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Production of Lithium Peroxide and Lithium Oxide in an Alcohol Medium

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Production of Lithium Peroxide and Lithium Oxide in an Alcohol Medium PRODUCTION OF LITHIUM PEROXIDE AND LITHIUM OXIDE IN AN ALCOHOL MEDIUM by J avad Khosravi Department ofMining, Metals and Materials Engineering McGill University, Montreal, Canada March2007 A thesis submitted to the Office of Graduate and Postdoctoral Studies in fulfillment of the requirements for the degree of Doctor of Philosophy © Javad Khosravi, 2007 Libraryand Bibliothèque et 1+1 Archives Canada Archives Canada Published Heritage Direction du Branch Patrimoine de l'édition 395 Wellington Street 395, rue Wellington Ottawa ON K1A ON4 Ottawa ON K1A ON4 Canada Canada Your file Votre référence ISBN: 978-0-494-38597-5 Our file Notre référence ISBN: 978-0-494-38597-5 NOTICE: AVIS: The author has granted a non­ L'auteur a accordé une licence non exclusive exclusive license allowing Library permettant à la Bibliothèque et Archives and Archives Canada to reproduce, Canada de reproduire, publier, archiver, publish, archive, preserve, conserve, sauvegarder, conserver, transmettre au public communicate to the public by par télécommunication ou par l'Internet, prêter, telecommunication or on the Internet, distribuer et vendre des thèses partout dans loan, distribute and sell theses le monde, à des fins commerciales ou autres, worldwide, for commercial or non­ sur support microforme, papier, électronique commercial purposes, in microform, et/ou autres formats. paper, electronic and/or any other formats. The author retains copyright L'auteur conserve la propriété du droit d'auteur ownership and moral rights in et des droits moraux qui protège cette thèse. this thesis. Neither the thesis Ni la thèse ni des extraits substantiels de nor substantial extracts from it celle-ci ne doivent être imprimés ou autrement may be printed or otherwise reproduits sans son autorisation. reproduced without the author's permission. ln compliance with the Canadian Conformément à la loi canadienne Privacy Act some supporting sur la protection de la vie privée, forms may have been removed quelques formulaires secondaires from this thesis. ont été enlevés de cette thèse. While these forms may be included Bien que ces formulaires in the document page count, aient inclus dans la pagination, their removal does not represent il n'y aura aucun contenu manquant. any loss of content from the thesis. ••• Canada "Engineering is the science of economy, of conserving the energy, kinetic and potential, provided and stored up by nature for the use of man. It is the business of engineering ta 'utilize this energy ta the best advantage, sa that there may be the least possible waste. " William A. Smith, 1908 ii ABSTRACT Experiments to measure (i) the reactivity oflithium peroxide and lithium oxide in arnbient air as a function of relative humidity and reactant particle size, (ii) the solubility of lithium hydroxide and lithium hydroxide monohydrate in three alcohols, namely methanol, ethanol and 1 and 2-propanol, as a function of time and temperature, (iii) the efficiency of the production of lithium peroxide in alcohol medium as a function of the concentration of LiOH.H20 in methanol, the concentration of hydrogen peroxide, the kind of alcohol, the kind of feed material, and temperature and the time of mixing, (iv) the analysis of the precipitates, (v) the temperature of the precipitate decomposition in isothermal and non­ isothermal conditions in arnbient and neutral conditions as function of time, (vi) the activation energy of the precipitate decomposition, (vii) the temperature of the lithium peroxide decomposition in isotherrnal and non-isothermal conditions as function of time and (viii) the activation energy oflithium peroxide decomposition were performed. The purpose of the study was to gather the data necessary to evaluate the production of lithium peroxide, Lh02, and subsequently lithium oxide, LhO, to be used as a feed for a silicothermic reduction process for the production of metallic lithium. The proposed basis for the production of Lh02 was the conversion of lithium hydroxide or lithium hydroxide monohydrate by hydrogen peroxide in an alcohol medium. Alcohols were chosen because they are members of a class of non-aqueous solvents that can selectively dissolve the anticipated contarninants while precipitating the desired products. It was found that the addition ofhydrogen peroxide to alcohol solutions containing lithium hydroxide monohydrate resulted in the formation of lithium peroxide as lithium hydroperoxidate trihydrate with eight adduct molecules of methanol, I.e., Lh02·H202·3H20·SCH30H and involved the peroxide group transfer. The optimum conditions for the production of lithium peroxide were found to be (i) the least water concentration in the system (ii) the use of the ternperature lower than arnbient temperature I~ iii and (iii) fast separation of the precipitate and raffinate to prevent dissociation of the precipitate or dissolving into the raffinate. The high solubility of LiOH.H20 and at thc samc timc thc low solubility of LizC03 and of Liz02 in methanol resulted in selection of methanol as the best alcohol of those studied for the proposed method of Li20 2 production. It also yielded high purity lithium peroxide. The production of Liz02 using H202 (35 %wt) required an excess of hydrogen peroxide equal to 2.6 times the stoichiometric amount. The thermal decomposition of the lithium hydroperoxidate trihydrate precipitate started with the rejection of the adduct methanol molecules, followed by co-evolution ofH20 and H202 from the resulting Liz02·H202·H20. The activation energy of the decomposition reaction of the precipitate was measured as 141 kJ/mol. At temperatures greater than 200 oC, lithium peroxide was found to be very reactive with atrnospheric air. However, in an argon atrnosphere, it rapidly decomposed losing the majority of the oxygen atoms, followed by the graduaI slow diffusion of oxygen gas absorbed on the lithium oxide. IV RESUME Des expériences pour mesurer (i) la réactivité du peroxyde de lithium et de l'oxyde de lithium dans l'air ambiant en fonction de l'humidité relative et de la distribution particulaire des réactants, (ii) la solubilité de l'hydroxyde de lithium et de l'hydroxyde de lithium monohydraté dans trois alcools, à savoir le méthanol, l'éthanol et le 1 et 2- propanol, en fonction du temps et de la température, (iii) l'efficacité de production du peroxyde de lithium en milieu alcoolique en fonction de la concentration de LiOH.H20 dans le méthanol, la concentration de peroxyde d'hydrogène, le type d'alcool, le type d'alimentation, et la température et la durée de mélange, (iv) l'analyse des précipités, Cv) la température de décomposition des précipités en conditions isothermes et non-isothermes en milieux ambiant et neutre en fonction du temps, (vi) l'énergie d'activation de décomposition des précipités, (vii) la température de décomposition du peroxyde de lithium en conditions isothermes et non-isothermes en fonction du temps et (viii) l'énergie d'activation de décomposition du peroxyde de lithium furent effectuées. Le but de cette étude était de récolter les données nécessaires à l'évaluation de la production de peroxyde de lithium, Lh02, et par la suite d'oxyde de lithium, LhO, pour être utilisé comme alimentation pour un procédé de réduction silicothermique pour la production de lithium métallique. La base proposée pour la production de Lh02 était la conversion d'hydroxyde de lithium ou d'hydroxyde de lithium monohydraté par le peroxyde d'hydrogène en milieu alcoolique. Les alcools furent choisis car ils font parti des membres de la famille des solvants non-aqueux qui peuvent dissoudre sélectivement les " contaminants engendrés tout en précipitant les produits désirés. Il fut établi que l'addition de peroxyde d'hydrogène aux solutions alcooliques contenant de l'hydroxyde de lithium monohydraté résultait en la formation de peroxyde de lithium sous la forme d'hydroperoxydes trihydratés avec huit molécules d'alcool liées, i.e. Lh02'H202'3H20'8CH30H et impliquant le transfert du groupe peroxyde. Les conditions optimales pour la production de peroxyde de lithium furent établies comme étant (i) v l'absence d'eau dans le system (ii) l'utilisation de températures inferieures à la température ambiante et (iii) la décantation rapide des précipités. Le Lh02 dans le méthanol résulta en la sélection du méthanol comme étant le meilleur alcool étudié pour la méthode proposée de production de Lh02. Ceci produisit aussi du peroxyde de lithium de haute pureté. La production de LhO utilisant du H20 2 (35 %m) demanda un excès de peroxyde d'hydrogène égal à 2.6 fois la quantité stoichiométrique. La décomposition thermique des précipités d'hydroxyperoxydes trihydratés de lithium débuta avec le rejet du méthanol lié, suivit par la co évolution de H20 et de H202 provenant de Lh02·H202·H20. L'énergie d'activation de la réaction de décomposition des précipités fut mesurée à 141 kJ/mol. A des températures supérieures à 200°C, le peroxyde de lithium apparut comme étant très réactif avec l'air atmosphérique. Cependant, dans une atmosphère d'argon, il se décomposa rapidement perdant la majorité des atomes d'oxygène, suivit par la lente graduelle diffusion de l'oxygène gazeux absorbé sur l'oxyde de lithium. VI ACKNOWLEDGMENTS l would like to express my sincerest appreciation to my supervisor, Professor Ralph Harris for his guidance and support throughout my studies in McGill. His approach to scientific issues encouraged me to broaden my insight beyond mere engineering and technical aspects. l would like to extend my greatest thanks to Prof. Janusz Kozinski, who graciously offered support for my research. l am grateful to Monique Riendeau for her assistance in the use of analytical instruments of the Department, Guillermo Mendoza-Suarez for performing TGAIDT A analysis. l am also thankful to Vincent Menard for translation of the abstract of my thesis to French. My grateful thanks go to Barbara Hanely, who always assisted me and patiently answered all my questions. Special thanks to John Roumeliotis for his perpetuaI assistance and helpful advice throughout the research all along, Graeme Goodall for proofreading the thesis, Sina Kashani-Nejad and Sadegh Firoozi for their friendship and outstanding help.
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