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Diagenesis and Formation Stress in Fracture Conductivity of Shaly Rocks Louisiana State University LSU Digital Commons LSU Doctoral Dissertations Graduate School 8-28-2017 Diagenesis and Formation Stress in Fracture Conductivity of Shaly Rocks; Experimental- Modelling Approach in CO2-Rock Interactions Abiola Olukola Olabode Louisiana State University and Agricultural and Mechanical College, [email protected] Follow this and additional works at: https://digitalcommons.lsu.edu/gradschool_dissertations Part of the Environmental Engineering Commons, Geotechnical Engineering Commons, and the Petroleum Engineering Commons Recommended Citation Olabode, Abiola Olukola, "Diagenesis and Formation Stress in Fracture Conductivity of Shaly Rocks; Experimental-Modelling Approach in CO2-Rock Interactions" (2017). LSU Doctoral Dissertations. 4105. https://digitalcommons.lsu.edu/gradschool_dissertations/4105 This Dissertation is brought to you for free and open access by the Graduate School at LSU Digital Commons. It has been accepted for inclusion in LSU Doctoral Dissertations by an authorized graduate school editor of LSU Digital Commons. For more information, please [email protected]. DIAGENESIS AND FORMATION STRESS IN FRACTURE CONDUCTIVITY OF SHALY ROCKS; EXPERIMENTAL-MODELLING APPROACH IN CO2-ROCK INTERACTIONS A Dissertation Submitted to the Graduate Faculty of the Louisiana State University and Agricultural and Mechanical College in partial fulfilment of the requirements for the degree of Doctor of Philosophy in The Craft & Hawkins Department of Petroleum Engineering by Abiola Olukola Olabode B.S., Obafemi Awolowo University, 2008 M.S., Louisiana State University, 2012 December 2017 1 To my mother, Adeyinka, who lived but for a while ii ACKNOWLEDGEMENTS My sincere gratitude goes to the following; Dr. Craig M Harvey for graciously serving as chair of my doctoral research committee; my committee members, Dr. Mayank Tyagi, Dr. Paulo Waltrich, Dr. Dandina Rao and the graduate school Dean’s Representative Dr. Chao Sun for their invaluable contributions and criticisms that have given shape to this work. I want to specially thank the Craft and Hawkins Department of Petroleum Engineering for availing me the multi-year resources that made this project a success. I appreciate Wanda LeBlanc, LSU AgCenter, Donmei Cao, and the LSU SIF staff members for assisting with post experimental data analysis. I also thank George Ohrberg for helping with computing needs in data acquisition and Fenelon Nunes for helping with laboratory ware purchases and maintenance. The financial support of the SPE and the GDL Foundation is kindly acknowledged. Thanks to LSU Graduate School for the Dissertation Year Fellowship that saw me through my final semesters. I am appreciative of colleagues with whom I shared and gained useful ideas. They include Nnamdi Agbasimalo, Chukwudi Chukwudozie, Wei Wang, Gbola Afonja, Paulina Mwangi, Louise Smith, Arome Oyibo, Darko Kupresan, Kolawole Bello, Ruixuan Guo and Hui Du to mention a few. Special thanks to my wife, Omoefe Kio-Olabode, for her unrelenting support throughout my graduate studies. Your children shall call you blessed. To our son, Mark Olayinka, thanks for beaming light on to our world at this junction in our lives. I deeply appreciate the fervent prayers and support of my father and siblings; Oladepo Olabode, Titilola Akinyemi and Motunrola Olaiya. Thanks to my uncle, Jinmi Olabode and cousin, Tolu Olabode for always checking on us all these years. Also, special thanks to the Chapel on Campus for the edification of my inner man since I arrived at LSU. iii TABLE OF CONTENTS ACKNOWLEDGEMENTS…………..……………………………………………………………………………………………..... iii LIST OF TABLES ……………………………………………………………………………………………………………………….. vi LIST OF FIGURES ……………………………………………………………………………………………………………..…….. viii NOMENCLATURE …………………………………………………………………………………………………………..……..... xv ABSTRACT ………………………………………………………………………………………………………………………..….... xvi CHAPTER 1. INTRODUCTION …………………………………………………………………………………………………….. 1 1.1 Background on Carbon Sequestration ..................................................................................... 1 1.2 Diagenesis and Fractures ......................................................................................................... 8 1.3 Problem Definition ................................................................................................................. 12 1.4 Objective of Research ……….………………………………………………………………………………………………. 13 CHAPTER 2. LITERATURE REVIEW ………………………………………….………………………………………………… 15 2.1 Diagenesis of Sedimentary Rocks …………................................................................................ 15 2.2 A Brief on Properties of CO2 Saturated Brine ........................................................................ 16 2.3 Shale Caprock Geochemical Alteration and Subsurface CO2 Migration ................................. 20 2.4 Geomechanical Effects ……………………………………………….. ....................................................... 43 2.5 Previous Experimental and Modeling Works ….……………………............................................... 55 CHAPTER 3. EXPERIMENTAL SETUP AND PROCEDURE ……………………………………………….…………… 62 3.1 Experimental Methods and Sample Preparation ……………………….……………………………………… 62 3.2 Experimental Setup................................................................................................................ 66 3.3 Experimental Shale Rocks Geology ........................................................................................ 66 3.4 Mineralogical Composition of Shale Rock Samples................................................................ 67 3.5 Experimental CO2-brine Fluid…............................................................................................... 70 3.6 Techniques in Rock and Fluid Analysis .................................................................................... 71 3.7 Experimental Parameters ……………………………………………………………………………………..………….. 74 3.8 Experimental Matrix ……………………………………………………………………………………………..………….. 76 CHAPTER 4. RESULTS FROM SHALE ROCK/FLUID INTERACTIONS EXPERIMENTS …………………….. 81 4.1 pH Measurement ……………………………………………………………………………………………………………... 81 4.2 Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES) Analysis.................... 82 4.3 Total Carbon Analysis …………………………………………………………................................................. 94 4.4 X-Ray Diffraction (XRD) Analysis ……………………………………….……………….................................. 96 iv 4.5 Electron Micro-Probe Analysis (EMPA) of Bulk Rock............................................................. 106 4.6 Micro-Indentation of Rock Samples .................................................................................... 120 4.7 Differential Pressure Analysis …………………………………………………………………………………………. 124 4.8 Fracture Conductivity Estimation ……………………………………………………………………………………. 128 CHAPTER 5. DISCUSSION OF RESULTS ROCK/FLUID INTERACTIONS EXPERIMENTS …..………….. 134 5.1 General Discussion of Experimental Results …………..………………………………………………………. 134 5.2 Integrated Experimental Observations ……………………….………..…………………………….…….……. 141 CHAPTER 6. CONCLUSIONS AND RECOMMENDATIONS …………………………………….……..……… 143 6.1 Conclusions ………………………………………………………………………………………………………….………… 143 6.2 Recommendations ……………………………………………………………………………………………….………… 146 REFERENCES............................................................................................................................... 147 APPENDICES …………………………………………………………………………………………………………………………. 166 A: EQUIPMENT AND MATERIALS USED FOR SHALE ROCK/CO2 BRINE EXPERIMENTS ……………… 166 B: EXPERIMENTAL PROCEDURE FOR ROCK-FLUID INTERACTION EXPERIMENTS ………………....... 172 C: pH DATA ……………………..………………………..…………………………..……………….………………….……..…. 175 D: INDUCTIVELY COUPLED PLASMA EMISSION SPECTROSCOPY (ICP-OES) DATA....................... 176 E: MICRO-INDENTATION OF SHALE ROCKS DATA ………………...................................................... 179 F: ADDITIONAL DATA FOR ELECTRON MICROPROBE ANALYSIS (EMPA).................................... 180 G: FLOW/PRESSURE DATA ......................................................................................................... 188 H: FRACTURE CONDUCTIVITY DATA AND CALCULATIONS ..……………….………………….................. 196 VITA ……………………………………………………………………………………………………………………….…..……….. 197 v LIST OF TABLES 1.1: Worldwide potential CO2 sequestration capacities and risks …………….………………..…..………… 2 2.1: Mineralogy of typical shale rock samples showing percentage composition ….………….….…. 22 2.2: Geochemical model for reaction of shale, sandstone and cement with CO2 and Na, Ca, Mg Chloride brines ……………….………………………………………………………………………………….………………….. 26 3.1. Geological properties of shale rock samples used in the experiment ……………….….…………… 67 3.2: Mineralogical composition of shale samples in percentages as captured by the ternary diagram of figure 3.5 …………………………….………………………………………………………………………………… 70 3.3: Experimental brine composition for Shale/CO2-brine flooding experiment based on flowback fluid composition from hydraulically fractured shale ………………………………………………………………..71 3.4: Experimental Matrix for CO2-brine/shale interaction at conditions of 50°C temperature and 1,000 psi pressure stated in A above .…………………………………………………………………………..……… 76 3.5: Experimental Matrix for CO2-brine/shale interaction at conditions of 50°C temperature and 1,000 psi pressure stated in B above .……………………………..…………………………………….…..……. 77 3.6: Micro-indentation; Hardness and Young Modulus at different temperature and pressure conditions of rock fluid interaction ………………………………………………….……………………….…………….
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