Dahmen, Nicolaus

Eberhard, Mark

Kolb, Thomas

Lam, H.

Mai, Robert

Michelfelder, Bernd

Niebel, A.

Otto, T.

Pfitzer, C.

Sauer, Jörg

Stapf, Dieter

Willy, Matthias

Zimmerlin, Bernd

English

KITopen

KIT – The Research University in the Helmholtz Associationbioliq     biomass to liquid Institute for Technical Chemistry, ITCInstitute for Catalysis Research and -Technologie, IKFTEngler-Bunte-Institute,  Fuel  Technology, EBI cebwww.kit.eduOperations of the bioliq® pilot plant - entrained flow gasification in 5 MW pilot scale B. Zimmerlin, M. Eberhard, N. Dahmen, H. Lam, R. Mai, B. Michelfelder, A. Niebel, T. Otto, C. Pfitzer, M. Willy, T. Kolb, J. Sauer, D. Stapf Waste2H2 - Workshop, KIT, September 19-26, 20222 2022.09.19 Institute for Technical Chemistrybioliq®  de-central / central conceptBernd ZimmerlinEnergy density: 2 GJ/m3 25 GJ/m3 36 GJ/m3Energy densification of biomass in regionally distributed fast pyrolysis plants Transport of intermediate bio-slurry over long distanceGasification + Synthesis in central large scale units 3 2022.09.19 Institute for Technical ChemistryTank farm(240 m³)2012-2018Biomass conditioningHot gas cleaning(2 MW, 700 Nm3/h)2009-2011Gasoline synthesis(2 MW, 50 kg/h)2009-2011Fast pyrolysis(2 MW, 500 kg/h)2005-2008High Pressure Entrained  Flow Gasification (5 MW, 1 t/h)2008-2013Biosyncrude2011-2014bioliq® pilot plant Bernd Zimmerlin4 2022.09.19 Institute for Technical ChemistryDesigned as pilot plant with many options concerning R&D for process optimization, not as a production plantOperated in 4 to 5 campaigns per year, each with 2-5 weeks of 24/7 operationOperated by a staff of about 40 operators and engineers in a 4-shift systembioliq® pilot plant Bernd Zimmerlin5 2022.09.19 Institute for Technical Chemistrybioliq® - Process Control System (PCS)Features Process control softwareSiemens SPPA -T3000 Fault-tolerant / fail-safe automation systems Simatic S7 400 series PROFIBUS connectivity to approximately 20 sub-systems  Extensive instrumentation, in total:~    200 electrical drives~    350 shut-off valves~ 2000 measured variables~  2400 alarms and warnings~    250 PID control loops~    150 SIL 1 & SIL 2 safety functions Fulfills operation requirements for:- explosion protection zones- functional safety acc. to IEC 61508 8 Operator workstations in central control room Secured external data access through Virtual Private Network (VPN) and Remote Desktop Protocol (RDP)Fault-tolerantapplication server Fault-tolerant / fail-safe  automation systemsData archiveWeb portalbioliq®FlashPyrolysisbioliq®BiosyncrudeConditioning& Tank Farmbioliq®Entrained Flow Gasifierbioliq®DME & GasolineSynthesisOperator workstations in central control roomBRENDACombustionPilot PlantS7 417 HS7 417 FHS7 417 HS7 410 FHbioliq®GasTreatmentS7 417 FHStratus ftS 4500Siemens SPPA-T3000Process Control SoftwareRDP serverRouterKIT-NetVPN accessS7 417 FHS7 410 FHFirewallVPNbioliq VLANBernd Zimmerlin6 2022.09.19 Institute for Technical Chemistrybioliq® - fast pyrolysisMain features (feed wheat straw)Twin screw mixer reactor (500 °C)Heat transfer by sand in a heat carrier loopGas retention time ~ 1-2 secTwo-stage condensation(~ 90 °C / ~ 30 °C) Main productsStraw char (d90 < 100 µm) Organic condensateAqueous condensate 5/6-2015 19-2014 KW 49 2013020406080100Product yields / wt.%Test campaigns Organic condensate Aqueous condensate Solids (char+ash) Pyrolysis gasBernd Zimmerlin7 2022.09.19 Institute for Technical Chemistrybioliq® - fast pyrolysisMCycloneQuench CondenserIReactorElectrostatic precipitator Acoustic system for pipe cleaning ⇒ prevents pipes from clogging∆p over quench coolercleaning cycles6 hours Automated mechanical cleaning unit ⇒ removes caking deposits⇒ avoids critical pressure drops  Two spiral heat exchangers ⇒ avoids fouling by viscous,solid containing bio-oil (“self cleaning”) Picture by Alfa Laval Macerator keeps solids < 300 𝜇𝜇𝜇𝜇⇒ prevents blockages in quenchnozzles and pipingPictures by hoelschertechnic-gorator®Optimization of organic condensate loopBernd Zimmerlin8 2022.09.19 Institute for Technical ChemistryStable operation and representative product yield since 2015Substantial increase of straw throughput per week from< 5 t in 2012 up to > 40 t in 2018> 260 t of wheat straw processedFeedstock flexibility was proven in campaigns  > 18 t of miscanthusOrganic condensate with remaining solids, can be used in the bioliq® gasifier without further treatment Biosyncrude from aqueous condensate & straw char is being qualified as a fuel for the entrained flow gasifier bioliq® - fast pyrolysis,  status quo Bernd Zimmerlin9 2022.09.19 Institute for Technical Chemistrybioliq® - entrained flow gasifier (EFG)Bernd Zimmerlin10 2022.09.19 Institute for Technical Chemistrybioliq® - EFG, fuel specificationBernd Zimmerlin0,00,51,01,52,02,53,03,50,0 0,2 0,4 0,6 0,8 1,0 1,2H/C (molar ratio)O/C (molar ratio)GlycolGlycol + beechwood char Glycol + straw charGlyclol + beechwood charPyrolysis oilStraw charBeechwood charGlycol + beechwoodchar (25 wt%)Liquid Phase: Glycol as surrogate / model fuel  BioSyncrude: straw based pyrolysis oil  Wood based pyrolysis oil Solid phase: Coke: Straw and wood based Ash: straw / glass0,010,101,0010,00100,001.000,001,E-03 1,E-01 1,E+01 1,E+03ƞ / Pa s𝛾𝛾 ̇ /  s-1Biosyncrude 20°CBiosyncrude 40°CBiosyncrude 80°CEtylenglycol 20°CFuel specification: LCV 13 – 25 MJ/kg  Solid content < 30 %wt Ash content   3 - 10 %wt dp 90 % < 100 µm / max 1 mm Viscosity < 1 Pas (70°C)11 2022.09.19 Institute for Technical Chemistrybioliq® - entrained flow gasifier (EFG)Main featuresTwo membrane walls and burnersfor operation at 40 bar / 80 bar Alternative quench configurations(dip tube / spray quench)Load range 700 - 1000 kg/h slurry (LHV 13 - 25 MJ/kg)Slurry viscosity up to 1 Pas at 70 °CSpecial equipment for R&D: Optical access to reaction chamber Sequential cooling in membrane walls (5 segments) Extensive instrumentation & sampling possibilities for complete mass, species and energy balancesTypical syngas composition (vol.%, dry)H2 CO CO2 N2 CH428 - 33 28 - 37 18 - 27 12 - 18 < 0.1 - 0.3Bernd Zimmerlin12 2022.09.19 Institute for Technical Chemistrybioliq® - EFG Sub-processes – conversion of suspension fuelsdropletevaporationchar pyrolysischargasificationslag particleFuel O2 / SteamSyngasRANS: TU Clausthal / IEVB HydrocarbonsSoot, tarcharEvaporation DecompositionGas phaseVolatiles, fuel vapor, syngasLiquid phaseH2 CO2 H2OCOSyngasRecircu-lationSecondary pyrolysisAtomizationMixing of fuel and gasification mediumFast heating-upGasification reactionsOxidation reactionsGasification mediumN2 O2 H2OSyngasH2 CO CO2 H2OGasification mediumFuelPrimary charSecondary charAsh / SlagGas phaseBernd Zimmerlin13 2022.09.19 Institute for Technical ChemistryProcess  ControlSlag Controlbioliq® EFG5MW80 barFuel ConversionNumerical SimulationSlagO2 / SteamfuelProcess EfficiencyRaw SyngasMeasuring TechniquesHigh Pressure AtomizationPATEntrained Flow GasificationREGAbioliq® - EFG,  integrated research approachBernd Zimmerlin14 2022.09.19 Institute for Technical ChemistryEFG – pilot plant- PLS Siemens T3000 - THETIS web-Portal- Excel-InterfaceBalance bioliq - EFG process- Plausibility check of measured values- Consumption- / emission dataASPEN-Model (stationary)Balance bioliq - EFG reactor- unmeasured parameters- characteristic indicators / numbers- Plausibility check of measured valuesValidatedDatabase~ 500 raw databioliq® - EFG,  balancing toolsBernd Zimmerlin15 2022.09.19 Institute for Technical Chemistry    Energy Mass and SpeciesInput Output Slurry  Waste water Oxygen  Syngas Nitrogen  Slag Steam Natural gas Process water Cooling water  Cooling waterbioliq® - EFG,  balancesBernd Zimmerlin16 2022.09.19 Institute for Technical Chemistrybioliq® - EFG,  balancesExperiment: V26; 7.42 hSlurry 34: MEG + 25% wood coke + 5% straw ash; (767.9 kg/h) Input:  slurry,   O2,    N2,  steam,  natural gasMass: 2208 kg/hCarbon:               421 kg/hHydrogen:           108 kg/hOxygen:            1437 kg/hEnergy: 5195 kW Output: waste waterMass: 2430 kg/hHydrogen:      269 kg/hOxygen:     21690 kg/hEnergy: 106.3 kW(Slag: 30  kg/h)Input: process waterMass: 1947 kg/hHydrogen:  216 kg/hOxygen:    1731 kg/hEnergy: 11.4 kWOutput: syngasMass: 1568.5 kg/hCarbon:        433 kg/hHydrogen:      43 kg/hOxygen:       882 kg/hEnergy: 2882.5 kWBalances:Mass:  97.0 %Carbon: 102.9 %Hydrogen: 96.2 %Oxygen: 96.0 %Energy: 98.5 %Output: burner coolingEnergy: 12.3 kWOutput: cooling screenEnergy: 741 kWOutput: Waste heat syngas cooling:  48.8 kWWaste heat quench: 1141 kW Heat loss reactor surface:        50 kW17 2022.09.19 Institute for Technical Chemistrybioliq® - EFG,  balance inorganics11.4 kg Chlorine28.7 kg Calcium72.3 kg Potassium6.3 kg Magnesium115.4 kg Silicon5.4 kg Phosphorus0.91 kg Chlorine25.78 kg Calcium54.14 kg Potassium5.93 kg Magnesium108.70 kg Silicon4.58 kg Phosphorus9.91 kg Chlorine2.54 kg Calcium22.63 kg Potassium1.01 kg Magnesium5.57 kg Silicon0.0164 kg Phosphorus0.65 kg Chlorine2.11 kg Calcium0.07 kg Potassium0.27 kg Magnesium0.0974 kg Silicon0.0018 kg PhosphorusV43,  15,67hSlurry 53:           848,84 kg/h; 3,6 % AshProcess water: 1151,47 kg/hWaste water:     1654,9  kg/h                           Slag:                       375  kgBalances:Slag/Ash:   78.3 %Cl:              90.0 %Ca:             91.8 %K:             106.1 %Mg:           106.0 %Si:               98.9 %P:                89.4 %Bernd Zimmerlin18 2022.09.19 Institute for Technical ChemistryDevelop simulation tools / guidelines forAdaption of process parameters to varying fuel specificationsOptimization of gasifier operationVirtual Spray Test RigExperiment SimulationDesign Spec Simulation ToolDigital Twin EFGGasificationDevolatilizationEvaporationInert Heating/CoolingRight: Particle law100 µm 200 µm50 µmLeft: Carbon in cokeHigh carbon contentLow carbon contentBurner stabilityChar conversionSlag flowCold gas efficiencySyngas qualityTurn-down ratiobioliq® - EFG, simulation toolsBernd Zimmerlin19 2022.09.19 Institute for Technical Chemistry0 100 200 300 400Seg. 5Seg. 4Seg. 3Seg. 2Seg. 1Heat flux / kW/m²ExperimentRANS, w/oslagging modelRANS, slaggingmodelSeebold et al., Thermophysical and chemical properties of bioliq slags, Fuel, Vol.197, June 2017, Pages 596-604RANS: solidRANS: liquidAfter experimentGlycol + wood char ;  5 MW ;  40 bar ;  λtech = 0,56 ;   Tad = 2381 Kslagging and heat releasebioliq® - EFG, modeling/balancingBernd Zimmerlin20 2022.09.19 Institute for Technical ChemistrySlag layer on cooling screenbioliq® - EFG, experimentalslag layer thickness and heat flux V82  V83   Reduction of gasification temperature by 55 KBernd Zimmerlin21 2022.09.19 Institute for Technical ChemistryV82  V84   Doubling the amount of ash componentsbioliq® - EFG, experimentalslag layer thickness and heat flux Slag layer on cooling screenBernd Zimmerlin22 2022.09.19 Institute for Technical Chemistrybioliq® - EFG, optimization slag dischargeChallenge:Frequently cloggingat quench coneSolution:Adjust slag viscosity andflow temperature by: reactor temperature additivesAdjust thermal conditions at reactor outlet by:  slag amount quench coolingCaused by slag lumps Integration of a slag crusherBernd Zimmerlin23 2022.09.19 Institute for Technical Chemistry𝐑𝐑𝐑𝐑𝐑𝐑𝐑𝐑𝐑𝐑 𝐑𝐑 =𝐂𝐂𝐂𝐂𝐑𝐑 + 𝐌𝐌𝐌𝐌𝐑𝐑 + 𝐅𝐅𝐅𝐅𝟐𝟐𝐑𝐑𝟑𝟑 + 𝐍𝐍𝐂𝐂𝟐𝟐𝐑𝐑 + 𝐊𝐊𝟐𝟐𝐑𝐑𝐒𝐒𝐒𝐒𝐑𝐑𝟐𝟐 + 𝐑𝐑𝐀𝐀𝟐𝟐𝐑𝐑𝟑𝟑 + 𝐑𝐑𝐒𝐒𝐑𝐑𝟐𝟐bioliq® - EFG, optimization slag dischargeslag flow temperature vs. acidic-alkaline ratioBernd Zimmerlin24 2022.09.19 Institute for Technical ChemistryBernd Zimmerlinbioliq® - EFG,  slag structures25 2022.09.19 Institute for Technical Chemistrybioliq® - EFG,  development of diagnostic toolsExample: High Pressure Optical Borescope camera based systems for analysis of atomizationHigh Dynamic Range CameraHigh Speed Camera Gasifier flame at 40 barCooperation with KIT Institute for Applied Computer Science, IAIBernd Zimmerlin26 2022.09.19 Institute for Technical Chemistrybioliq® - EFG,  development of diagnostic toolsExample: High Pressure Optical Borescope camera based systems for analysis of atomizationHigh Dynamic Range CameraHigh Speed Camera Cooperation with KIT Institute for Applied Computer Science, IAIBernd ZimmerlinIncrease in the recording rate 50 fps  3500 fps (slow motion)Exposure time 30µs 27 2022.09.19 Institute for Technical ChemistryVersuchsnr. ʎ Brennstoff-leistungBrennstoff-mengeZerstäuber-dampfmenge ZD / BSDampf zu SauerstoffV107.1 Grundeinstellung0,45 4,5 MW 990 kg/h 199 kg/h 0,2 73,5 kg/h V107.2 0,45 4,5 MW 990 kg/h 100 kg/h 0,1 67,9 kg/hV107.3 0,55 4,5 MW 990 kg/h 199 kg/h 0,2 62,2 kg/hV107.4 0,55 3,5 MW 768 kg/h 155 kg/h 0,2 ~52 kg/hV107.5 Grundeinstellung0,45 4,5 MW 990 kg/h 199 kg/h 0,2 73,5 kg/hReduction of atomization steam about 50% 200 kg/h           100 kg/hExposure time 30µs,  Real Time 50 fpsAbel Inversion V107.1 (30µs)3500fpsAbel Inversion V107.2 (30µs)3500fpsReduction of the atomizing medium leads to higher radiation intensityAbeln Inversion  Averaging of light intensity over 1000 images, mirroring of the mean value images at the center axis.V107.1 V107.2Glycol + 4,5% A-Glass bioliq® - EFG,  development of diagnostic toolsCooperation with KIT Institute for Applied Computer Science, IAIExample: High Pressure Optical Borescope camera based systems for analysis of atomizationBernd Zimmerlin28 2022.09.19 Institute for Technical ChemistryIncrease of Lambda:   0,45  0,55Exposure time 30µsReal Time 50 fpsV107.1 V107.3Abel Inversion V107.1 (30µs)3500fpsAbel Inversion V107.3 (30µs)3500fpsIncrease of Lambda leads to lower radiation intensityCooperation with KIT Institute for Applied Computer Science, IAIVersuchsnr. ʎ Brennstoff-leistungBrennstoff-mengeZerstäuber-dampfmenge ZD / BSDampf zu SauerstoffV107.1 Grundeinstellung0,45 4,5 MW 990 kg/h 199 kg/h 0,2 73,5 kg/h V107.2 0,45 4,5 MW 990 kg/h 100 kg/h 0,1 67,9 kg/hV107.3 0,55 4,5 MW 990 kg/h 199 kg/h 0,2 62,2 kg/hV107.4 0,55 3,5 MW 768 kg/h 155 kg/h 0,2 ~52 kg/hV107.5 Grundeinstellung0,45 4,5 MW 990 kg/h 199 kg/h 0,2 73,5 kg/hGlycol + 4,5% A-Glass bioliq® - EFG,  development of diagnostic toolsExample: High Pressure Optical Borescope camera based systems for analysis of atomizationAbeln Inversion  Averaging of light intensity over 1000 images, mirroring of the mean value images at the center axis.Bernd Zimmerlin29 2022.09.19 Institute for Technical Chemistrybioliq® - EFG,  status quoSince 2013 about 1690 tons of different slurries processedat approximately 2250 hours of operation with different slurriesSlurry compositionsOrganic condensate of bioliq® fast pyrolysisWood based pyrolysis oilsEthylene glycol as model fuelWith different types of solids (wood- / straw char, ashes, glass)Ongoing optimization inFuel flexibilitySlagging behaviorOnline-diagnostics Bernd Zimmerlin30 2022.09.19 Institute for Technical Chemistrybioliq® - hot gas cleaningMain features HTHP gas cleaningOperation up to 80 bar and up to 800 °CLoad range 700 Nm³/h Syngas (2 MWth)Ceramic filter candles, mounted horizontallyRe-cleaned by Couple-Pressure-Pulse (CPP)Fixed bed sorption for sour gases, alkali and heavy metalsCatalyst bed for N-species and hydrocarbons decompositionChallengesMeet extremely low target levels of contaminants (< 0.1 mg/m³ STP)for catalytic syngas conversionLong term operation behaviorFilterSyngas fromGasifierSyngas toSynthesisSorption CatalystBernd Zimmerlin31 2022.09.19 Institute for Technical Chemistrybioliq®- hot gas cleaning,  reactor designFunctional Separation ofHigh-Temperature and  High-PressureSyngas-tubes (inside)max. temperature       800 °Clow overpressure        0.5 barPressure Vessel (outside)max. temperature      350 °Cmax. overpressure      85 barChallengeConnections of syngas-tubes are not absolutely gas tightAvoidance of syngas-bypass-flowthrough insulationMaximum bypass-flowCraw gas ≈ 200 ppmVCclean gas < 0.1 ppmVE = 100 % (supposed)𝒃𝒃𝒃𝒃𝒃𝒃𝒃𝒃𝒃𝒃𝒃𝒃 𝒇𝒇𝒇𝒇𝒇𝒇𝒇𝒇𝒕𝒕𝒇𝒇𝒕𝒕𝒃𝒃𝒇𝒇 𝒇𝒇𝒇𝒇𝒇𝒇𝒇𝒇< 𝟎𝟎.𝟏𝟏𝟐𝟐𝟎𝟎𝟎𝟎= 𝟎𝟎,𝟎𝟎𝟎𝟎 %Fixed BedSorptionFixed Bed CatalysisBernd Zimmerlin32 2022.09.19 Institute for Technical Chemistrybioliq® - hot gas cleaning,  status quoRequired purity specifications for sour gases achieved with fixed bed adsorption at 700 °C / 400 °C Online-gas-analysis for S, Cl and Nspecies proofed (clean and raw gas side)Ongoing workInvestigation of different HTHP-sorbents mixtures with improved measurement technologyConstruction and commissioning of a dry entrained flow adsorption for continuous operationFilterSyngasfromGasifierSyngasSorptionEntrained flowsorptionCatalystCatalytic Ceramic FilterSyngasfromGasifierSyngasEntrained flowsorptionBernd Zimmerlin33 2022.09.19 Institute for Technical ChemistryMain featuresOperation up to 60 barLoad range 700 Nm³/h Syngas (2 MWth)One step DME synthesis, operated at 240 - 250 °C (Vcatalyst = 1000 liters)Gasoline synthesis, operated at 350 - 370 °C (Vcatalyst = 600 liters)bioliq® - fuel synthesisEmpty and filled reactor/heat-panel bedsBernd Zimmerlin34 2022.09.19 Institute for Technical Chemistrybioliq® - fuel synthesis,   productRaw Gasoline Rectificationtop-productRectificationbottom-productRaw Gasoline-MixBernd Zimmerlin35 2022.09.19 Institute for Technical ChemistryRevision of both reactors in 2017 for improved temperature and residence time behavior⇒ CO conversion increased by a factor of 2.5 Production of 5200 l bio-based raw gasoline in 830 h (8 campaigns) since Nov / Dec 2017Syngas bottling (200 bar) for external applicationsApplication tests of different fuel blends:reFuels project in Baden-Württembergstate with automotive industry, oil refinery Syngas bottlingbioliq® - fuel synthesis,   status quoBernd Zimmerlin36 2022.09.19 Institute for Technical Chemistrybioliq® pilot plant  - next stepsAfter proof of concept has been achieved in 2017, work is focused on efficiency improvement and further development of process componentsContinued R&D activities within HGF-research program, national and international projects (20 Phd works ongoing):Feedstock flexibility and process efficiencyScalability from lab- to pilot- to commercial scaleDevelopment of concepts for process implementation, including CO2 utilization by external hydrogen productionBack bone of EnergyLab 2.0 at KIT for Energy Transition in GermanyBernd Zimmerlin37 2022.09.19 Institute for Technical Chemistrybioliq®  www.bioliq.deThanks to…• funding agencies and institutions• partners from industry and academia• the teams from KIT• …and to the audiencecontact:Bernd ZimmerlinKarlsruhe Institute for TechnologyInstitute for Technical Chemistryphone: +49 721 608 24116mail: bernd.zimmerlin@kit.eduL. TkotzInvestition in die Zukunft gefördert durch die Europäische Union Europäischer Fonds für regionale Entwicklung und das Land Baden-Württemberg

Operations of the bioliq® pilot plant - entrained flow gasification in 5 MW pilot scale

https://publikationen.bibliothek.kit.edu/1000151172/149393044

Operations of the bioliq® pilot plant - entrained flow gasification in 5 MW pilot scale

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