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Polyamidoamine Epichlorohydrin-Based Papers : Mechanisms of Wet Strength Development and Paper Repulping Eder José Siqueira

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Polyamidoamine Epichlorohydrin-Based Papers : Mechanisms of Wet Strength Development and Paper Repulping Eder José Siqueira Polyamidoamine epichlorohydrin-based papers : mechanisms of wet strength development and paper repulping Eder José Siqueira To cite this version: Eder José Siqueira. Polyamidoamine epichlorohydrin-based papers : mechanisms of wet strength devel- opment and paper repulping. Other. Université de Grenoble, 2012. English. NNT : 2012GRENI035. tel-00952991 HAL Id: tel-00952991 https://tel.archives-ouvertes.fr/tel-00952991 Submitted on 28 Feb 2014 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. THÈSE Pour obtenir le grade de DOCTEUR DE L’UNIVERSITÉ DE GRENOBLE Spécialité : Mécanique des Fluides, Energétique, Procédés Arrêté ministériel : 7 août 2006 Présentée par Eder José SIQUEIRA Thèse dirigée par Evelyne MAURET et codirigée par Mohamed Naceur BELGACEM préparée au sein du LGP2 – Laboratoire de Génie des Procédés Papetiers dans l'École Doctorale IMEP2 POLYAMIDEAMINE EPICHLOROHYDRIN-BASED PAPERS: MECHANISMS OF WET STRENGTH DEVELOPMENT AND PAPER REPULPING Thèse soutenue publiquement le 05 juin 2012, devant le jury composé de : Madame Ana Paula COSTA Professeur - Universidade da Beira Interior. Covilhã - PORTUGAL, Rapporteur Madame Marie-Pierre LABORIE (Présidente du jury) Professeur - Institute of Forest Utilization and Works Science - Albert- Ludwigs University of Freiburg. Freiburg - ALLEMAGNE, Rapporteur Monsieur Jean-Pierre JOLY Chargé de Recherche CNRS, Université Henri Poincaré Nancy I. Vandoeuvre - FRANCE, Examinateur Madame Séverine SCHOTT Docteur Ingénieur - Ahlstrom LabelPack. Pont-Evêque - FRANCE, Examinateur Madame Evelyne MAURET Professeur – Institut National Polytechnique de Grenoble (PAGORA). FRANCE, Directeur de Thèse Monsieur Mohamed Naceur BELGACEM Professeur – Institut National Polytechnique de Grenoble (PAGORA). FRANCE, Directeur de Thèse Eder José Siqueira ABSTRACT Polyamideamine epichlorohydrin (PAE) resin is a water soluble and the most used permanent wet strength additive in alkaline conditions for preparing wet strengthened papers. In this thesis, we studied some properties of PAE resins and wet strengthened papers prepared from them. In order to elucidate PAE structure, liquid state, 1H and 13C NMR was carried out and permitted signals assignment of PAE structure. PAE films were prepared to study cross-linking reactions and then thermal and ageing treatments were performed. According to our results, the main PAE cross-linking reaction occurs by a nucleophilic attack of N atoms in the PAE and/or polyamideamine structures forming 2-propanol bridges between PAE macromolecules. A secondary contribution of ester linkages to the PAE cross-linking was also observed. However, this reaction, which is thermally induced, only occurs under anhydrous conditions. The mechanism related to wet strength development of PAE-based papers was studied by using CMC as a model compound for cellulosic fibres and PAE-CMC interactions as a model for PAE- fibres interactions. Based on results from NMR and FTIR, we clearly showed that PAE react with CMC that is when carboxylic groups are present in great amounts. Consequently, as the number of carboxylic groups present in lignocellulosic fibres is considerably less important and the resulting formed ester bonds are hydrolysable, we postulate that ester bond formation has a negligible impact on the wet strength of PAE- based papers. In the second part of this work, a 100% Eucalyptus pulp suspension was used to prepare PAE-based papers. PAE was added at different dosages (0.4, 0.6 and 1%) into the pulp suspension and its adsorption was indirectly followed by measuring the zeta potential. Results indicate that the adsorption, reconformation and/or penetration phenomena reach an apparent equilibrium at around 10 min. Moreover, we showed that the paper dry strength was not significantly affected by the conductivity level (from 100 to 3000 µS/cm) of the pulp suspension. However, the conductivity has an impact on the wet strength and this effect seems to be enhanced for the highest PAE dosage (1%). We also demonstrated that storing the treated paper under controlled conditions or boosting the PAE cross-linking with a thermal post-treatment does not necessarily lead to the same wet strength. Degrading studies of cross-linked PAE films showed that PAE degradation in a persulfate solution at alkaline medium was more effective. A preliminary study of coated and uncoated industrial PAE-based papers was also performed. For uncoated paper, persulfate treatment was the most efficient. For coated papers, all treatments were inefficient in the used conditions, although a decrease of the wet tensile force of degraded samples was observed. The main responsible of the decrease of persulfate efficiency for coated papers was probably related to side reactions of free radicals with the coating constituents. Key-words: polyamideamine epichlorohydrin resin, PAE cross-linking reactions, carboxymethylcellulose, wet strength mechanism, PAE-based papers, polyelectrolytes adsorption, paper recycling. ii Eder José Siqueira RÉSUMÉ EN FRANÇAIS 1. Introduction Le travail présenté dans ce manuscrit s’intéresse au mode d’action des résines thermodurcissables utilisées pour conférer au matériau papier des propriétés spécifiques. En effet, certains papiers sont destinés, au cours de leur usage, à être en contact avec des liquides et en particulier de l’eau. C’est le cas, par exemple, des papiers absorbants, de certains papiers filtres, mais aussi de papiers pour étiquettes ou pour billets de banque. En présence d’eau, les papiers perdent rapidement leur résistance mécanique, essentiellement due à la présence en grand nombre de liaisons hydrogène, d’où la nécessité d’un traitement μ l’objectif est de maintenir un certain niveau de résistance des papiers saturés en eau. Ces traitements consistent à introduire dans la suspension fibreuse, en cours d’élaboration, des pré-polymères cationiques s’adsorbant à la surface des fibres. Après la formation de la feuille de papier, la feuille humide est séchée et c’est au cours de cette étape que s’amorce la réticulation de ces polymères. Elle conduit à la formation d’un réseau tridimensionnel de polymère dans le matelas fibreux. Ce réseau permet au papier de conserver ses propriétés mécaniques lorsqu’il est en contact avec de l’eau. Il présente ce que l’on appelle communément une résistance à l’état humide (REH). Un des inconvénients de ce type de traitement est lié aux difficultés de recyclage des papiers obtenus. Il nécessite un traitement particulièrement intensif et coûteux qui couple une action mécanique (désintégration, dépastillage) à une action chimique (utilisation d’hydroxyde de sodium, par exemple). Même si ces produits sont largement utilisés, les mécanismes mis en jeu que ce soit pour le développement des propriétés de REH ou pour le recyclage ne sont pas totalement compris. Dans ce contexte, ce travail a pour objectif d’étudier le mode d’action de pré-polymères de polyamideamine épichlorhydrine (PAE), couramment utilisés en papeterie pour conférer au matériau papier une résistance à l’état humide (REH). Il s’intéresse à la caractérisation de solutions commerciales de PAE et à l’étude des mécanismes réactionnels de ces pré- polymères. Il traite également de l’effet de certains paramètres de production du papier sur l’efficacité des traitements. Enfin, il apporte de éléments nouveaux sur la compréhension de l’étape de recyclage. iii Eder José Siqueira Le manuscrit est divisé en deux parties : (i.) Caractérisation des résines PAE pour une meilleure compréhension des phénomènes de réticulation, (ii.) Utilisation des résines PAE en papeterie : préparation et recyclage de papiers traités. 1.1. Caractérisation des résines PAE pour une meilleure compréhension des phénomènes de réticulation Dans cette partie, nous nous sommes intéressés à la caractérisation de solutions commerciales de PAE : des analyses spectroscopique en RMN du liquide ont été menées et des titrations colloïdales ont été réalisées en fonction du pH et de la force ionique du milieu. Dans un second temps, un travail approfondi a été conduit pour comprendre les phénomènes de réticulation se produisant dans des films de PAE. Pour ce faire, nous avons effectué : (i.) un travail de recherche bibliographique approfondie du sujet, (ii.) la mise au point de protocoles de formation de films, (iii.) la mise au point d’un protocole de traitement thermique des films pour provoquer de façon reproductible la réticulation de la PAE (polymères thermodurcissables) et ceci en testant différentes températures et durées, (iv.) la caractérisation de ces films : recherche de solvants, comportement dans l’eau, caractérisation par FTIR en transmission principalement, par analyse mécanique dynamique (DMA), par analyse calorimétrique différentielle (DSC), en RMN du solide, étude en microscopie électronique à balayage. La même approche expérimentale a ensuite été appliquée à la caractérisation de films composés de PAE et de carboxy-méthylcellulose (CMC) dans différentes proportions en masse (75%/25% ; 50%/50% ; 25%/75%) avant et après traitement
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