Renata Barbosa

Polyamide 66/Brazilian clay nanocomposites

Polyamide 66 (PA66)/Brazilian clay nanocomposites were produced via direct melt intercalation. A montmorillonite sample from the Brazilian state of Paraiba was organically modified with esthearildimethylammonium chloride (Praepagen), quaternary ammonium salt and has been tested to be used in polymer nanocomposites. The dispersion analysis and the interlayer spacing of the clay particles in matrix were investigated by X-ray diffraction (XRD) and transmission electron microscopy (TEM). Thermal behavior of the obtained systems was investigated by differential scanning calorimetry (DSC), thermogravimetry (TG), and heat deflection temperature (HDT) was reported too. The nanocomposites exhibited a partially exfoliated structure, very interesting HDT values which are higher than those of pure PA66, and good thermal stability.

Efeito de sais quaternários de amônio na organofilização de uma argila bentonita nacional

Bentonite clay, mainly composed by montmorillonite that provides the physical properties, concentrates the majority of the national reserve (62%) in the Paraiba State. The transformation of bentonite clay to organoclay is made with a simple laboratory procedure and this modification can be obtained by cation (Na+ or Ca2+) exchange reaction that are present on the surface and in the interlayer space of the mineral clays by quaternary ammonium salts. In this, the organoclays bentonite were preparedwith four different types of quaternary ammonium salts such as alkyldimethylbenzylammonium chloride (Dodigen), esthearildimethylammonium chloride (Praepagen), cethyltrimethylammonium chloride (Genamin) and cethyltrimethylammonium bromide (Cetremide). The organoclays were characterized by thermogravimetry, X-ray diffraction, chemical analysis and X-ray fluorescence. The results showed that the salts were incorporated in the clay structure, confirming the organophilization. The Praepagen and Cetremide salts presented a higher range of thermal stability.

Preparação de argilas organofílicas e desenvolvimento de nanocompósitos com matrizes poliméricas de polietileno e nylon6. Parte 1: comportamento mecânico

Bentonite clays from Boa Vista/PB were used to obtain organophilic clays. Organophilic clays were obtained with four types of quaternary salts of ammonium: asalkyldimethylbenzylammonium chloride (Dodigen), esthearildimethylammonium chloride (Praepagen), cethyltrimethylammonium chloride (Genamin) and cethyltrimethylammonium bromide (Bromide). The treated clays with salts and untreated clays were characterized by X- ray diffraction (XRD) and Fourier transformed infrared spectroscopy (FTIR). Then, the clays were incorporated into polyethylene (PE) and Nylon6 (PA6) polymer matrices using conventional processing techniques. The mixtures were characterized by XRD, scanning electron microscopy (SEM) and mechanical properties. The results obtained by FTIR showed the presence of specific groups of the salts in the clay, while their intercalation among the clay layers was verified by XRD. As for the mechanical properties, the mixtures were more rigid than the pure polymers.

Nanocompósitos de polietileno/argila bentonita nacional: influência da argila e do agente compatibilizante PE-g-MA nas propriedades mecânicas e de inflamabilidade

High density polyethylene/national bentonite clay nanocomposites were prepared with the melt intercalation technique. The effect of the clay without treatment and clay treated with quaternary ammonium salt Cetremide with polyethylene-graft-maleic anhydride as coupling agent was evaluated. The systems were characterized by flammability, mechanical and rheological properties, X ray diffraction and transmission electron microscopy. In general, the results of X ray diffraction and transmission electron microscopy showed partially exfoliated and/or intercalated structures with higher tensile modulus and torque value. The flammability test showed that the addition of clay in the polymer matrix and PE-g-MA reduced the burning rate, indicating an improved flammability resistance of the nanocomposites. In general, the system containing PE-g-MA coupling agent led to partially exfoliated nanocomposites with higher thermal stability than the high density polyethylene matrix. The polyethylene-graft-maleic anhydride promoted the exfoliation of clay and adhesion between matrix and filler, thus resulting in enhanced mechanical properties.

Morfologia de nanocompósitos de polietileno e poliamida-6 contendo argila nacional

High density polyethylene and nylon 6 nanocomposites with national bentonite clay were prepared with the melt intercalation technique. Different quaternary ammonium salts were used to obtain the organoclays. The unmodified and modified clays with the salts were incorporated in the polymer matrices and different procedures were used for the modification of clays: for the polyethylene nanocomposites, the clay was prepared with four quaternary ammonium salts and for the nylon 6 nanocomposites only one type of quaternary ammonium salt was used, which had its contents varied in the organophilization of the clay. The objective of this work was to obtain polyethylene and nylon 6 nanocomposites. They were characterized by transmission electron microscopy (TEM) and by X-ray diffraction (XRD). The results indicated that the polyethylene/organoclay systems presented structures of intercalated nanocomposites and/or partially exfoliated. The nylon 6/organoclay systems presented an exfoliated morphology with clay particles dispersed in the matrix.

Nanocompósitos de poliamida 6/Argila organofílica: efeito do peso molecular da matriz na estrutura e propriedades mecânicas e termomecânicas

Polyamide 6/organoclay nanocomposites were prepared by the melt intercalation technique. The clay was treated with a quaternary ammonium salt (Genamin) to obtain the organoclay (OMMT), being characterized by X ray fluorescence (XRF) and X ray diffraction (XRD). The results confirmed the incorporation of the salt into the clay structure, i.e. the organophilization. The nanocomposites were obtained with a counter-rotational twin screw extruder with 3 wt.% of clay and characterized by XRD, transmission electron microscopy (TEM), tensile testing, dynamical-mechanical thermal analysis (DMTA) and heat deflection temperature (HDT). The XRD and TEM results showed exfoliated and/or partially exfoliated structures. The tensile properties were superior to those of the pure polyamide 6.The analysis with DMTA and HDT also showed that the incorporation of the organoclay into the polymer matrix increased the rigidity (storage modulus) of the system, confirming the reinforcing effect of the clay on the polymer.

Effect of reprocessing cycles on the degradation of PP/PBAT-thermoplastic starch blends

The solid waste management problems caused by the accumulation of plastics require measures to mitigate the environmental damage, and mechanical recycling of plastics is among the possible solutions. In this context, the present study aimed to evaluate the effects of mechanical recycling on the properties of a polypropylene/poly(butylene adipate co-terephthalate)-thermoplastic starch blend (PP/PBAT-Thermoplastic starch blend) when it was subjected to seven reprocessing cycles by a single-screw extruder. The observations by infrared spectroscopy indicated that the chemical structures of the blend and the polypropylene matrix did not present significant changes with the reprocessing cycles. The X-ray diffraction analyses showed that the PP crystals were most affected when reprocessed in their pure form. The observations by thermogravimetry and differential scanning calorimetry indicated that the thermal stability of the blend was higher than that of polypropylene during the extrusion cycles. The scanning electron microscopy images indicated a weak interfacial interaction between the components of the blend, and the mechanical properties showed that the reprocessing improved the elasticity modulus and yield stress, with a consequential decrease of the impact strength.

Preparação de argilas organofílicas e desenvolvimento de nanocompósitos de polietileno. Parte 2: comportamento de inflamabilidade

High density polyethylene/Bentonite clay nanocomposites were prepared by the melt intercalation technique. The clay was organically modified with different quaternary ammonium salts to obtain the organoclay. The unmodified and modified clays with the quaternary ammonium salts were introduced in a polyethylene matrix with 1 and 3 wt. % of clay. The thermal stability and the flammability of the systems were investigated by thermogravimetry and UL-94HB standard, respectively. The dispersion analysis and the interlayer distance (d001) of the clay particles were obtained by X ray Diffraction (XRD) and transmission electron microscopy (TEM). The organoclay presence in the polymer matrix increased the degradation temperature in relation to the pure polymer. The systems showed a reduction on the burning rate, indicating that the flammability resistance of the nanocomposites was improved.

Influence of processing variables on the mechanical behavior of HDPE/clay nanocomposites

Nanocomposites were processed using the technique of melt intercalation, starting from a concentrated polar compatibilizer/organoclay (PE-g-MA/organoclay) prepared in an internal mixer. The concentrate was incorporated into the matrix of HDPE by two methods: I) counter-rotating twin-screw extruder and II) co-rotating twin-screw extruder, using two screw profiles (ROS and 2KB90). After extrusion, the specimens of the extruded composites were injection molded. The X-ray diffraction (XRD) technique was used to analyze the degree of expansion of the prepared clays. To analyze the degree of exfoliation of obtained nanocomposites, XRD and TEM (transmission electron microscopy) were used. The influence of processing variables on mechanical properties was studied through the behavior of the modulus and tensile strength of nanocomposite systems. By XRD and TEM, it was seen that the clay was well dispersed in the matrix and the presence of intercalated and partially exfoliated hybrid structure for nanocomposites was observed when the systems were prepared in counter-rotating twin-screw extruder. A similar behavior was observed in the use of screws (2KB90 or ROS) of the nanocomposites, with a reduction in modulus and tensile strength. Although the mixing process by extruding be the most common industrial practice, and also it is the preferred strategy for the preparation of polymer nanocomposites, much of the literature was directed to the study of chemical modification of clay, type and level of compatibilizer, in order to maximize the compatibility between clay and the polymeric matrix. On the other hand, studies about the role of the processing and configurations of screws are relatively scarce. The main motivation of this work was to expand and to contribute to spread a better understanding of the effects of processing to obtain polymer nanocomposites.

Obtenção de membranas microporosas a partir de manocompósitos de poliamida 6/argila nacional. Parte 1: influência da presença da argila na morfologia das membranas

Polymeric membranes were produced from nylon 6 nanocomposites and a clay using the immersion-precipitation technique. The clay was organically modified by using a quaternary ammonium salt, Dodigen. Nanocomposites were obtained from nylon 6 with untreated clay (MMT) and treated clay (OMMT). The nanocomposites were studied by XRD and TEM. The morphological structure consisted of an exfoliated and partially exfoliated clay layers in the polymeric matrix. The membranes were produced by phase inversion method and characterized by XRD and SEM. The X-ray diffraction of the membranes confirmed the results for the nanocomposites. The SEM image of the membrane top surface showed irregular pores. As for the membranes with the nanocomposites, a larger number of better distributed pores were observed, indicating that the presence of the clay altered the membrane morphology. The cross section SEM image showed an asymmetric morphology structure, comprising two layers, namely a skin with small and closed pores, and a porous layer with large, uniformly distributed pores.