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Vapour-Liquid Equilibrium of Carbon Dioxide in Newly Proposed Blends

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Vapour-Liquid Equilibrium of Carbon Dioxide in Newly Proposed Blends Vapour-liquid Equilibrium of Carbon Dioxide in Newly Proposed Blends of Alkanolamines Thesis submitted in partial fulfillment of the requirement for the degree of Doctor of Philosophy in Chemical Engineering by Gaurav Kumar (Roll No – 509CH103) Under the guidance of Dr. Madhusree Kundu Department of Chemical Engineering National Institute of Technology Rourkela, Odisha – 769008 August 2013 i Dedicated to My Parents and Late Dadajee ii Department of Chemical Engineering National Institute of Technology, Rourkela Odisha, India – 769008 Certificate This is to certify that the thesis entitled ‘Vapour-liquid Equilibrium of Carbon Dioxide in Newly Proposed Blends of Alkanolamines’ submitted by Gaurav Kumar is a record of an original research work carried out by him under my supervision and guidance in partial fulfillment of the requirements for the award of the degree of Doctor of Philosophy in Chemical Engineering during the session July’2009 – August’ 2013 in the Department of Chemical Engineering, National Institute of Technology, Rourkela. Neither this thesis nor any part of it has been submitted for the degree or academic award elsewhere. Dr. Madhusree Kundu Associate Professor Department of Chemical Engineering National Institute of Technology, Rourkela iii PRELUDE The thesis entitled ‘Vapour-liquid equilibrium of carbon dioxide in newly proposed blends of alkanolamines’, is a pursuit of my PhD work; being carried out in the Department of Chemical Engineering at National Institute of Technology Rourkela, India. The motive behind the present work was to propose newer blends of alkanolamines, which could be best used for effective removal of CO2 from natural gas, power plant flue gas, refinery off gases etc. Adsorption using MOFs, de-sublimation of CO2 from natural gas or flue gas stream by cryogenic cooling, and membrane separation are the technologies available for CO2 removal and are under trial for commercialization. Aqueous amine absorption/stripping is by far the best technology currently available for CO2 removal. Recently room temperature ionic liquids (ILs’); called green solvents are emerging as promising candidates to capture CO2 due to their wide liquid range, low melting point, negligible vapour pressure, high CO2 solubility and reasonable thermal stability. However, it is difficult to realize ionic liquids industrially owing to its high viscous nature and high cost, which left us with limited options like CO2 absorption in alkanolamines or in Sodium and Potassium salts of primary or tertiary amino acids promoted with reactive alkanolamines. The first aqueous alkanolamine used commercially was triethanolamine; way back in 1930. Henceforth, various alkanolamines including some proprietary formulations of alkanolamine solutions were proposed in this regard. Because of the need to exploit poorer quality crude and natural gas twined with the enhanced environmental obligations, energy efficient and selective acid gas treating at a competitive price are of dire need. As a result, there has been a rekindling of interest in new alkanolamine formulations and particularly in aqueous blends of those alkanolamines. For the rational design of gas treating processes knowledge of vapour liquid equilibrium of the acid gases in alkanolamines are essential, besides the knowledge of mass transfer and kinetics of absorption and regeneration. The experimentation on VLE of CO2 in the proposed alkanolamine blends corroborated multi-component and multiphase equilibria. iv Present thesis is organized into the following chapters: Chapter 1: Background, origin of the work, objective, and outline of the thesis are being discussed here. Chapter 2: Chemical reaction equilibria and thermodynamics related to CO2 gas treating through alkanolamine solutions is presented here. This chapter also presents the recent literature on CO2 removal using aqueous alkanolamine solvents. Chapter 3: This chapter includes experimentation set-up, methods, and their validation. Generated VLE data on aqueous, (DEA + MDEA/AMP), N-methyl-2- ethanolamine (MAE) and aqueous N-ethyl-ethanolamine (EAE) solutions have been reported here. The deprotonation and carbamate reversion constants for EAE are also reported here. Chapter 4: Experimental VLE data on (EAE + MDEA/AMP) and (MAE + MDEA/AMP) blends for various relative amine compositions over a wide range of temperature and CO2 pressure are reported with analysis. The CO2 solubility in the newly proposed blends has been compared with (DEA + MDEA/AMP) blends. Present chapter also includes the correlation of VLE data of (CO2 + EAE + MDEA + H2O) system using rigorous thermodynamic model. Chapter 5: COSMO solvation model, calculation of thermodynamic property using COSMO-RS, computational procedure and applicability of COSMO-RS are included here. This chapter provides the COSMO predicted thermodynamic properties of binary (MAE/EAE + water) and ternary (CO2+ MAE/EAE + water) systems. Chapter 6: This chapter is devoted to density data generation of (EAE + MDEA + H2O), (EAE + AMP + H2O), (MAE + AMP + H2O) and (MAE + MDEA + H2O) systems and their correlation using Redlich-Kister equation and the Nissan type of correlation. Chapter 7: In an ending note, chapter 7 concludes the thesis with future recommendations. Based on the dissertation, five numbers of publications in various International journals are already published. Publication number 2 & 3 (as per the vita) is related to chapter 3. Publication number 1 & 5 (as per the vita) is related to chapter 4. Publication number 4 (as per the vita) is related to chapter 6. Another research article (number 6 as per the vita) is related to chapter 5 has been communicated. v Acknowledgement I would like to express my respect and sincere gratitude to my thesis supervisor, Dr. Madhusree Kundu, for giving me an opportunity to work under her supervision for my doctoral program at the National Institute of Technology, Rourkela. I am indebted to professor Kundu for her invaluable supervision and esteemed guidance. As my supervisor, her insight, observations and suggestions helped me to establish the overall direction of the research and to achieve the objectives of the work. Her continuous encouragement and support have been always a source of inspiration and energy for me. I express my sincere thanks to Prof. R. K. Singh, Head, Chemical engineering department and members of Doctoral Scrutiny Committee (DSC) Prof. P. Rath, Prof. B. Munshi and Prof. S. Sarkar, and all the faculty members of Chemical Engineering Department for their suggestions and constructive criticism during the preparation of the thesis. I acknowledge all my seniors like Dr. Achyut Panda, Dr. Nihar Ranjan Biswal, Dr. Ramakrishna Gottipatti, Dr. Nagesh Tripathy, research scholars, and staff of Chemical Engineering Department for their support during my research work. Thanks are also due to Mr. Rajib Ghosh, Mr. Yogesh, Mr. Akhilesh, Mr. Arun, Mr. & Mrs. Jeevan, Mr. Sachin, Mr. Arvind, Mr. vamsi, Mr. Sambhurisha, Mr. Tripathy, Mr. Sujeevan, Mr. Sheshu, Ms. Shivani, Mr. Deokaran and other friends and family members of mine, whom I could not mention here, for their encouragement and moral support. I must acknowledge the academic resources provided by N.I.T., Rourkela and the research fellowship granted by Ministry of Human Resource and Development (MHRD), vi and project fund given by Department of Science and Technology (DST), New delhi, India, to carry out this work. Finally, I am forever indebted to my parents, brother, brother-in-law, sister and sister-in-law for their understanding, endless patience and encouragement from the beginning; and heartiest love to adolescent’s from my family like my younger brother & sister Nishu, Guddi, Sonali and Sanu. Special love and fondness to Apporva, Mayank, Gunja, Rounak, Dolly and Adhikaar………. National Institute of Technology Gaurav Kumar Rourkela, Odisha August 2013 vii ABSTRACT VAPOUR-LIQUID EQUILIBRIUM OF CARBON DIOXIDE IN NEWLY PROPOSED BLENDS OF ALKANOLAMINES BY GAURAV KUMAR In the backdrop of a major climatic change vastly due to the greenhouse gas emission, gas treating has become a significant area of interest as it has never been earlier. Carbon dioxide (CO2), one of the major greenhouse gases are treated mainly by absorption in alkanolamine solvents, though ionic liquids and Sodium and Potassium salts of primary or tertiary amino acids are given consideration presently for effective and energy efficient CO2 capture. Gas treating research is actually passing through a transition which has been chronicled in the present work. Among the different technologies available for CO2 mitigation, capture of CO2 by chemical absorption is the technology that is closest to get implemented commercially. In the present context, the role of alkanolamine solvents in sour gas treating research should be revered, hence, N-methyl-2-ethanolamine (MAE), and 2- (ethylamino) ethanol (EAE) has been prudently explored for CO2 capture. Apart from the knowledge of mass transfer and kinetics, the equilibrium solubility of acid gases over alkanolamines presumes an instrumental role in gas treating processes. To exploit poorer quality crude and natural gas twined with the enhanced environmental legislations, highly selective and economic acid gas treating processes are in an unprecedented need. In view of this, the present work was taken up to investigate the possibility of (EAE/MAE + MDEA/AMP) solvent as effective blends towards CO2 absorption. Measurement of solubility of CO2 in aqueous single amine,
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