Os revestimentos cerâmicos aderidos têm grandes vantagens estéticas e funcionais e seu emprego no mercado nacional vem sendo crescente, sobretudo com o uso de placas de porcelanato. Essas vantagens somente se concretizam com uma adequada durabilidade e vida útil, o que não vem ocorrendo com esses revestimentos aplicados em bases sujeitas a deformações e ou movimentações, como o caso de fachadas. Como camada de ligação entre o substrato e a placa cerâmica, as argamassas colantes apresentam papel fundamental para o revestimento cerâmico, tais como: suportar deformações e ou movimentações diferenciais, apresentar resistência mecânica duradoura e ter capacidade de aderir com segurança em qualquer substrato e placa cerâmica. O objetivo desse trabalho foi de estudar o comportamento de argamassas colantes com a aditivação de látex acrílico. Foi realizado um estudo experimental comparativo entre argamassas colantes monocomponentes e argamassas colantes aditivadas com látex acrílico. Para verificar o comportamento que essa aditivação proporciona, foram realizados ensaios de resistência de aderência, flexibilidade, resistência à compressão, resistência à tração na flexão com determinação de módulo de deformação e tempo em aberto com placas de porcelanato. Os resultados mostraram de uma forma geral que a aditivação de argamassas colantes proporcionam aumento significativo na flexibilidade. Ocorre melhora na resistência de aderência, resistência à compressão e resistência à tração na flexão e também na capacidade de absorver deformações com o aumento do teor de polímero/argamassa. A aderência em placas de baixa porosidade como o porcelanato é melhorada e o tempo em aberto de laboratório também é estendido para as argamassas modificadas com látex. / The directed adhere ceramic tiles has aesthetic and functional advantages, and its use in the national market is increasing specially with the use along with porcelain tile. These advantages can only be seen though, if the system has adequate durability and service live, which doesn\'t happen once it is applied on irreversible or cyclic movement basis as building façades. As the clingy layer between the ceramic tile and the substrate, the tile adhesives have fundamental importance for the directed adhered ceramic tile, working on deformation and movements support capability, long-term durability mechanic resistance and safety and reliability to adhere on all type of substrates and ceramic tile. The purpose of this work was to study the behavior of dry set mortar modified with acrylic latex. An experimental study has been done, comparing dry set mortar to acrylic latex Portland cement mortar. To verify the behavior that the latex provides, the following tests were realized: tensile bond adhesion, deformability, compressive strength and tensile strength with deformation modulus and open time with porcelain tile. The results showed in general, that the latex improved the flexibility of dry set mortar and the improvement of the tensile adhesion, compressive and tensile strength and deformability capacity by increasing the polymer/mortar content. The adhesion and open time in porcelain tile has been improved with latex Portland cement mortar.

Les propriétés des latex, produits aux larges applications industrielles, dépendent d’un grand nombre de facteurs : le type de monomère, les stabilisants, les initiateurs ou encore la taille des particules. Les procédés comme les formulations utilisés sont nombreux. La répartition des particules – taille moyenne, écart moyen, polydispersité – est souvent gérée par une étape de coagulation qui suit la nucléation, menée dans un post réacteur. La maîtrise de la coagulation nécessite un contrôle parfait du procédé. Ces travaux de thèse, réalisés dans le cadre de l’ANR SCALE-UP, ont pour objectif d’étudier la coagulation de latex acryliques dans un procédé continu de taille millimétrique opérant en régime laminaire. Les mécanismes de coagulation sont mis en évidence dans des conditions physico-chimiques et hydrodynamiques contrôlées, et l’influence des différents paramètres sur la cinétique de coagulation est quantifiée. Une méthodologie à l’interface de plusieurs domaines (génie des procédés, physico-chimie, numérique) est adoptée. Dans un premier temps, les bases essentielles à la compréhension du phénomène de coagulation sont introduites. Cette étude permet de distinguer deux types de coagulation : péricinétique (liée au mouvement Brownien), et orthocinétique (reliée au cisaillement). Les modèles associés sont présentés, et l’influence du procédé discutée. La déstabilisation des latex par coagulation Brownienne est ensuite examinée. Après avoir introduit les principales techniques analytiques existantes et caractérisé les latex étudiés, une étude physico-chimique est menée. Un modèle permettant d’estimer le temps de coagulation en fonction des conditions de pH, force ionique et concentration du milieu est proposé, basé sur des mesures de mobilité électrophorétiques. La troisième partie consiste en l’étude hydrodynamique par CFD de deux réacteurs millimétriques : un tube enroulé et un réacteur intensifié (Dean-Hex), comparés à un tube droit. Le régime visé est le régime laminaire. La coagulation orthocinétique dépendant des taux de cisaillement dans le réacteur, l’objectif est d’observer l’écoulement ainsi que les distributions de ces taux dans le réacteur, afin d’anticiper l’influence du changement de géométrie sur la coagulation. Des informations locales sur l’écoulement sont obtenues par suivi lagrangien de particules. La répartition des taux de cisaillement comme les temps passés dans les zones aux plus forts taux sont très différents selon le réacteur, laissant présager des résultats différents en termes de mécanismes de coagulation et de taille finale des agrégats. Le quatrième chapitre présente les résultats expérimentaux obtenus en milliréacteur. Un pilote a été développé, permettant la mise en écoulement des fluides par pressurisation de réservoirs. La coagulation de latex de trois tailles initiale différente y est menée. Les échantillons prélevés le long du réacteur sont analysés par diffraction laser (Mastersizer 2000). Outre les distributions de taille, des informations sur la dimension fractale des agrégats sont extraites. Dans le cas de réacteurs tubulaires enroulés, des résultats en fonction de la concentration, du pH et du débit sont obtenus, permettant de déterminer l’influence de ces paramètres sur la cinétique. Des informations sur l’équilibre agrégation-rupture sont également disponibles à partir des expériences réalisées sur un des latex. Le régime d’écoulement laminaire, impliquant un mode de collision balistique, permet d’obtenir des agrégats de forme pratiquement sphérique. Une discussion concernant les conditions de travail en milliréacteur est menée, afin de cerner l’applicabilité de ce procédé. Dans une dernière partie, une méthode d’estimation de noyaux cinétiques, par Quadrature des Moments est présentée et appliquée à des résultats obtenus en réacteur de Taylor-Couette. De par le contrôle de l’hydrodynamique qu’il propose, un tel réacteur est parfaitement adapté à cette application. / Due to their large applicability, latexes are widely used in industries. Their properties depend on many parameters including the monomer, stabilizers and initiators used, and also the particle size. The particle size distribution of these suspensions is often regulated by a coagulation step, occurring after nucleation in a reactor. Coagulation control thus means perfect process control. This thesis, led in the framework of the project ANR SCALE-UP, aims at studying acrylic latex coagulation in millimetric-scale reactors in laminar flow. Coagulation mechanisms are highlighted in controlled physico-chemical and hydrodynamic conditions, and the influence of the various parameters on coagulation kinetics is quantified. A scientific methodology based on chemical engineering, physical-chemistry and fluid mechanics is employed. The first part of the thesis aims at presenting the theoretical basis of this work, where by the differences between perikinetic coagulation (driven by Brownian motion) and orthokinetic coagulation (related to shear) are distinguished. Models related to coagulation and rupture of aggregates are presented. As the reactor geometry is expected to have a significant impact on coagulation due to its sensitivity to shear, the influence of the geometry is also discussed. The second part of the work focuses on the stability of latex, which is related to Brownian coagulation. The main analysis techniques related to the size determination of aggregates are firstly discussed and a complete characterization of the latex used is presented. A physical-chemical study is then performed, resulting in the proposition of a model that allows the calculation of a coagulation time as a function of the properties of the latex suspension, namely pH, concentration and ionic strength. The third part presents a CFD study of two millimetric-scale reactors – a coiled tube and a meandering channel (Dean-Hex) reactor – and compares them with a straight tubular reactor. This work aims at studying the flow properties and shear rates produced inside these reactors in order to better understand their influence on the coagulation process. At equal flow rates, the Dean-Hex reactor proposes a narrower shear rate distribution compared with the tubular geometries, however very high shear rates are also generated and these are likely to modify the particle size distribution by breaking the aggregates. The fourth part of the thesis details the experimental results of the latex coagulation process in the coiled tube. A pilot-scale set-up was designed and constructed allowing the reactant feeds to be regulated and product sampling at eight points such that coagulation could be monitored with residence time. Samples were analyzed using dynamic light scattering (Mastersizer 2000), which enable the fractal dimension of aggregates to be obtained. The results of aggregate growth as a function of pH, flowrate and latex concentration are presented and provide information on the aggregation kinetics. A more concentrated latex is used to gain insight on aggregation-rupture equilibrium. Considering the fractal dimension of the larger aggregates, the equilibrium size was found to linearly decrease with the average shear rate. Also, laminar flow was found to result in more spherical aggregates than what is obtained in a batch reactor due to the ballistic collision mode involved. A discussion on the effects of experimental conditions (concentration, pH and flow rates) and the limitations of millimetric-scale equipment for latex aggregation is initiated. The final part of the work aims at introducing a population balance model for the aggregation process using the Quadrature Method of Moments (QMOM) and results obtained in a Taylor-Couette reactor. This device offers good control of hydrodynamics and it istherefore well suited to the determination of aggregation and rupture kernels.

Os revestimentos cerâmicos aderidos têm grandes vantagens estéticas e funcionais e seu emprego no mercado nacional vem sendo crescente, sobretudo com o uso de placas de porcelanato. Essas vantagens somente se concretizam com uma adequada durabilidade e vida útil, o que não vem ocorrendo com esses revestimentos aplicados em bases sujeitas a deformações e ou movimentações, como o caso de fachadas. Como camada de ligação entre o substrato e a placa cerâmica, as argamassas colantes apresentam papel fundamental para o revestimento cerâmico, tais como: suportar deformações e ou movimentações diferenciais, apresentar resistência mecânica duradoura e ter capacidade de aderir com segurança em qualquer substrato e placa cerâmica. O objetivo desse trabalho foi de estudar o comportamento de argamassas colantes com a aditivação de látex acrílico. Foi realizado um estudo experimental comparativo entre argamassas colantes monocomponentes e argamassas colantes aditivadas com látex acrílico. Para verificar o comportamento que essa aditivação proporciona, foram realizados ensaios de resistência de aderência, flexibilidade, resistência à compressão, resistência à tração na flexão com determinação de módulo de deformação e tempo em aberto com placas de porcelanato. Os resultados mostraram de uma forma geral que a aditivação de argamassas colantes proporcionam aumento significativo na flexibilidade. Ocorre melhora na resistência de aderência, resistência à compressão e resistência à tração na flexão e também na capacidade de absorver deformações com o aumento do teor de polímero/argamassa. A aderência em placas de baixa porosidade como o porcelanato é melhorada e o tempo em aberto de laboratório também é estendido para as argamassas modificadas com látex. / The directed adhere ceramic tiles has aesthetic and functional advantages, and its use in the national market is increasing specially with the use along with porcelain tile. These advantages can only be seen though, if the system has adequate durability and service live, which doesn\'t happen once it is applied on irreversible or cyclic movement basis as building façades. As the clingy layer between the ceramic tile and the substrate, the tile adhesives have fundamental importance for the directed adhered ceramic tile, working on deformation and movements support capability, long-term durability mechanic resistance and safety and reliability to adhere on all type of substrates and ceramic tile. The purpose of this work was to study the behavior of dry set mortar modified with acrylic latex. An experimental study has been done, comparing dry set mortar to acrylic latex Portland cement mortar. To verify the behavior that the latex provides, the following tests were realized: tensile bond adhesion, deformability, compressive strength and tensile strength with deformation modulus and open time with porcelain tile. The results showed in general, that the latex improved the flexibility of dry set mortar and the improvement of the tensile adhesion, compressive and tensile strength and deformability capacity by increasing the polymer/mortar content. The adhesion and open time in porcelain tile has been improved with latex Portland cement mortar.

Made available in DSpace on 2014-12-17T15:41:43Z (GMT). No. of bitstreams: 1 ZilvanMS.pdf: 850138 bytes, checksum: 377846a49fcf47805db83b68c5e1b5f7 (MD5) Previous issue date: 2007-07-31 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior / Latexes based on acrylic acid, acrylamide, ethyl methacrylate, and ethyl acrylate were synthesized via emulsion polymerization with different monomer compositions. The resultant latices were thickened with different molar ratios of NaOH to acrylic acid and were analyzed in terms of acid‐basis titrimetry, turbidimetry, rheology, and tensiometry. Titrimetry, turbidimetry, and rheometry were used to analyze factors such as carboxyl group availability and particle solubilization, tensiometry monitoring the influence of carboxyl neutralization on polymer‐surfactant interactions. For the acrylic acid content used in this work (20 wt%), the results indicated that as carboxyl groups distribution became more homogeneous, the process of latex thickening became more effective / L?tices baseados em ?cido acr?lico, acrilamida, acrilato de etila e metacrilato de etila foram sintetizados via polimeriza??o em emuls?o com diferentes composi??es monom?ricas. Os l?tices resultantes foram espessados a diferentes raz?es molares de NaOH/?cido acr?lico. Titrimetria ?cido‐base, turbidimetria, reometria e tensiometria foram usados para analisar fatores tais como a disponibilidade de grupos carboxila e a solubiliza??o de part?culas, a tensiometria sendo usada para monitorar a influ?ncia da neutraliza??o de grupos carboxilas nas intera??es pol?mero‐surfactante. Para o teor de ?cido acr?lico usado neste trabalho (20 m/m%), os resultados indicaram que, a medida em que a distribui??o de grupos carboxilas torna‐se mais homog?nea, o processo de espessamento tornou‐se mais efetivo