OPTIMIZATION OF THE ELECTRON DONOR SUPPLY TO SULPHATE REDUCING BIOREACTORS TREATING INORGANIC WASTEWATER Luis Carlos Reyes Alvarado Optimization of the electron donor supply to sulphate reducing bioreactors treating inorganic wastewater Joint PhD degree in Environmental Technology Docteur de l’Université Paris-Est Spécialité : Science et Technique de l’Environnement Dottore di Ricerca in Tecnologie Ambientali Degree of Doctor in Environmental Technology Thèse – Tesi di Dottorato – PhD thesis Luis Carlos Reyes Alvarado Optimization of the electron donor supply to sulphate reducing bioreactors treating inorganic wastewater Defended on December 16th, 2016 In front of the PhD committee Dr. Artin Hatzikioseyian Reviewer Prof. Dr. Erkan Sahinkaya Reviewer Prof. Dr. Ir. Piet Lens Promotor Dr. Eldon R. Rene Co-promotor Prof. Dr. Giovanni Esposito Co-promotor Prof. Dr. Michel Madon Co-promotor Hab. Dr. Eric D. van Hullebusch Examiner Erasmus Joint Doctorate Programme in Environmental Technology for Contaminated Solids, Soils and Sediments (ETeCoS3) Thesis commettee Promotor Prof. Dr. Ir. Piet N. L. Lens Professor of Environmental Biotechnology UNESCO‐IHE Delft, The Netherlands Co-promotors Dr. Eldon R. Rene Senior Lecturer in Resource Recovery Technology UNESCO‐IHE Delft, The Netherlands Prof. Dr. Giovanni Esposito Professor in Environmental Engineering University of Cassino and Southern Lazio Cassino, Italy Prof. Dr. Michel Madon Professor in Biogeochemistry University of Paris‐Est Marne‐la‐Vallée, France Other members Dr. Artin Hatzikioseyian School of Mining and Metallurgical Engineering National Technical University of Athens (NTUA), Greece Prof. Dr. Erkan Sahinkaya Professor of Bioengineering Medeniyet Üniversitesi Goztepe, Istanbul, Turkey Hab. Dr. Eric D. van Hullebusch Hab. Associate Professor in Biogeochemistry University of Paris‐Est Marne‐la‐Vallée, France This research was conducted under the auspices of the Erasmus Mundus Joint Doctorate in Environmental Technologies for Contaminated Solids, Soils, and Sediments (ETeCoS3) and the Graduate School for Socio‐Economic and Natural Sciences of the Environment (SENSE). CRC Press/Balkema is an imprint of the Taylor & Francis Group, an informa business © 2018, Luis Carlos Reyes-Alvarado Although all care is taken to ensure integrity and the quality of this publication and the information herein, no responsibility is assumed by the publishers, the author nor IHE Delft for any damage to the property or persons as a result of operation or use of this publication and/or the information contained herein. A pdf version of this work will be made available as Open Access via http://repository.tudelft.nl/ihe This version is licensed under the Creative Commons Attribution-Non Commercial 4.0 International License, http://creativecommons.org/licenses/by-nc/4.0/ Published by: CRC Press/Balkema Schipholweg 107C, 2316 XC, Leiden, the Netherlands [email protected] www.crcpress.com – www.taylorandfrancis.com ISBN: 978-1-138-34331-3 Table of contents LIST OF FIGURES XIV LIST OF TABLES XVI ACKNOWLEDGMENTS XIX ABSTRACT XX RESUMÉ XXII SAMENVATTING XXIV SOMMARIO XXVI CHAPTER 1 INTRODUCTION 1 1.1 Backg round 2 1.2 The PhD thesis structure 4 1.3 References 6 CHAPTER 2 LITERATURE REVIEW 9 Abstract 10 2.1 Anaerobic digestion 11 2.1.1 Hydrolysis-fermentation 11 2 .1.2 Acetogenesis 11 2.1.3 Methanogenesis 12 2.2 The sulphate reduction process 13 2.2.1 Sulphur cycle 13 2 .2.2 Biological sulphate reduction 14 2.2.3 Sulphate reducing bacteria (SRB) 17 2.3 Electron donors for SRB 18 2.3.1 Organic solids 19 2.3.1.1 Starch 19 2.3 .1.2 Cellulose 20 2.3.1.3 Proteins 20 2.3.1.4 Chitin 21 2.3.2 Se lection of electron donors for biological sulphate reduction 21 2.3.2.1 Efficiency of sulphate removal 22 2.3 .2.2 Availability and cost of electron donor 22 2.3.3 En vironmental parameters affecting sulphate reduction 23 vii 2.3.3.1 Temperature 23 2.3.3.2 pH and S2- concentration 23 2.3.3.3 Hydraulic retention time (HRT) 24 2.4 Con ventional bioreactors for sulphate reduction 24 2.4.1 UASB bioreactor 26 2 .4.2 Inverse fluidized bed reactor 26 2.4.3 Factors affecting bioreactor performance 28 2.4 .3.1 Characteristics of organic substrate 28 2.4 .3.2 Particle size of electron donors 29 2.4.3.3 Source of inoculum 30 2.4.3.4 Physical and chemical conditions in a bioreactor 30 2.4.3.5 Biomass morphology 31 2.5 Mod elling biological sulphate reduction 32 2.5.1 Monod type modelling for biological sulphate reduction 32 2 .5.2 Artificial neural network (ANN) based modeling 33 2.5 .2.1 Fundamentals of ANN 33 2.5 .2.2 Multi-layer perceptron 34 2.5.2.3 Back propagation algorithm 34 2.5.2.4 Internal network parameters 35 2.5.2.5 ANN modelling for bioreactors 36 2.6 Con clusions 38 2.7 References 38 CHAPTER 3 FORECASTING THE EFFECT OF FEAST AND FAMINE CONDITIONS ON BIOLOGICAL SULPHATE REDUCTION IN AN ANAEROBIC INVERSE FL UIDIZED BED REACTOR USING ARTIFICIAL NEURAL NETWORKS 51 Abstract 52 3.1 Introduction 53 3.2 Material and methods 56 3.2.1 Synthetic wastewater composition 56 3 .2.2 Carrier material 56 3.2.3 Inoculum 56 3.2.4 Anaerobic IFB bioreactor set up 57 3.2.5 IFB bioreactor operational conditions 57 3.2.6 RTD studies 58 3.2.7 Chemical analysis 59 3.2.8 Data processing 59 3.2 .8.1 Performance and comparison of the IFB bioreactors 59 3.2 .8.2 Evaluation of RTD 60 3.2.8.3 ANN modelling 60 3.3 Resu lts 65 3.3.1 RTD of the IFB bioreactor 65 viii 3.3.2 Biological sulphate reduction under steady state feeding conditions 66 3.3.3 Biological sulphate reduction under non steady feeding conditions 71 3.3.4 ANN Modelling 72 3.3 .4.1 Selecting the best training network parameters 72 3.3.5 ANN model predictions and sensitivity analysis 74 3.4 Discussion 76 3.4.1 Performance of the IFB bioreactors under steady feeding conditions (periods I-IV) 76 3.4.2 Effect of transient feeding conditions on IFB bioreactor operation 77 3.4.3 Ro bustness of biological sulphate reduction in IFB bioreactors 79 3.4.4 ANN modelling and transient feeding conditions 80 3.5 Conclusions 82 3.6 References 82 CHAPTER 4 HIGH RATE BIOLOGICAL SULPHATE REDUCTION IN A LACTATE FED INVERSE FLUIDIZED BED REACTOR AT A HYDRAULIC RETENTION TIME OF 3 H 89 Abstract 90 4.1 Introduction 91 4.2 Material and methods 92 4.2.1 Synthetic wastewater 92 4 .2.2 Inoculum 92 4.2.3 Carrier material 92 4.2.4 Anaerobic inverse fluidized bed bioreactor 93 4.2.5 Hydrodynamic evaluation of the IFB 93 4.2 .5.1 Residence time distribution 93 4.2 .5.2 Bed expansion 94 4.2.6 Re actor operation conditions 94 4.2.7 Ch emical analysis 95 4.2.8 Kinetic analysis 97 4.2 .8.1 Second order substrate removal model 97 4.2 .8.2 The Stover-Kincannon model 97 4.3 Resu lts 98 4.3.1 Hydrodynamic evaluation 98 4.3.1.1 Residence time distribution 98 4.3 .1.2 Relative bed expansion 98 4.3.2 Su lphate reduction in the high rate IFBB 100 4.3.2.1 Sulphate and COD removal efficiency 100 4.3 .2.2 Sulphide production in the IFBB 102 4.3.2.3 The pH in the IFBB during the biological sulphate reduction 102 4.3.2.4 Biomass production during the IFBB operation 102 4.3.3 Ki netic analysis of the IFBB performance 103 4.3.3.1 Grau second order substrate removal 103 4.3 .3.2 The Stover-Kincannon model 103 ix