The aim of the present study is to investigate the production of biochar from anaerobic digestion (AD) digestate. Re-Cord selected digestate from real and representative (regarding the scale and the process technology) anaerobic digestion plant.
Please click on the file below for full content of the abstract

Bettucci, Lorenzo

Casini, David

Chiaramonti, David

Lotti, Giulia

Miliotti, Edoardo

Prussi, Matteo

Rizzo, Andrea Maria

English

Engineering Conferences International

Engineering Conferences InternationalECI Digital ArchivesBiochar: Production, Characterization andApplications Proceedings8-20-2017Lab-scale pyrolysis and hydrothermalcarbonization of biomass digestate:Characterization of solid productsEdoardo MiliottiCREAR/Department of Industrial Engineering, University of Florence, ItalyDavid CasiniRE-CORD Renewable Energy Consortium for R&D, Florence, ItalyMatteo PrussiRE-CORD Renewable Energy Consortium for R&D, Florence, ItalyGiulia LottiRE-CORD Renewable Energy Consortium for R&D, Florence, ItalyLorenzo BettucciRE-CORD Renewable Energy Consortium for R&D, Florence, ItalySee next page for additional authorsFollow this and additional works at: http://dc.engconfintl.org/biocharPart of the Engineering CommonsThis Abstract and Presentation is brought to you for free and open access by the Proceedings at ECI Digital Archives. It has been accepted for inclusionin Biochar: Production, Characterization and Applications by an authorized administrator of ECI Digital Archives. For more information, pleasecontact franco@bepress.com.Recommended CitationEdoardo Miliotti, David Casini, Matteo Prussi, Giulia Lotti, Lorenzo Bettucci, Andrea Maria Rizzo, and David Chiaramonti, "Lab-scalepyrolysis and hydrothermal carbonization of biomass digestate: Characterization of solid products" in "Biochar: Production,Characterization and Applications", Franco Berruti, Western University, London, Ontario, Canada Raffaella Ocone, Heriot-WattUniversity, Edinburgh, UK Ondrej Masek, University of Edinburgh, Edinburgh, UK Eds, ECI Symposium Series, (2017).http://dc.engconfintl.org/biochar/54AuthorsEdoardo Miliotti, David Casini, Matteo Prussi, Giulia Lotti, Lorenzo Bettucci, Andrea Maria Rizzo, and DavidChiaramontiThis abstract and presentation is available at ECI Digital Archives: http://dc.engconfintl.org/biochar/54Lab‐scale pyrolysis and hydrothermal carbonization of biomass digestate: characterization of solid productsChiaramonti DavidMiliotti E., Casini D., Lotti G., Bettucci L., Pennazzi S., Rizzo A. M. Biochar: Production, Characterization and ApplicationsAugust 20‐25, 2017, Hotel Calissano, Alba, ItalyBiochar: Production, Characterization and Applications, August 20‐25, 2017, Alba, ItalySummary2 Feedstock: the digestate Experimental units: Slow Pyrolysis reactor and Micro‐HTC Process conditions of thermochemical experiments Char analysis results Comparison with EBC, IBI, Italian fertilization decree Complementary analyses: HTC liquid phase ConclusionBiochar: Production, Characterization and Applications, August 20‐25, 2017, Alba, ItalyOrigin:• Anaerobic digestion plant in Grosseto, Italy• Mesophilic conditions (~40˚C)• Fed mainly with barley silage (60%), but also with wheat and herbaceous silage and poultry manureTreatments:• Mechanical separation  75% w/w water contentAnalyses:• CHN, S, ash,  higher heating value, inorganics, BET, pH3Feedstock: The digestateBiochar: Production, Characterization and Applications, August 20‐25, 2017, Alba, Italy 4Experimental unit: Pyrolysis reactor• Continuous reactor operated in batch mode• Gross reactor volume: 31 l• Electric heating system• Inner stirring system• Constant N2 flow under suctionCharBiochar: Production, Characterization and Applications, August 20‐25, 2017, Alba, Italy 5Experimental unit: Micro‐reactor test‐bench MRTB• Custom‐made test‐bench• Batch reactor: 27ml• P and T sensors• Fluidized sand bath• Shaking deviceReactorBiochar: Production, Characterization and Applications, August 20‐25, 2017, Alba, ItalyOperating conditions Slow Pyrolysis HTCPretreatment Drying Drying, millingDigestate input 1 kg_DM 2 g_DMTemperature 500°C 200‐250°CTime 1 h 0.5‐3 hBiomass/water ratio ‐ 10 wt%6Thermochemical batch experimentsBiochar: Production, Characterization and Applications, August 20‐25, 2017, Alba, ItalyParameter Value NormMoisture content [wt% w.b.] 76.2 UNI 13040Ash content [wt%] d.b. 9.3 UNI 13039Volatile matter [wt%] d.b. 68.9 UNI 15148Fixed carbon [wt%] d.b. 21.8 CalculatedC [wt%] d.b. 46.71 UNI 15104H [wt%] d.b. 5.50 UNI 15104N [wt%] d.b. 1.15 UNI 15104S [wt%] d.b. 0.46 Internal methodO [wt%] d.b. 36.88 CalculatedK [wt%] d.b. 0.97 UNI EN 15290P [wt%] d.b. 0.28 UNI EN 15290Higher Heating Value [MJ/kg] d.b. 19.24 UNI 14918Lower Heating Value [MJ/kg] d.b. 17.95 UNI 14918pH [‐] 7.7 DIN ISO 10390Surface area [m2/g] 3.72 ASTM D 6556‐10Total pore volume [cm3/g] 1.10∙10‐2 ASTM D 6556‐10Average pore diameter [nm] 11.61 Calculated7Feedstock characterizationBiochar: Production, Characterization and Applications, August 20‐25, 2017, Alba, Italy 8ResultsBiochar: Production, Characterization and Applications, August 20‐25, 2017, Alba, ItalySolid yield & C content• Slow Pyrolysis: Solid yield 33.1 wt%; Carbon content 64.3 wt% db• Hydrothermal Carbonization: Effect of reaction severity increase (T, t)• Decrease in solid yield from 72.6 to 51.0 wt% db• Increase in carbon content from 49.7 to 62.9 wt% db• Trade‐off: Quantity VS Quality9Char analysis resultsHydrochar PyrocharBiochar: Production, Characterization and Applications, August 20‐25, 2017, Alba, ItalyElemental analysis values are on dry basis• Comparison between  digestate, hydrochar with highest C% (250˚C‐3h) and pyrocharDifferent char quality: Pyrochar has lower O/C & H/C molar ratio10Char analysis resultsH. Huang, S. Wang, K. Wang, M.T. Klein, W.H. Calkins, A. Davis, Thermogravimetric and Rock‐Eval studies of coal properties and coal rank, Energy and Fuels. 13 (1999) 396–400. doi:10.1021/ef980088q.Biochar: Production, Characterization and Applications, August 20‐25, 2017, Alba, ItalyPyrochar: Polycyclic Aromatic Hydrocarbons• DIN CEN TS 16181: Soxhlet-extraction with toluene and determination with HPLCChar analysis results11PAHs ppm dbAcenaphthene 0.07Acenaphthylene 0.00Anthracene  0.04Benz(a)anthracene  0.00Benzo(a)pyrene 0.00Benzo(b)fluoranthene 0.00Benzo(ghi)perylene 0.00Benzo(k)fluoranthene 0.06Chrysene  0.53Dibenz(a,h)anthracene  0.02Fluoranthene 0.00Fluorene 0.28Indeno(1,2,3‐cd)pyrene 0.17Naphthalene  0.26Phenanthrene 0.16Pyrene 0.89TOTAL PAHs 2.47Sample Surface area Average pore diameterTotal pore volume[m2/g] [nm] [cm3/g]Digestate 3.72 11.61 1.1∙10‐2Hydrochar 250‐3 4.92 16.50 2.0∙10‐2Pyrochar 23.10 14.80 8.5∙10‐2BET analysisPyrochar: pH‐Value 9.4Biochar: Production, Characterization and Applications, August 20‐25, 2017, Alba, ItalyInorganic elements12Char analysis resultsElement[mg/kg] Al B Ba Ca Cd Cr Cu Fe K Mg Mn Mo Na P Si Ti V ZnDigestate 339 7.9 21 8315 2.9 3.1 7.2 387 9656 1224 70 7.6 1962 2751 812 9.7 2.9 41Hydrochar 250‐3  720 4 26 11480 8.7 bdl 21 820 364 1850 125 bdl 73 7100 718 34 bdl bdlPyrochar 672 114 59 21397 21 63 143 1470 28170 4877 204 22 5752 10030 2179 47 3.6 bdlbdl= below detection limit, 0.1 mg/kgHTC Slow PyrolysisBiochar: Production, Characterization and Applications, August 20‐25, 2017, Alba, ItalyParameter Hydrochar 250‐3 Pyrochar EBC IBI D.L. 29 APRILE 2010, N. 75Carbon content [% w/w] d.b. 62.85 64.34 Not requiredClass 1: >=60Not requiredClass 2: >=30 & <60Class 3: >=10 & <30Total organic carbon [% w/w] d.b. n.m. n.m. >=50 Not requiredClass 1: >60Class 2: >30 & <=60Class 3: >=20 & <=30Ash content [% w/w] d.b. 12.3 24.6 Declaration DeclarationClass 1: <10Class 2: >=10 & <=40Class 3: >40 & <=60H/Corg 1.06 0.5 <=0.7 <=0.7 <=0.7O/Corg 0.2 0.07 <=0.4 Not required Not requiredpH ‐ Value n.m. 9.4 Not required Not required 4‐12Granulometry through 0.5mm[% w/w] d.b. n.m. 71.2 Declaration Declaration DeclarationSurface area [m2/g] 4.9 23.1 Declaration;better >150m2/g Declaration DeclarationPAHs [mg/kg] d.b. n.m. 2.47Premium: <46‐300 <6Basic: >4 & <12Comparison with European and International biochar standards13Char analysis resultsCalc. with Ctot not Corgn.m.: not measuredInternational Biochar Initiative, Standardized Product Definition and Product Testing Guidelines for Biochar That Is Used in Soil, (2014); European Biochar Foundation (EBC), European Biochar Certificate ‐ Guidelines for a SustainableProduction of Biochar, (2016); Decreto Legislativo 29 aprile 2010, n.75: “Riordino e revisione della disciplina in materia di fertilizzanti, a norma dell’artico‐lo 13 della legge 7 luglio 2009, n. 88”, Gazzetta Ufficiale, 2010Biochar: Production, Characterization and Applications, August 20‐25, 2017, Alba, ItalyComparison with European and International biochar normative: ContaminantsValues in [mg/kg] d.b.nm: not measured Element DigestateHydrochar 250‐3 Pyrochar EBC IBID.L. 29 APRILE 2010, N. 75Cd 2.9 8.7 21Basic: <1.51.4‐39 <1.5Premium: <1Cr 3.1 <0.1 63Basic: <9064‐1200 <0.5 (hexavalent)Premium: <80Co <0.1 <0.1 <0.1 Not required 40‐150 Not requiredCu 7.2 21 143Basic: <10063‐1500 <230Premium: <100Pb <0.1 <0.1 <0.1Basic: <15070‐500 <140Premium: <120Mo 7.6 <0.1 22 Not required 5‐20 Not requiredZn 41 <0.1 <0.1Basic:  <400200‐7000 <500Premium: <40014Char analysis resultsInternational Biochar Initiative, Standardized Product Definition and Product Testing Guidelines for Biochar That Is Used in Soil, (2014); European Biochar Foundation (EBC), European Biochar Certificate ‐ Guidelines for a SustainableProduction of Biochar, (2016); Decreto Legislativo 29 aprile 2010, n.75: “Riordino e revisione della disciplina in materia di fertilizzanti, a norma dell’artico‐lo 13 della legge 7 luglio 2009, n. 88”, Gazzetta Ufficiale, 2010Biochar: Production, Characterization and Applications, August 20‐25, 2017, Alba, ItalyInorganic elements15HTC Aqueous phaseElement [mg/kg] Al B Ba Ca Cd Cu Fe K Mg Mn Mo Na P Si Ti ZnDigestate 339 7.9 21 8315 2.9 7.2 387 9656 1224 70 7.6 1962 2751 812 9.7 41Hydrochar 250‐3 720 4 26 11480 8.7 21 820 364 1850 125 bdl 73 7100 718 34 bdlLiquid phase 250‐3 0.3 1.5 1.4 172 1.3 0.2 7.4 1153 117 1.7 0.2 249 bdl 362 1.6 1.9bdl= below detection limit, 0.1 mg/kg• Increase in reaction severityincreases inorganic concentration• Temperature impacts more thantime• Ca, Mg, P end up in hydrochar• K in liquidBiochar: Production, Characterization and Applications, August 20‐25, 2017, Alba, Italy0 10 20 30 400.05.0x1041.0x1051.5x1052.0x1050 10 20 30 400.05.0x1041.0x1051.5x1052.0x1052.5x1053.0x1050 10 20 30 400.02.0x1054.0x1056.0x1058.0x1051.0x1061.2x1060 10 20 30 400.05.0x1041.0x1051.5x1052.0x1052.5x1053.0x1053.5x1054.0x1050 10 20 30 400.05.0x1051.0x1060 10 20 30 400.05.0x1051.0x1060 10 20 30 400.05.0x1051.0x1060 10 20 30 400.05.0x1051.0x106Ret.TimeRet.TimeRet.TimeRet.Time200-0.5-10SC200-3-10SCRet.Time250-3-10SC250-0.5-10SCGas chromatography ‐mass spectrometry (GC‐MS) – DCM extract16HTC Aqueous phaseReaction severityFurfuralGuaiacolSyringol200‐0.5200‐3250‐0.5250‐3Biochar: Production, Characterization and Applications, August 20‐25, 2017, Alba, ItalyHPLC (High Performance Liquid Chromatography) values are measured in g/lHTC Aqueous phase17Aqueous phase Acetic acid Furfural HMF200‐0.5 0.65 0.16 <0.025200‐3 1.72 0.21 <0.025250‐0.5 2.68 <0.025 <0.025250‐3 3.26 <0.025 <0.025• Acetic acid concentration increases with severity• Furfural slightly increases with time only at 200˚C• HMF always below detection limitBiochar: Production, Characterization and Applications, August 20‐25, 2017, Alba, ItalyGas chromatography ‐ Flame Ionization Detector (GC‐FID) – DCM extract18HTC Aqueous phaseBiochar: Production, Characterization and Applications, August 20‐25, 2017, Alba, Italy 19ConclusionBiochar: Production, Characterization and Applications, August 20‐25, 2017, Alba, ItalyCONCLUSIONS• Digestate was successfully converted into char by SP and HTC• HTC: temperature has a greater effect on char yield & C content than time (quantity VS quality)• Pyrochar: better quality than hydrochar due to more extended carbonization (similar C content, but lower O/C & H/C molar ratio)• Very low surface area for both chars (pyrochar 1 OM higher)• Pyrochar: almost all investigated inorganics increased in concentration; Hydrochar: lower increase and major dilution (K)• Many hydrochar and pyrochar properties met most biochar standards• By increasing reaction severity, the concentration of acetic acid, guaiacols, syringol, ketones and phenols increase in HTC aqueous phaseFUTURE WORKS• Anaerobic digestion of HTC aqueous phase• Increase of pyrochar surface area through physical or chemical activationAcknowledgment• Ministry for Agriculture (MIPAAF) – AGROCHAR Project20Conclusions and future worksdavid.chiaramonti@unifi.itThank you for your attention!Edoardo MiliottiDavid CasiniGiulia LottiLorenzo BettucciSilvia PennazziAndrea Maria RizzoDavid ChiaramontiLAB‐SCALE PYROLYSIS AND HYDROTHERMAL CARBONIZATION OF BIOMASS DIGESTATE: CHARACTERIZATION OF SOLID PRODUCTSChiaramonti DavidMiliotti E., Casini D., Lotti G., Bettucci L., Pennazzi S., Rizzo A. M. Biochar: Production, Characterization and ApplicationsAugust 20‐25, 2017, Hotel Calissano, Alba, ItalyBiochar: Production, Characterization and Applications, August 20‐25, 2017, Alba, ItalySlow Pyrolysis experiments Preliminary TGA Minimum obtainable solid residue 27.8% w/w d.b. at 900˚C Biochar: Production, Characterization and Applications, August 20‐25, 2017, Alba, ItalySlow Pyrolysis experiments24Experiment mode BatchFeedstock [g] 1074Reactor heater temperature [°C] 600Gas‐line heater temperature [°C] 550Mean reactor temperature [°C] 506Holding time [h] 1Nitrogen flow [l/min] 5.0Stirring system ActiveMean heating rate [°C/min] 7Biochar: Production, Characterization and Applications, August 20‐25, 2017, Alba, ItalyHydrothermal carbonization experiments25T [°C] Time [h] B/W db [w/w] P0 [bar] HR mean [°C/min] T mean [°C] Pfin‐P0 [bar]200 0.5 10% 20.15 33.96 201.27 0.99200 3.0 10% 20.40 33.46 201.21 0.67250 0.5 10% 45.23 42.97 251.49 1.41250 3.0 10% 45.23 40.86 250.80 2.63Biochar: Production, Characterization and Applications, August 20‐25, 2017, Alba, ItalyHTC Product recovery and GC analyses methodology26

Lab-scale pyrolysis and hydrothermal carbonization of biomass digestate: Characterization of solid products

https://dc.engconfintl.org/cgi/viewcontent.cgi?article=1030&amp;context=biochar

Lab-scale pyrolysis and hydrothermal carbonization of biomass digestate: Characterization of solid products

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