O objetivo deste trabalho foi estudar a aplicação de reator anaeróbio serial (RAS) no processamento de vinhaça de cana-de-açúcar para a remoção de matéria orgânica e produção de biogás, submetido ao aumento gradativo de carregamento orgânico. Para tanto, foi utilizado um reator composto por quatro câmaras em série denominadas C1, C2, C3 e C4, com capacidade de 5 L cada, totalizando um volume de 20 L. A primeira etapa do trabalho (Etapa 1) consistiu na operação e monitoramento do reator RAS partindo-se da aplicação da carga orgânica volumétrica (COV) de 0,5 kg DQO m-3.d-1 até a obtenção da COV de 2,5 kg DQO m-3.d-1. Na segunda etapa (Etapa 2) foram operados reatores em batelada sequencial, simulando a operação contínua do reator RAS, visando estudar o efeito do aumento de taxas de carregamento orgânico aplicado. O reator RAS operou sob baixos valores de COVglobal e COALglobal aplicados na Etapa 1, obtendo-se máximas de 2,50 kg DQO m-3.d-1 e 0,167 kg STV m-3.d-1, respectivamente. Os resultados obtidos da Etapa 1 indicam satisfatória remoção global média de matéria orgânica na forma de DQO, superiores a 90 %, propiciada pela adaptação da biomassa ao longo dos reatores sequenciais. O metano apresentou-se como o gás predominante na composição do biogás produzido, com valores acima de 75 %, que confirmam o estabelecimento do sistema metanogênico pleno. Em todos os compartimentos dos reatores sequenciais verificou-se maior abundância relativa para os domínios Archaea e Bacteria os gêneros Methanosaeta, produtores de metano e, T78, responsável pela degradação de açúcares, respectivamente. Principalmente para os reatores C3 e C4, observou-se adaptação de algumas populações para ambos os domínios Bacteria e Archaea indicado pelo menor índice de diversidade e aumento da dominância. O aumento das taxas de carregamento orgânico aplicado ao lodo, estipuladas nos ensaios em batelada na Etapa 2, propiciou o aumento dos valores de carga orgânica aplicada para todos os reatores. Com o aumento do carregamento orgânico aplicado, observa-se o aumento e acúmulo de ácidos orgânicos para todas as fases dos ensaios, principalmente o acético. A produção de metano foi significativa na operação dos reatores em batelada, principalmente em C1. De forma geral, os resultados obtidos demonstraram o bom desempenho do processamento da vinhaça de cana-de açúcar em reator compartimentado tipo RAS para a remoção de matéria orgânica e produção de biogás. / The aim of this study was to investigate the application of an anaerobic serial reactor (ASR) in the sugarcane stillage processing for the removal of organic matter and biogas production, submitted to the gradual increase in organic loading rate. ASR reactor consisted of four reactors operated in series (C1, C2, C3 and C4), each with a reaction volume of 5 L (total volume of 20 L). The first step (Step 1) consisted of reactor operation and monitoring; organic loading rate was gradually increased from 0.5 kg COD m-3d-1 up to 2.5 kg COD m-3 d-1. In the second step (Step 2), sequential batch reactors were operated, simulating the continuous ASR reactor operation, aiming to study the effect of the increase of organic load applied to sludge (OLS). The ASR reactor operated under low values of COVglobal and COALglobal applied in Step 1, obtaining a maximum 2.50 kg COD m-3d-1 and 0.167 kg TVS/m-3d-1, respectively. The results obtained from Step 1 indicated satisfactory removal of the global average organic matter in the form of COD more than 90 %, caused by adaptation of the biomass along the sequential reactors. Methane appeared to be the predominant gas in biogas composition, with values above 75%, which confirmed the establishment of the full methanogenic system. In all compartments of the sequential reactors, there was a higher relative abundance for the domains Archaea and Bacteria of the genera Methanosaeta, methane producers, and T78, which is responsible for degradation of sugars, respectively. Especially for the reactors C3 and C4, the adaptation of some populations for both domains Bacteria and Archaea indicated was observed by the lower diversity index and increase in dominance. The increase of the organic loading rates applied to the sludge, as established in the batch tests, increased the organic load values applied to all reactors. With the increase of organic loading applied, an increase in the accumulation of organic acids, mainly acetic, for all stages and the batch tests. Methane production was significant in the operation of batch reactors, mainly in the C1. In general, the results obtained showed good performance of the processing of the sugarcane stillage in serial reactor (ASR) for the removal of organic matter and biogas production.

Com o propósito de explorar o potencial de geração de metano a partir de vinhaça de cana-de-açúcar e propor procedimentos de controle do processo anaeróbio, foi utilizado um reator UASB (Upflow Anaerobic Sludge Blanket) em escala piloto, equipado de separador gás-sólido-líquido modificado e sem recirculação de efluente. A unidade foi inoculada com lodo granular e utilizou-se substrato concentrado (DQO de 20 g.L-1) para sua alimentação. O reator foi submetido a cargas orgânicas volumétricas (COV) de 0,7 a 7 KgDQO.m-3.d-1, durante 300 dias de operação. O procedimento operacional baseou-se no aumento de carga por escalonamento da vazão de alimentação em função da manutenção de variação inferior a 10% para a eficiência do sistema. Para o tamponamento da vinhaça de alimentação, no início da operação utilizou-se 1g NaHCO3.g-1DQOafluente, com redução gradativa até 0,125g NaHCO3.g-1DQOafluente. O monitoramento do desempenho do processo anaeróbio se deu pela avaliação dos parâmetros: eficiência de remoção de DQO, pH, alcalinidade, ácidos voláteis, razão alcalinidade intermediária/alcalinidade parcial, razão Prop:Ac, vazão de metano e porcentagem de metano no biogás. O reator UASB apresentou valor médio de eficiência de remoção de DQO de 92±4,4%, para cargas aplicadas entre 0,7 e 4,8 KgDQO.m-3.d-1. A maior produção média de metano observada durante o período operacional foi 5 m3CH4.m-3 de vinhaça aplicada para cargas orgânicas entre 4,1 e 5,6 KgDQO.m-3.d-1. A produção de biogás apresentou valor médio de metano de 70±7% para 1 a 5,6 Kg DQO.m-3.d-1. A operação do reator com cargas aplicadas acima de 5,6 KgDQO.m-3.d-1 gerou menor produção de biogás, redução na porcentagem de metano e aumento da carga de ácidos voláteis efluente, assim como queda na eficiência de remoção de DQO. Devido ao acréscimo de carga (0-2 para 4-6 KgDQO.m-3.d-1), a variação da concentração para cada tipo de ácido foi: acético (56±70 para 216±121 mg.L-1), propiônico (26±28 para 165±150 mg.L-1) e butírico (4±7 para 60±18 mg.L-1). Notou-se que a relação entre as concentrações de ácido propiônico e ácido acético (razão Prop:Ac) pode ser utilizada como parâmetro de monitoramento da estabilidade do reator. A elevação de COV de 3,9 a 6,4 KgDQO.m-3.d-1acarretou alteração na razão Prop:Ac de 0,8 a 1,75, corroborando descontroles do processo anaeróbio associado à queda de eficiência na geração de metano. / In order to explore the potential of methane generation from sugarcane vinasse and propose procedures for the anaerobic process control, was utilized a pilot scale UASB reactor (Upflow Anaerobic Sludge Blanket), equipped with modified gas-solid-liquid separator and without recirculation of effluent. The unit was inoculated with granular sludge and concentrated substrate was used (COD 20 g.L-1) for feeding. The reactor was submitted to volumetric organic load (VOL) from 0.7 to 7 KgCOD.m-3.d-1, during 300 days of operation. The reactor operation was based on the increase of load by staggering the feed flow in function of the maintenance of variation lower than 10% for the system efficiency. For buffering the feedings vinasse was used 1g NaHCO3.g-1CODinfluent at the beginning of the operation, with gradual reduction to the value of 0.125 g NaHCO3.g-1CODinfluent. The monitoring of the anaerobic process performance was due to the evaluation of the following parameters: efficiency of COD removal pH, alkalinity, intermediate alkalinity/partial alkalinity ratio; Prop:Ac ratio, methane flow and percentage of methane in the biogas. The UASB reactor demonstrated a COD average removal efficiency of 92±4.4%, to applied loads between 0.7 and 4.8 KgCOD.m-3.d-1. The highest average methane production observed during the operational period was 5 m3CH4.m-3 of vinasse applied for organic loads between 4.1 and 5.6 KgCOD.m-3.d-1. The biogás production demonstrated a methane average of 70±7% for 1 to 5.6 KgCOD.m-3.d-1. The reactor operation with loads up to 5.6 KgCOD.m-3.d-1 caused lower production of biogas, reduction in the percentage of methane and increase for effluent volatile acids load, as well as decrease of COD removal efficiency. Due to the additional load (0-2 to 4-6 KgCOD.m-3.d-1), the change in concentration for each type of acid was: acetic acid (56±70 to 216±121 mg.L-1), propionic acid (26±28 to 165±150 mg.L-1) and butyric acid (4±7 to 60 ± 18 mg.L-1). It was noted that the relationship between the concentrations of propionic acid and acetic acid (ratio Prop:Ac) may be used as a monitoring parameter of the reactor stability. The increase in VOL of 3.9 to 6.4 KgCOD.m-3.d-1 caused change in the Prop:Ac ratio of 0.8 to 1.75, confirming the upsets on the anaerobic process associated with efficiency drop in methane generation.

Accélérer la dégradation anaérobie des déchets enfouis, optimiser la production de biogaz et diminuer le temps et le coût de surveillance sont les enjeux principaux d'installation de stockage des déchets non dangereux (ISDND)-bioactives, ainsi que, plus classiquement, minimiser leurs impacts sanitaires et environnementaux. L'une des méthodes les plus efficaces pour atteindre ces objectifs est la recirculation de lixiviat et l'augmentation de l'humidité des déchets. Les objectifs du bioréacteur ne seront pas atteints sans une connaissance rationnelle des phénomènes hydrauliques, biologiques et thermiques qui s’y développent et de l’influence de l'un de ces phénomènes sur les autres. Les observations in situ, les expérimentations en laboratoire ainsi que les modèles numériques permettent ensemble une approche rationnelle de ces phénomènes. C’est ce qui constitue le corps de ce travail de thèse, où nous avons étudié le comportement hydro-thermo-biologique des déchets dans la phase anaérobie en laboratoire, sur site à partir de données hydro-thermiques de deux bioréacteurs situés en France et en développant un modèle numérique pour simuler ce comportement couplé des bioréacteurs. Les travaux en laboratoire nous ont permis d’étudier l’effet de la saturation et de la densité (compactage des déchets) sur la dégradation anaérobie des déchets ménagers et l’influence de ces paramètres sur la production de biogaz. Les données hydrauliques et thermiques in-situ des bioréacteurs nous ont permis de connaître les variations des paramètres essentiels comme la température et la saturation dans les déchets, à différentes profondeurs, et estimer d’autres paramètres qui sont difficile à déterminer expérimentalement. Le modèle numérique nous a permis d’étudier le comportement couplé, hydro-thermo-biologique, des bioréacteurs à long terme (pendant une dizaine d’années) aussi bien qu’à court terme pendant la recirculation de lixiviat. L’interdépendance des différents paramètres qui influent la dégradation des déchets est la principale raison nous ayant conduits à développer un modèle de couplage qui nous permette d'étudier chaque paramètre en fonction des autres. Les travaux en laboratoire et les données thermiques de site nous ont conduits à développer un modèle d'écoulement diphasique du liquide et du gaz dans les déchets, considérant les phénomènes biologiques, en fonction des paramètres clés de la dégradation comme la température et la saturation, pour aboutir à la production de biogaz et de chaleur. Les trois parties de ce travail, les expérimentations en laboratoire, le développement d'un modèle numérique et l’analyse des données de site ont été effectuées en parallèle de façon complémentaire. Les expérimentation de laboratoire tout comme l’analyse des données de site, nous ont montré l'importance des paramètres qu'il faut considérer dans le modèle et en retour le modèle numérique nous a aidé à diriger les expérimentations en laboratoire et montré la nécessité de conduire certaines analyses sur les pilotes expérimentaux, comme l’analyse de la biomasse, de la DCO et des AGV. L'analyse des données hydrauliques et thermiques de sites de bioréacteur nous a permis de caler les paramètres hydrauliques, biologiques et thermiques des déchets qui sont difficile à définir sur le site sans le perturber (comme la conductivité hydraulique, la saturation, la conductivité thermique, la capacité calorifique, la concentration en biomasse et en AGV). Le travail réalisé dans la thèse a permis de développer un modèle couplé hydro-thermo-biologique et de tester sa capacité à prévoir le comportement thermique d'un bioréacteur, la production totale et le taux de production de méthane. Nous avons montré qu'il était adopté à l'étude du comportement à long terme d'un bioréacteur, aussi bien qu'à court terme pendant la réinjection de lixiviat, là où les techniques de mesure et le temps sont limitants en laboratoire ou sur site / The main objectives of bioreactor landfills are to accelerate anaerobic degradation of waste in order to minimize the environmental impacts, to optimize biogas production and to minimize the time of waste stabilization as well as the costs and time of monitoring of landfill sites after operation. One of the most important and cost-effective method to achieve these objectives is liquid addition and management. The objectives of bioreactor landfills could not be achieved without enough knowledge of its hydraulic, thermal and biological parameters and processes and the effects of each of them on the others. Site observations and data and laboratory experiments as well as numerical models could help to develop the knowledge of these phenomena and processes, which is the objective of this work. In this thesis we study the coupled hydro-thermo-biological behavior of bioreactor landfills in the anaerobic phase in the laboratory and using site data of two bioreactor landfills in France and developing a numerical coupled model. The laboratory experiments help us to know the effect of such important parameters as saturation and density of wastes on anaerobic degradation and biogas production. The site data help us to know the variations of saturation and temperature of wastes in a bioreactor landfill in different depths, as two key factors of anaerobic degradation and biogas production. Site analysis helps also to estimate some parameters as hydraulic and thermal conductivity of wastes, which are hard to measure in situ without disturbing the landfill site. The numerical model helps us to study the coupled behavior of bioreactor landfills during leachate recirculation, as well as on the long term during many years. The interdependence of various parameters which influence waste degradation and thermo-biological phenomena in a bioreactor landfills is the main reason of development of this coupled model. This model makes it possible to study each key parameter, as saturation and temperature, as a function of other parameters. Laboratory experiments and site data analysis lead to develop a biological model of degradation to be coupled with a two-phase flow model of liquid and gas. The three parts of this thesis, laboratory experiments, site data analysis and development of the numerical coupled model were carried out in parallel and in a complementary manner. Laboratory experiments as well as site data analysis showed us the importance of some parameters to be considered in the numerical model and coupled behavior. In return numerical model showed the importance of considering the temperature dependence behavior of microbial activity and the necessity of biomass, VFA and COD analysis in laboratory experiments. The analysis of hydraulic and thermal site data led to estimate parameters which are hard to measure in situ or in the laboratory, as hydraulic and thermal conductivity of waste, saturation, thermal conductivity of cover layer and heat capacity of waste. The numerical coupled hydro-thermo-biological model seems to be efficient enough to predict biogas and methane production in bioreactor and classical landfills and to reproduce their correct behavior

Carbon dioxide is released by natural and anthropogenic processes, such as the production and combustion of fossil fuels. Production of biogas also generates carbon dioxide, but of biogenic origin. The global, yearly emissions of greenhouse gases are regularly increasing, although agreements such as the Paris Agreement is signed by parties globally. Sweden has the goal to reach net-zero emissions by 2045, and thereafter to only obtain negative emission levels. To reach these goals the biogenic version of Carbon Capture and Storage (CCS) called Bioenergy with Carbon Capture and Storage (BECCS) is considered to be an essential strategy. Using carbon dioxide, through Carbon Capture and Utilization (CCU), in for example products, can complement BECCS since the strategy can increase the value of carbon dioxide. These strategies make it possible to reduce the climate impact of biogas production.  This master thesis aimed to chart different techniques in CCS and CCU to examine how they can be used to utilize or store carbon dioxide from biogas plants. What technical demands different solutions create was explored. The different techniques were assessed through a multi criteria analysis by a technological, environmental, marketable and economical standpoint to investigate which ones were the most suitable for a specific, studied case – Tekniska verken’s biogas plant. One suitable technique within CCU was analyzed through a screening of actors in the region. An environmental assessment of one technique in CCS and one in CCU were compared with the reference case Business as usual, to explore how a simulated biogas plant’s climate impact can change through the implementation of CCS and CCU.  The charting of literature gave findings of 42 different techniques, which were sifted down to 7; algae farming for wastewater treatment, BECCS in saltwater aquifers, carbon dioxide curing of concrete, bulk solutions, production of methanol, production of methane through Power To Gas and crop yield boosting in greenhouses. The multi criteria analysis pointed out carbon dioxide curing of concrete and BECCS in saltwater aquifers as suitable solutions for the studied case. The implementation of these techniques requires a liquefaction plant, infrastructure for transportation as well as business partners.  A life cycle assessment of the studied cases climate impact was given through modelling and simulation of a model plant of the studied case, with the functional unit 1 Nm3 biomethane. The reference case Business as usual had a climate impact of 0,38 kg CO2 eq, which corresponds to approximately one eighth of the climate impact of fossil fuels such as gasoline or diesel. By storing the carbon dioxide through BECCS in saltwater aquifers the climate impact decreased to - 0,42 kg CO2 eq. By utilizing the carbon dioxide through curing of concrete the biomethane’s climate impact decreased to -0,72 kg CO2 eq. The results thereby evince that Swedish biogas producers can improve their climate performance through CCS and CCU. / Koldioxid släpps ut av såväl naturliga som antropogena processer, exempelvis vid produktion och förbränning av fossila bränslen. Även vid biogasproduktion uppkommer koldioxid, men av biogent ursprung. Årliga globala utsläpp av växthusgaser ökar regelbundet, trots överenskommelser som Parisavtalet som syftar till att begränsa klimatförändringarna. Sverige ska nå nettonollutsläpp senast 2045 och därefter ha negativa utsläppsnivåer. För att uppnå detta mål anses en biogen version av Carbon Capture and Storage (CCS), det vill säga avskiljning och lagring av koldioxid, kallad Bioenergy with Carbon Capture and Storage (BECCS) vara en essentiell strategi. Tillvaratagande av koldioxid, genom Carbon Capture and Utilization (CCU), kan ge ett bra komplement till BECCS eftersom det nyttiggör koldioxid i produkter och kan öka värdet av koldioxid. Tekniker inom CCS och CCU möjliggör minskad klimatpåverkan inom biogasproduktion.  Detta examensarbete syftade till att kartlägga olika alternativ inom teknikerna CCS och CCU för att undersöka hur dessa kan användas för att nyttiggöra eller lagra koldioxid från biogasanläggningar, samt att undersöka vilka tekniska krav som ges av lösningarna. Utifrån en multikriterieanalys bedömdes vilka lösningar som var tekniskt, miljömässigt, marknadsmässigt och ekonomiskt motiverade för tillvaratagande av koldioxid. Bedömningen genomfördes genom att studera specifikt fall som var Tekniska verken i Linköpings biogasanläggning. Den lösning som valdes ut som lämplig inom CCU analyserades ur ett marknadsmässigt perspektiv genom en översiktlig kartläggning av aktörer i regionen. Därefter studerades klimatpåverkan från en förenklad modell av Tekniska verkens biogasanläggning för att undersöka hur denna förändras vid implementering av en lämplig lösning inom CCS respektive CCU.  Genom en screening av lösningsförslag identifierades 42 lösningsförslag inom CCS och CCU som sållades ner till sju stycken; algodling vid vattenrening, BECCS i saltvattenakviferer, betong härdad av koldioxid, bulklösning, metanoltillverkning, tillverkning av metan genom Power To Gas samt växthusodling. Multikriterieanalysen visade att koldioxidhärdad betong inom CCU och BECCS i saltvattenakviferer inom CCS var lämpliga lösningar för det studerade fallet. För implementering av förslagen krävdes bland annat en förvätskningsanläggning, infrastruktur för transport och samarbetspartners.  De studerade scenariernas klimatmässiga livscykel erhölls genom modellering och simulering av en modellanläggning av det studerade fallets biogasanläggning i programvaran SimaPro med användning av den funktionella enheten 1 Nm3 fordonsgas. Resultatet visade att fordonsgasen i referensfallet har en klimatpåverkan på 0,38 kg koldioxidekvivalenter. Fordonsgasens klimatpåverkan var cirka en åttondel av fossila bränslen såsom bensin och diesels klimatpåverkan. Vid lagring av koldioxid genom BECCS i saltvattenakviferer förändrades klimatpåverkan till - 0,42 kg koldioxidekvivalenter. När koldioxid användes till härdning av betong förändrades fordonsgasens klimatpåverkan till -0,72 kg koldioxidekvivalenter. Detta innebär att svenska producenter av biogas kan förbättra sin klimatpåverkan genom såväl lösningar inom CCS som CCU.

To develop anaerobic digestion (AD), innovative solutions to increase methane yields in existing AD processes are needed. In particular, the adoption of low energy pre-treatments to enhance biomass biodegradability is needed to provide efficient digestion processes increasing profitability. To obtain these features, hydrodynamic cavitation has been evaluated as an innovative solutions for AD of waste activated sludge (WAS), food waste (FW), macro algae and grass, in comparison with steam explosion (high energy pre-treatment). The effect of these two pre-treatments on the substrates, e.g. particle size distribution, soluble chemical oxygen demand (sCOD), biochemical methane potential (BMP) and biodegradability rate, have been evaluated. After two minutes of hydrodynamic cavitation (8 bar), the mean fine particle size decreased from 489- 1344 nm to 277- 381 nm (≤77% reduction) depending of the biomasses. Similar impacts were observed after ten minutes of steam explosion (210 °C, 30 bar) with a reduction in particle size between 40% and 70% for all the substrates treated.  In terms of BMP value, hydrodynamic cavitation caused significant increment only within the A. nodosum showing a post treatment increment of 44% compared to the untreated value, while similar values were obtained before and after treatment within the other tested substrates. In contrast, steam explosion allowed an increment for all treated samples, A. nodosum (+86%), grass (14%) and S. latissima (4%). However, greater impacts where observed with hydrodynamic cavitation than steam explosion when comparing the kinetic constant K. Overall, hydrodynamic cavitation appeared an efficient pre-treatment for AD capable to compete with the traditional steam explosion in terms om kinetics and providing a more efficient energy balance (+14%) as well as methane yield for A. nodosum. / Det behövs innovativa lösningar för att utveckla anaerob rötning i syfte att öka metangasutbytet från biogassubstrat. Beroende på substratets egenskaper, kan förbehandling möjliggöra sönderdelning av bakterieflockar, uppbrytning av cellväggar, elimination av inhiberande ämnen och frigörelse av intracellulära organiska ämnen, som alla kan leda till en förbättring av den biologiska nedbrytningen i rötningen. För att uppnå detta har den lågenergikrävande förebehandlingsmetoden hydrodynamisk kavitation prövats på biologiskt slam, matavfall, makroalger respektive gräs, i jämförelse med ångexplosion. Effekten på substraten av dessa två förbehandlingar har uppmäts genom att undersöka distribution av partikelstorlek, löst organiskt kol (sCOD), biometan potential (BMP) och nedbrytningshastigheten. Efter 2 minuters hydrodynamisk kavitation (8 bar) minskade partikelstorleken från 489- 1344 nm till 277- 281 nm (≤77 % reduktion) för de olika biomassorna. Liknande påverkan observerades efter tio minuters ångexplosion (210 °C, 30 bar) med en partikelstorlekreducering mellan 40 och 70 % för alla behandlade substrat. Efter behandling med hydrodynamisk kavitation, i jämförelse med obehandlad biomassa, ökade metanproduktionens hastighetskonstant (K) för matavfall (+65%), makroalgen S. latissima (+3%), gräs (+16 %) samtidigt som den minskade för A. nodosum (-17 %). Förbehandlingen med ångexplosion ökade hastighetskonstanten för S. latissima (+50 %) och A. nodosum (+65 %) medan den minskade för gräs (-37 %), i jämförelse med obehandlad biomassa. Vad gäller BMP värden, orsakade hydrodynamisk kavitation små variationer där endast A. nodosum visade en ökning efter behandling (+44 %) i jämförelse med obehandlad biomassa. Biomassa förbehandlade med ångexplosion visade en ökning för A .nodosum (+86 %), gräs (14 %) och S. latissima (4 %). Sammantaget visar hydrodynamisk kavitation potential som en effektiv behandling före rötning och kapabel att konkurrera med den traditionella ångexplosionen gällande kinetik och energibalans (+14%) samt metanutbytet för A. nodosum.

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