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A simple and inexpensive method for the production of graphene-based masterbatch via polymer-assisted shear exfoliation of graphite in water was comprehensively investigated. In detail, a modified polyvinyl alcohol (mPVOH) characterized by surface energy comparable with that of graphene was used as surfactant for the production of graphene-like particles. The proposed approach allowed a yield in graphene-like particles higher than that obtained by using common surfactants, along with a narrower size distribution. A mPVOH-masterbatch containing 4.38 wt% of graphene-like particles was produced by removing the aqueous solvent from a dispersion and directly used for production of polymer nanocomposites by melt processing. Films prepared by blending the masterbatch with polyvinyl alcohol in order to have a graphene-like particles content equal to 0.3 wt% showed a 78% reduction in water permeability and a 48% increase in storage modulus as compared with pristine polymers. Improved barrier properties were also observed for polylactic acid (PLA) and low-density polyethylene (LDPE)-based composite films, whereas an increment of about 520% in the storage modulus was observed for the composite obtained with PLA. The obtained results are very relevant and the proposed process will open up a new pathway for using graphene-based masterbatch in the packaging industry. Keywords: Graphene production, Graphene masterbatch, Polymer composite, Barrier and mechanical properties, Packaging

Neste trabalho foi avaliada a influência de uma resina hidrocarbônica hidrogenada (RHH), de baixo peso molecular, na morfologia e propriedades finais de nanocompósitos de polipropileno. Os nanocompósitos foram obtidos utilizando-se duas argilas organofílicas, uma de caráter catiônico (MMT, C-l5A) e outra de caráter aniônico (HDL, Perkalite), e dois agentes compatibilizantes de polipropileno com diferentes teores de anidrido maleico. Os nanocompósitos foram preparados pelo método de intercalação no estado fundido em câmara de mistura e em extrusora dupla rosca. Um estudo preliminar, em câmara de mistura, foi realizado para verificar o efeito da ordem de mistura dos componentes principalmente sobre a morfologia dos nanocompósitos. Os resultados mostraram que uma melhor distribuição e dispersão das partículas de argila foram alcançadas na matriz polimérica quando argila e RHH foram primeiramente misturadas e, somente depois de decorridos 3 minutos de processamento o polipropileno foi incorporado. A partir destes resultados, optou-se em realizar uma pré-mistura constituída de argila, compatibilizante e RHH em um misturador intensivo, e esta foi incorporado ao PP na extrusora dupla-rosca. Os resultados mostraram que o uso de pré-misturas da argila Cloisite-15A, compatibilizante Polybond 3150 e RHH resultaram em uma morfologia com maior distribuição e dispersão das partículas de argila, melhores propriedades mecânicas com incremento de 57% no módulo elástico, aumento na estabilidade térmica e redução de 58% na permeabilidade ao oxigênio. Tais resultados mostraram que a RHH conseguiu auxiliar na esfoliação da argila pelo uso do misturador intensivo. Para os nanocompósitos com a argila Perkalite o uso do misturador intensivo não influenciou na morfologia. O módulo elástico dos nanocompósitos com essa argila apresentaram resultados superiores comparados com a argila C-15A quando a mistura de todos os componentes foi feita em uma única etapa na extrusora dupla rosca cujo ganho é atribuído à ação da RHH que conseguiu auxiliar na dispersão da argila Perkalite. In this study it was evaluated the effect of a low molecular weight hydrogenated hydrocarbon resin (RHH) in morphology and final properties of polypropylene nanocomposites. The nanocomposites were obtained using two organoclays, a cationic (MMT) and a anionic (HDL) and two compatibilizing agents of polypropylene grafted with different amounts of maleic anhydride. Nanocomposites were prepared by intercalation in molten state by using batch mixer and twin-screw extruder. A preliminary study in the batch mixer was conducted to determine the effect of mixing order of the components on the final morphology of nanocomposites. The results showed that a better distribution and dispersion of the clay particles have been achieved in the polymeric matrix when the clay and RHH were first mixed during 3 minutes, then incorporated into the polypropylene. From these results, further tests were conducted with a pre-mixture consisting of clay, compatibilizer and RHH in an intensive mixer was incorporated into the PP on a twin-screw extruder. The results showed that the use of premixes clay Cloisite 15A, compatibilizer Polybond 3150 and RHH exhibited a morphological enhancement in distribution and dispersion of clay particles, improving mechanical properties up to 57% on Young’s modulus, increased thermal stability and reduction of oxygen permeability in 58%. For Perkalite clay nanocomposites, the use of intensive mixer did not influence the morphology. The Young’s modulus of nanocomposites with this clay showed superior results compared with the clay 15A-C when the mixture of all components was performed in a single step in a twin screw extruder, shown that RHH could assist in dispersion of Perkalite.