4 kwh/m 3 FO kwh/m 3 30 Coday, B.D., Miller-Robbie, L., Beaudry, E.G., Munakata-Marr, J., Cath, T.Y., Life cycle and economic assessment of engineered osmosis and osmotic dilution for desalination of Haynesville shale pit water, Desalination, 2015, 369 (2015) 188-

Assessing the Environmental Impacts: Inventory of the life cycle assessment o FO system: 24 x 8 spiral wound FO elements Brine consumption 26% NaCl [A] OD 0.27 m3/m3 prod. water EO 0.002 m3/m3 prod.

31 Assessing the Environmental Impacts: Inventory of the life cycle assessment o FO system: 24 x 8 spiral wound FO elements Brine consumption 26% NaCl [A] OD 0.27 m3/m3 prod. water EO m3/m3 prod. water Energy demand 15 kwh/m 3 prod. water Membrane cleaning 1/month, KL7330 Membrane lifespan 3 years 31 [A} Hutchings, Nathan R., Eric W. Appleton, and Robert A. McGinnis. "Making high quality frac water out of oilfield waste." SPE Annual Technical Conference and Exhibition. Society of Petroleum Engineers, 2010.

water Membrane cleaning 1/week, KL7330 Membrane lifespan 3 years o NF system: 3 x 4

32 Assessing the Environmental Impacts: Inventory of the life cycle assessment o RO system: 12 x 8 spiral wound RO elements Energy demand 6.5 kwh/m3 prod. water Membrane cleaning 1/week, KL7330 Membrane lifespan 3 years o NF system: 3 x 4 spiral wound NF elements Energy demand 0.5 kwh/m3 prod. water Membrane cleaning 1/week, KL7330 Membrane lifespan 3 years 32

33 0 Hr 6 Hr 12 Hr 18 Hr 24 Hr OB 30 Hr 36 Hr 42 Hr 48 Hr 0 Hr 6 Hr 12 Hr 18 Hr 24 Hr OB 30 Hr 36 Hr 42 Hr 48 Hr 0 Hr 6 Hr 12 Hr 18 Hr 24 Hr OB 30 Hr 36 Hr 42 Hr 48 Hr 0 Hr 6 Hr 12 Hr 18 Hr 24 Hr OB 30 Hr 36 Hr 42 Hr 48 Hr Normalized water flux, % Membrane Performance Results Effects of Operating Conditions: Increased TMP Standardized Testing Methods [A] Chevron Feed Spacer Spiral Wound Crossflow Velocities Increased Transmembrane Pressure Test Set A Tast Set B Test Set C Test Set D Osmotic backwash 33

34 Normalized water flux (J /J o ), % Flux Recovery Membrane Cleaning and Surface Characterization KL7330 EDTA CC Permeate volume, L Membrane flux recovery TFC2 CTA TFC1 34

35 Flux Recovery Membrane Cleaning and Surface Characterization TFC1 TFC2 >50% difference Water & solute permeability (A&B) and Structural parameter (S) Membrane surface energetics and hydrophilicity Membrane zeta potential 35

85 80 75 70 65 60 55 50 Test Set A Test Set D CTA TFC1 TFC2 TFC1 Draw Solution EEM TFC2 Draw Solution EEM 36

36 DOC rejection, % Rejection of O&G Feed Species Inorganic Ions and Dissolved Organic Compounds K Li Sr Ba Ca Inorganics rejection, % CTA Draw Solution EEM Ni Mg Test Set A Test Set D LC-QTOF Test Set A Test Set D CTA TFC1 TFC2 TFC1 Draw Solution EEM TFC2 Draw Solution EEM 36 DOC Dissolved organic carbon EEM Excitation-emission Matrix LC-QTOF Liquid chromatography quadrupole time of flight

37 37 Impacts of Raw Produced Water on the Physiochemical Properties and Solute Selectivity of Forward Osmosis Membranes

38 Research Objectives & Relevance o Research objectives: To investigate the impacts of produced water exposure on FO membranes: o Relevance: Pure water flux Reverse salt flux & specific reverse salt flux (SRSF) Contaminant rejection Membrane physiochemical properties Unique changes in TFC membrane solute selectivity after exposure to O&G WW regardless of: Feed stream sample System operating conditions Cleaning method employed 38

Change in SRSF, % Impacts of Exposure to Produced Water Shifts in Membrane Performance 40 30 CTA TFC2 20 KL7330 EDTA 10 0-10 -20 2.5 3.2-32.4-27.

39 Change in SRSF, % Impacts of Exposure to Produced Water Shifts in Membrane Performance CTA TFC2 20 KL7330 EDTA Post chemical cleaning Specific Reverse Salt Flux (SRSF) = Js Jw B A Loss of draw solution salt/volume of water recovered 39 J s Reverse solute flux J w Water flux B Solute perm. coef. A Water perm. coef.

40 Water flux, L/m 2 -hr Reverse salt flux, mmol/m 2 -hr Water flux, L/m 2 -hr Reverse salt flux, mmol/m 2 -hr Impacts of Exposure to Produced Water Water Flux and Reverse Salt Flux Post Exposure CTA Pre exposure Post exposure TFC2 Pre exposure Post exposure Draw solution conc., M Draw solution conc., M SRSF 0 = 0.65 g/l SRSF 1 = 0.61 g/l SRSF 0 = 0.24 g/l SRSF 1 = 0.13 g/l 40 SRSF = J s J w

41 41 Pilot-scale Investigation of Engineered Osmosis for Treatment of O&G Produced Water and Fracturing Flowback Water

42 Pilot-scale Study DJ Basin/Niobrara Shale Northeastern Colorado Denver Basin 42

43 Pilot-scale Study 3x 4040 Element FO System Front View 43

44 Pilot-scale Study 3x 4040 Element FO System cont. 20 GPM feed flow rate Back View LabView/DAQ System 44

45 Pilot-scale Study 3x 2540 Element RO System RO System Front View 45

46 46 Hybrid FO/RO Pilot-scale System

47 FO Water Flux, LMH Specific FO Flux FO Feed Conductivity, ms/cm Hybrid FO/RO Pilot-scale Performance FO Flux (LMH) Time, Hours FO Feed Time, Hours 47

48 The Future of FO for Complex WW o Solute and contaminant transport Optimization of TFC membrane (active & support structure) to minimize RSF & ICP (TMP study) Electrostatic surface properties might help to better predict contaminant rejection further testing in complex matrices is needed Understanding hydrocarbon transport and specific polymer interactions is a future challenge of FO in O&G o The application of FO for O&G WW Are spiral wound modules the best fit for O&G WW with no pretreatment? Where are the breakpoints between pretreatment and economic viability? How might increased pretreatment lower the current energy demands of FO? 48

Acknowledgements 49 o o o o o o o o Membrane manufacturer - Hydration Technology Innovations Membrane manufacturer - Oasys Water NGL Energy Partners (formerly High Sierra)

Association (AWRA) WateReuse Colorado (WRCO) Technical Advisors Dr. Dave Stewart, Dr. Wayne Buschmann, Mr. John Veil Colorado School of Mines AQWATEC / Cath Research Group Dr.

49 Acknowledgements 49 o o o o o o o o Membrane manufacturer - Hydration Technology Innovations Membrane manufacturer - Oasys Water NGL Energy Partners (formerly High Sierra) test site support Bayswater E&P produced water supply Financial support US Department of Energy/RPSEA American Water Works Association (AWWA) American Water Resources Association (AWRA) WateReuse Colorado (WRCO) Technical Advisors Dr. Dave Stewart, Dr. Wayne Buschmann, Mr. John Veil Colorado School of Mines AQWATEC / Cath Research Group Dr. Dean Heil, Dr. Mengistu Geza, Dr. Leslie Miller-Robbie External academic support Prof. Pei Xu, Prof. Amy Childress, Dr. Christiane Hoppe-Jones, Dr. Thomas Luxbacher, Prof. Shane Snyder

50 Contacts Principal Investigator: Tzahi Cath Colorado School of Mines Project Manager: Sandy McSurdy NETL Technical Coordinator: Kent Perry RPSEA

Forward Osmosis Principles, Trends, and Applications

Forward Osmosis Principles, Trends, and Applications Tzahi Y. Cath Department of Civil and Environmental Engineering Colorado School of Mines Golden, Colorado DesalTech 215 San Diego, CA August 28, 215