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Carbon Materials Synthesis by Hydrothermal Carbonization of Olive Stones : Process and Product Characterization Asma Jeder

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Carbon Materials Synthesis by Hydrothermal Carbonization of Olive Stones : Process and Product Characterization Asma Jeder Carbon materials synthesis by Hydrothermal Carbonization of olive stones : Process and Product Characterization Asma Jeder To cite this version: Asma Jeder. Carbon materials synthesis by Hydrothermal Carbonization of olive stones : Process and Product Characterization. Chemical Sciences. Université de Lorraine; Université de Gabès (Tunisie), 2017. English. NNT : 2017LORR0219. tel-01906214 HAL Id: tel-01906214 https://hal.univ-lorraine.fr/tel-01906214 Submitted on 3 Dec 2018 HAL is a multi-disciplinary open access L’archive ouverte pluridisciplinaire HAL, est archive for the deposit and dissemination of sci- destinée au dépôt et à la diffusion de documents entific research documents, whether they are pub- scientifiques de niveau recherche, publiés ou non, lished or not. The documents may come from émanant des établissements d’enseignement et de teaching and research institutions in France or recherche français ou étrangers, des laboratoires abroad, or from public or private research centers. publics ou privés. AVERTISSEMENT Ce document est le fruit d'un long travail approuvé par le jury de soutenance et mis à disposition de l'ensemble de la communauté universitaire élargie. Il est soumis à la propriété intellectuelle de l'auteur. Ceci implique une obligation de citation et de référencement lors de l’utilisation de ce document. D'autre part, toute contrefaçon, plagiat, reproduction illicite encourt une poursuite pénale. Contact : [email protected] LIENS Code de la Propriété Intellectuelle. articles L 122. 4 Code de la Propriété Intellectuelle. articles L 335.2- L 335.10 http://www.cfcopies.com/V2/leg/leg_droi.php http://www.culture.gouv.fr/culture/infos-pratiques/droits/protection.htm THÈSE Pour l‘obtention du double titre de : DOCTEUR de L‘UNIVERSITÉ DE LORRAINE Spécialité: Chimie Et DOCTEUR du L‘ÉCOLE NATIONALE D‘INGÉNIEURS DE GABES Spécialité: Génie Chimique et procédés Présentée par : Asma JEDER Matériaux carbonés par voie hydrothermale à partir de noyaux d'olive: étude du procédé, caractérisation des produits et applications Thèse soutenue publiquement le 14 décembre 2017 à Gabés devant le jury composé de : M Mehrez ROMDHANE Professeur de l‘Ecole Nationale d‘Ingénieur de Gabés Examinateur M. Hamza EL FIL Professeur de Centre de Recherche et des Rapporteur Technologies des Eauxde Borj-Cédria M. Jean-Michel LEBAN Directeur de Recherches, Inra, Xylologist Rapporteur Mme Andreea PASC Maître de conférencesNANO Group, HDR, MC Examinatrice Mme Vanessa FIERRO Directeur de Recherches au CNRS, HDR, IJL Directrice de thèse M. Abdelmottaleb Professeur de l‘Ecole Nationale d‘Ingénieur de Gabés Directeur de thèse OUEDERNI Institut Jean Lamour –UMR 7198- Département N2EV – Equipe 402 ENSTIB - CS 60036- 88026 EPINAL Cedex Université de Lorraine – Pôle M4 - Collegium Sciences et Technologie Ecole Nationale d'Ingénieurs de Gabès, Université de Gabès, Rue Omar Ibn Elkhattab, 6029 Gabès, Tunisie ABSTRACT Asma JEDER Matériaux carbonés par voie hydrothermale à partir de noyaux d'olive: étude du procédé, caractérisation des produits et applications Encadré par: Abdelmottaleb Ouederni and Vanessa Fierro La carbonisation hydrothermale transforme les déchets municipaux (copeaux de bois, boues d'épuration, bagasse, feuilles…) en un produit solide appelé bio-charbon. Le produit hydrothermal connu sous le nom hydrochar est fréquemment utilisé comme carburant ou engrais, mais aussi il pourrait être converti en un produit à haute valeur ajoutée, à savoir le charbon actif. L‘objectif principal de cette thèse est d‘étudier la transformation de grignon d‘olive, précurseur lignocellulosique largement disponible en Tunisie et en pays méditerranéen, en hydrochar et en charbon actif. Dans cette étude, un réacteur discontinu de laboratoire a été conçu et construit. Les grignons d‘olive transformés en hydrochar ont été préparés à différentes sévérités et avec addition de sels, acide et ammoniac. Les hydrochars ont été caractérisés par plusieurs méthodes d‘analyse. L‘eau de traitement de la carbonisation hydrothermale a été analysée et les résultats montrent qu‘elle contient des composants à haute valeur ajoutée comme le furfural et le 5-HMF. Les charbons actifs ont été préparés à partir du hydrochar suivant des voies d‘activation physique (à l‘aide de l‘agent d‘activation CO2) et voies d‘activation chimique (par l‘agent d‘activation KOH). Les matériaux obtenus ont une surface spécifique élevée (1400 m2g-1) et aussi une chimie de surface riche en groupe fonctionnel. Les performances de ces charbons actifs dans l‘adsorption de molécules pharmaceutiques en phase liquide et de l‘hydrogène en phase gazeuse ont été examinées. Des capacités intéressantes ont été relevées pour les deux applications. Mots-clés : Carbonisation hydrothermale, charbon actif, biomasse lignocellulosique, adsorption de molécules pharmaceutiques, adsorption d‘hydrogène. ABSTRACT Carbon materials synthesis by Hydrothermal Carbonization of olive stones: Process and Product Characterization Asma JEDER Advisors: Abdelmottaleb Ouederni and Vanessa Fierro Hydrothermal carbonization process uses green waste from municipalities (Wood chips, sewage sludge, bagasse, leaves …) to produce solid bio-coal. The solid HTC product known as hydrochar commonly used as a fuel or fertilizer but it could be converted also into high- value products like activated carbon. The principal purpose of this thesis is to study the conversion of olive stones, widely available lignocellulosic biomass in Tunisia and Mediterranean country, into hydrochar and then activated carbon. In this study, a laboratory scale batch reactor has been designed and built. The hydrothermally carbonized olive stones were prepared at different reaction severity and with addition of salts, acid or ammonia. All prepared hydrochar are characterized by different analysis methods. The HTC water was also analyzed and the results show that HTC-liquid contains high added value components such as furfural and 5-HMF. The hydrothermally carbonized olive stones were activated by both physical activation, using CO2 and chemical activation, using KOH. The materials had high surface area (as high as 1400 m2 g-1) and rich surface chemistry. The potential for pharmaceuticals (Ibuprofen and Metronidazole) and hydrogen adsorption were assessed for HTC-activated carbon and they showed good performance in both application. Keywords: Hydrothermal Carbonization, Carbon materials, olive stones, Pharmaceutical Adsorption, Hydrogen Adsorption Acknowledgement I would like to thank my supervisors Pr. Abdelmottaleb Ouederni and Dr. Vanessa Fierro for providing interesting research subject to work on it. In addition, I would like to thank them for their professional help to the realization of this thesis. I am also grateful to Pr Alain Cerlzard for accepting me on their group and to Dr Vanessa Fierro for giving me the opportunity to receive a scholarship from Lorraine University. I would like also to thank the member of jury: Mr Mehrez Romdhane, Mr Hamza El Fil, Mr Jean-Michel LEBAN and Mrs Andrea PASC Special thanks to Philippe Gadonneix for being patient and for performing some analysis during my work in the Tunisian laboratory. Thanks to my friends in ENIG Ines, Hanen, Marwa, Manel, Abir, Besma, Souhir, Zohour, Amina, Mouzaina, Fatma, khaoula, Ameni we spent a good time and I have been lucky to work with you, Asma and Hayet for their patient despite my numerous questions. And my colleagues in ENSTIB Flavia, Luda, Andrejz, Guiseppe, Antonio, Taher, Clara, Jimena, Sébestian, Marie and angela, it was pleasure to meet you. Special thanks to Elmouwahidi abdelhaim and Sihem amirou for their moral support in my most difficult time. I would like to thank also Eric Masson for his collaboration in Project Title: Understanding hydrothermal Carbonization mechanisms Great thanks to my parents, brothers Chokri and Chawki, my sister Leila, my little nephew Hassen and my step-sister Maria-Olympia for their support and encouragement; you are the most precious person in my life. Table of contents Résumé de la thèse ................................................................................................................................. 1 Introduction ........................................................................................................................................... 14 Chapter 1: State of the art ..................................................................................................................... 14 I.1 Lignocellulosic biomass ........................................................................................................ 15 I.1.1 Cellulose ............................................................................................................................ 16 I.1.2 Hemicellulose .................................................................................................................... 17 I.2.3 Lignin ................................................................................................................................ 17 I.1.4 Olive stones ....................................................................................................................... 18 I.2 Hydrothermal carbonization .................................................................................................. 19 I.2.1 HTC mechanism ................................................................................................................ 21 I.2.2 Water properties ...............................................................................................................
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