sic ceramic membrane de-oiling pilot prelimineary results - ptac 2009

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SiC CERAMIC MEMBRANE

DE-OILING PILOT

PRELIMINARY RESULTS

Ceramic Membrane Ceramic Membrane -- TypesTypes

Carrier Support Carrier Support ‘‘MonolithMonolith’’ with Thin Active Membrane Layerwith Thin Active Membrane LayerMembrane Layer Typically SlipMembrane Layer Typically Slip--Cast and SinteredCast and SinteredCommon Membrane Layer MaterialsCommon Membrane Layer Materials

OxidesOxides: Alumina: Alumina--, Titania, Titania-- and Zirconia oxidesand Zirconia oxidesNonNon--oxidesoxides: carbides, borides, nitrides: carbides, borides, nitridesCompositesComposites: combinations of oxides and non: combinations of oxides and non--oxides.oxides.CSP CSP –– Polymer Grafted to CeramicPolymer Grafted to Ceramic

Active membrane layer

Carrier support structure

Silicon Carbide (SiC) MembranesSilicon Carbide (SiC) MembranesSiC Monolith & SiC Membrane SiC Monolith & SiC Membrane SiC Membrane SiC Membrane

No liquid phase sintering of No liquid phase sintering of particlesparticlesFired at 2400Fired at 2400˚̊CCSublimation of fine grainsSublimation of fine grains

Results in:Results in:High flux rate High flux rate Highly HydrophilicHighly HydrophilicHighly Chemical ResistantHighly Chemical ResistantHighly Abrasion ResistantHighly Abrasion ResistantThermally RobustThermally RobustHigh durabilityHigh durabilityAllows Agressive Cleaning Allows Agressive Cleaning RegimesRegimes

Pilot Plants Pilot Plants

FilterBoxxFilterBoxx Has Constructed Two Ceramic Has Constructed Two Ceramic Membrane Pilot Plants Membrane Pilot Plants One Pilot Configured for Solid/Liquid SeparationOne Pilot Configured for Solid/Liquid SeparationOne Pilot Configured for DeOne Pilot Configured for De--Oiling ApplicationsOiling ApplicationsFully SelfFully Self--Contained Units Contained Units (Skid Mounted/Building (Skid Mounted/Building Enclosure)Enclosure)

Oil Oil –– Water Separation with Water Separation with SiC Ceramic MembranesSiC Ceramic Membranes Preliminary Pilot ResultsPreliminary Pilot Results

DeDe--Oiling Pilot PlantOiling Pilot Plant

Treating Desalter Bottoms at an Alberta Heavy Oil Treating Desalter Bottoms at an Alberta Heavy Oil RefineryRefineryIntent of Pilot to be Intent of Pilot to be ‘‘Proof of ConceptProof of Concept’’ for Application of for Application of Technology for DeTechnology for De--oiling of Produced Water from oiling of Produced Water from Thermal Heavy Oil OperationsThermal Heavy Oil OperationsExtreme Levels of Oil and SolidsExtreme Levels of Oil and SolidsUtilized Full Size Commercial Membrane Utilized Full Size Commercial Membrane (142mm x 865 mm)(142mm x 865 mm)

Examine Performance of Membrane Under Examine Performance of Membrane Under ‘‘Worst CaseWorst Case’’ScenarioScenarioObtain Basic Operating InformationObtain Basic Operating Information

DeDe--Oiling Pilot PlantOiling Pilot Plant

Basic Pilot ProcessBasic Pilot Process

Inlet Feed Surge Surge TankTank

Ceramic Membrane De-Oiling

Recirculation

Permeate

Back Pulse

Membrane Feed

Permeate Permeate TankTank

Reject Reject TankTank

Disposal

Pilot Program ObjectivesPilot Program Objectives‘‘Proof of ConceptProof of Concept’’ for Application of Technology for Defor Application of Technology for De--oiling of Produced Water from Thermal Heavy Oil Opsoiling of Produced Water from Thermal Heavy Oil OpsDemonstrate Demonstrate SiCSiC Ceramic Membranes Ability to Deliver Ceramic Membranes Ability to Deliver Consistent Permeate Quality Under Extreme Inlet Consistent Permeate Quality Under Extreme Inlet ConditionsConditionsDemonstrate Membrane System Ability to Treat Effluent @ Demonstrate Membrane System Ability to Treat Effluent @ Elevated Process Temperatures (up to 95Elevated Process Temperatures (up to 95oo C)C)Observe Basic Operating Parameters Observe Basic Operating Parameters (Flux, TMP, % Recovery)(Flux, TMP, % Recovery)

Obtain Analytical ResultsObtain Analytical Results

Pilot MembranePilot MembraneParameter Ceramic Membrane

Membrane Size 144 mm x 865 mm

Surface area/module (m2) (5mm x 5mm feed channels)

6.5

Max TMP(bar) 10 .3

Recommended minimum cross flow(liters/min)

1136

Clean water pressure drop (KPa)@ rec’d Cross flow

34

Material SiC MonolithSiC Membrane

Pore Size (µm) 0.04 & 0.1

Feed channels (mm x mm) 5 x 5

Pilot StartPilot Start--UpUpStarted System and Tested Clear Water Flux on Membranes at appliStarted System and Tested Clear Water Flux on Membranes at applied ed pressures of 10 to 40 pressures of 10 to 40 psipsiFlux of 650 LMH/bar observed for 0.04 micron membraneFlux of 650 LMH/bar observed for 0.04 micron membraneStarted Operation on Process Fluid Started Operation on Process Fluid Initial Membrane Flux of >500 LMH at a TMP of 20 Initial Membrane Flux of >500 LMH at a TMP of 20 psipsi decreasing to 350 decreasing to 350 LMH LMH

Operating TemperatureOperating Temperature

Feed CharacteristicsFeed CharacteristicsFeed O&G/TSS Highly VariableFeed O&G/TSS Highly VariableO&G Exceeding 250,000 mg/L O&G Exceeding 250,000 mg/L TSS Exceeding 20,000 mg/LTSS Exceeding 20,000 mg/L

Permeate CharacteristicsPermeate CharacteristicsPermeate Quality Permeate Quality –– ExcellentExcellentPermeate Quality Independent of FeedPermeate Quality Independent of FeedAt At TMPsTMPs Exceeding Critical Value Permeate Quality Impacted Exceeding Critical Value Permeate Quality Impacted (0.04 (0.04 micron 30 micron 30 psipsi, 0.1 micron 15 , 0.1 micron 15 psipsiBelow Critical TMP Membrane was Positive Barrier to OilBelow Critical TMP Membrane was Positive Barrier to Oil

Qualitative ResultsQualitative Results

FluxFluxFlux for 0.04 micron Membrane 200Flux for 0.04 micron Membrane 200--280 LMH @ 25 280 LMH @ 25 PsiPsiFlux for 0.1 micron Membrane 190Flux for 0.1 micron Membrane 190--320 LMH @10 320 LMH @10 PsiPsi

Flux MaintenanceFlux MaintenanceInitially No Flux Maintenance Processes Initially No Flux Maintenance Processes –– XX--flow onlyflow onlyBack Pulse Attempted on 0.04 micron membrane Back Pulse Attempted on 0.04 micron membrane –– Results not what was Results not what was expectedexpectedLater Found Faulty Check Valve on BackLater Found Faulty Check Valve on Back--Pulse PumpPulse PumpReRe--attempted with 0.1 micron membrane with clearly encouraging resuattempted with 0.1 micron membrane with clearly encouraging resultsltsLow Pressure (60psi) Steam was examined as flux maintenance toolLow Pressure (60psi) Steam was examined as flux maintenance tool with with encouraging resultsencouraging results

RecoveryRecoveryOverall Recovery Determined Based on Flow BalanceOverall Recovery Determined Based on Flow BalanceRecovery in Excess of 95% was AchievedRecovery in Excess of 95% was Achieved

Unusual EventsUnusual EventsShutShut--DownDown

Shortly After StartShortly After Start--up Pilot was halted due to site related issues. up Pilot was halted due to site related issues. Resulted in a longer than expected 10Resulted in a longer than expected 10--day shutday shut--down.down.Membrane had not been cleaned (only back flushed) and it was notMembrane had not been cleaned (only back flushed) and it was notknown that backknown that back--pulse system not working.pulse system not working.Noticeable StepNoticeable Step--Wise Decline in Flux upon ReWise Decline in Flux upon Re--starting pilot (Initial starting pilot (Initial Flux Dropped from 500 Flux Dropped from 500 LMH @ 20 LMH @ 20 psipsi to 300 LMH @30 to 300 LMH @30 psipsi))

Major Fouling EventMajor Fouling EventRag Layer of Rag Layer of DesalterDesalter was Inadvertently Directed into the Pilot Plantwas Inadvertently Directed into the Pilot PlantResulted in Major Fouling of the 0.04Resulted in Major Fouling of the 0.04μμ Membrane and Major Flux DeclineMembrane and Major Flux DeclinePermeate Quality During Event was not ImpactedPermeate Quality During Event was not ImpactedAttempts to clean the membrane and recover the flux were attemptAttempts to clean the membrane and recover the flux were attempted with limited ed with limited result.result.Pilot was continued with 0.1Pilot was continued with 0.1μμ membranemembrane

SummarySummary of Resultsof ResultsInitial Results Encouraging Initial Results Encouraging –– Achieved Achieved ““Proof of ConceptProof of Concept””SiCSiC Ceramic Membrane Capable of Producing Permeate Virtually Ceramic Membrane Capable of Producing Permeate Virtually Free of Dispersed and Emulsified Oil. However, dissolved organiFree of Dispersed and Emulsified Oil. However, dissolved organics cs present.present.Permeate with <10 mg/L Oil possible even with feed O&G exceedingPermeate with <10 mg/L Oil possible even with feed O&G exceeding240,000 mg/L240,000 mg/LAt Elevated At Elevated TMPTMP’’ss and High Oil Concentrations in the Feed and High Oil Concentrations in the Feed Permeate Quality Could be CompromisedPermeate Quality Could be Compromised

Above 30 Above 30 psipsi for 0.04 micron membranefor 0.04 micron membraneAbove 15 Above 15 psipsi for 0.1 micron membranefor 0.1 micron membrane

Permeate Recovery > 90% was possiblePermeate Recovery > 90% was possibleBackBack--Pulse with Permeate Found to be Effective in Flux Maintenance Pulse with Permeate Found to be Effective in Flux Maintenance with 0.1with 0.1μμ membranemembrane

Pulse Interval and Duration of 15Pulse Interval and Duration of 15--20 min and 20 to 30 seconds found to be most 20 min and 20 to 30 seconds found to be most effectiveeffective

In Normal Operation, Cleaning with Steam @ 60 In Normal Operation, Cleaning with Steam @ 60 psipsi found to be found to be Effective for Flux MaintenanceEffective for Flux Maintenance

Next StepsNext Steps

Discussions on FollowDiscussions on Follow--up Pilotup PilotOperation of Pilot Plant on SAGD/CSS Flows to Operation of Pilot Plant on SAGD/CSS Flows to Determine Operating FluxesDetermine Operating FluxesLonger Term Pilot (6 months)Longer Term Pilot (6 months)

Focus on Fouling and Flux MaintenanceFocus on Fouling and Flux Maintenance

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