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Étude Des Saumures Naturelles Et Industrielles: Approche Expérimentale Et Par Modélisation De L'extraction Du Lithium Par Évaporation

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Étude Des Saumures Naturelles Et Industrielles: Approche Expérimentale Et Par Modélisation De L'extraction Du Lithium Par Évaporation THÈSE UNIVERSITÉ DE PAU ET DES PAYS DE L’ADOUR ÉCOLE DOCTORALE DES SCIENCES EXACTES ET LEURS APPLICATIONS Présentée et soutenue le 13 octobre 2017 par Anne-Laure THADEE pour obtenir le grade de docteur de l’Université de Pau et des Pays de l’Adour Spécialité : Génie des Procédés Etude des saumures naturelles et industrielles : approche expérimentale et par modélisation de l’extraction du lithium par évaporation MEMBRES DU JURY RAPPORTEURS • Mme. Karine BALLERAT-BUSSEROLLES IR-CNRS Docteur-HDR / Université Blaise Pascale-ICCF • M. Lionel MERCURY Professeur / Université d’Orléans EXAMINATEURS • M. Arnault LASSIN Docteur / BRGM • Mme. Anna CHROSTOWSKA Professeur/Université de Pau et des Pays de l’Adour DIRECTEURS • M. Pierre CÉZAC Professeur / Université de Pau et de Pays de l’Adour • M. Jean-Paul SERIN Professeur / Université de Pau et de Pays de l’Adour INVITE • M. Sylvain GUIGNOT Docteur BRGM Contenu Liste des figures ....................................................................................................................................... 5 Liste des tableaux .................................................................................................................................... 7 Introduction ........................................................................................................................................... 11 1. Bibliographie ...................................................................................................................................... 15 1.1 Usage et demande en sels de lithium ......................................................................................... 15 1.2 Les ressources en lithium ............................................................................................................ 18 A. Sources de lithium ................................................................................................................. 18 B. Formation des saumures lithinifères ..................................................................................... 20 C. Répartition des ressources en lithium ................................................................................... 22 D. Composition des saumures majeures ................................................................................... 23 1.3 Les procédés de production des sels de lithium ......................................................................... 26 A. Procédés de production de sels de lithium à partir de saumures ......................................... 27 B. Comparaison des procédés d’extraction du lithium sous forme de carbonates .................. 32 C. Extraction du lithium et impacts sur l’environnement ......................................................... 34 1.4. Conclusion du chapitre bibliographique .................................................................................... 35 Références du chapitre bibliographique ........................................................................................... 36 2. Modélisation des saumures .............................................................................................................. 43 2.1. Description thermodynamique et géochimique des saumures ................................................. 43 A. Propriétés macroscopiques des saumures ............................................................................ 43 B. Propriétés thermodynamiques et géochimiques .................................................................. 45 C. Définitions ............................................................................................................................. 50 D. Modèle de Pitzer ................................................................................................................... 50 2.2. Modélisation ............................................................................................................................... 53 A. L’outil de modélisation : PhreeqC ......................................................................................... 53 B. Optimisation des systèmes électrolytiques lithinifères ........................................................ 55 2.3. Scénario, prédimensionnement et sensibilité ............................................................................ 65 A. Simulation de l’évaporation d’une saumure naturelle ......................................................... 65 B. Etude de sensibilité ............................................................................................................... 69 C. Scénario exploratoire de production de zabuyelite .............................................................. 75 D. Conclusion ............................................................................................................................. 79 2.4 Conclusion générale du chapitre de modélisation des saumures ............................................... 80 3 Références du chapitre modélisation ............................................................................................... 81 3. Expérimental ..................................................................................................................................... 85 3.1. Matériels..................................................................................................................................... 85 A. Les pilotes de travail .............................................................................................................. 85 B. Techniques d’analyse du solide ............................................................................................. 87 C. Techniques d’analyses liquides : la chromatographie ionique.............................................. 89 D. Produits utilisés ..................................................................................................................... 91 3.2. Expériences ................................................................................................................................. 92 A. Etalonnage des appareils de chromatographie ionique........................................................ 92 B. Préparation des saumures..................................................................................................... 94 C. Essais sur l’enceinte climatique ............................................................................................. 96 D. Essais sur le pilote de cristallisation .................................................................................... 102 3.3. Discussion ................................................................................................................................. 107 3.4 Conclusion du chapitre expérimental ....................................................................................... 111 Conclusion ........................................................................................................................................... 113 Annexes ............................................................................................................................................... 116 Annexe A : Liste des brevets étudiés ............................................................................................... 117 Annexe B : Diagrammes de solubilité des systèmes Li-Na-K-Ca-Mg-Cl-SO4-CO3............................. 121 Annexe C: Influence de la température sur la solubilité du Li2CO3 ................................................. 129 Annexe D : Détail des analyses TEM pour identification des cristaux............................................. 131 4 Liste des figures Figure 1 : Consommation de lithium par secteur d’activité, d’après Jaskula (2016) ............................ 15 Figure 2 : Evolution de la consommation mondiale de lithium au cours du temps .............................. 17 Figure 3 : Exemple d’une roche lithinifère (Brown et al., 2016) ........................................................... 19 Figure 4 : Modèle de dépôt des saumures lithinifères (Bradley et al. 2013) ........................................ 21 Figure 5 : Distribution des gisements de lithium (Labbé et Daw 2012) ................................................ 22 Figure 6 : Estimation de la teneur en lithium des différentes saumures (% massique) ........................ 24 Figure 7 : Sels de lithium et leurs applications (Ebensperger et al. 2005) ............................................ 26 Figure 8 : Déroulement d'un procédé d'extraction ............................................................................... 27 Figure 9 : Illustration de la pression osmotique 훱 ................................................................................ 49 Figure 10 : Exemple d’un diagramme de solubilité pour le système Li-K-Cl à 25°C .............................. 60 Figure 11 : Exemple d’ajustement pour le système Li-Na-SO4, ............................................................. 61 Figure 12 : Exemple d’ajustement pour le système Li-Ca-Cl (Lassin, com. pers.) ................................. 62 Figure 13 : Simulation de l'évaporation d'une saumure type Atacama (naturelle) .............................. 66 Figure 14 :Simulation de l'évaporation de la solution Atacama2'......................................................... 68 Figure 15 :Séquence d'évaporation pour Atacama 2' + 0.2 mol de Na2CO3 et suivi du pH................... 69 Figure 16 : Séquence d’évaporation simulée pour Atacama2’ + 0.4 mol de Na2CO3 et suivi du pH ....
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