This study focuses on the methodology to obtain nanocellulose from vegetal fibers. An experimental planning was carried out for the treatment of curaua fibers and parameters were estimated, having the concentration of H 2 SO 4 , hydrolysis time, reaction temperature and time of applied sonication as independent variables for further statistical analysis. According to the estimated parameters, the statistically significant effects were determined for the process of obtaining nanocellulose. With the results obtained from the thermogravimetric analysis (TGA) it was observed that certain conditions led to cellulose with degradation temperatures near or even above that of the untreated cellulose fibers. The crystallinity index (I C ) obtained after fiber treatment (by X-ray diffraction technique) was higher than that of the pure fiber. Treatments with high acid concentrations led to higher IC. After the statistical experimental design, mixtures of polypropylene with fibers prepared after different treatments were performed in a mini-extruder. It was possible to observe a sharp increase in the mechanical properties through the dynamic mechanical thermal analysis (DMTA).
Oxidized (GO) and expanded (G-Exp) graphite were employed to prepare composites with ultrahigh molecular weight polyethylene (UHMWPE) matrix using masterbatches of polyethylene with different compositions. The materials and a blend of UHMWPE/HDPE were prepared by extrusion and their properties were evaluated. The effect of carbon fillers on the crystalline structure, thermo dynamic-mechanical (DMTA) and thermal properties (melting and crystallization temperatures) of the composites were discussed. The thermogravimetric analysis (TGA), differential scanning calorimetry (DSC) and wide-angle X-ray diffraction (WAXD) measurements showed that the addition of masterbatch with GO and G-Exp significantly increased the crystallite size of composites, increasing the temperatures of melting, degradation, glass transition and the degree of crystallinity of polyethylene. DMTA analysis indicated the storage and loss moduli of composites in relation to neat UHMWPE, the blend and UHMWPE/composites. SEM micrographs showed a flatter, continuous and uniform surface meaning a compact lamellar structure. The present work resulted in interesting findings on the effects of GO on the crystalline structures, mechanical and thermal properties of UHMWPE, which can lead to generalizations useful for future work.
The use of cellulose fibers derived from renewable resources as reinforcement in polymeric composites provides positive environmental benefits with respect to disposal and raw material savings. Microcrystalline cellulose is a regenerated cellulose material that is free of lignin and hemicellulose, widely used in various applications. Recently, there has been enormous interest in producing polymer nanocomposites using cellulose nanofibers as reinforcement. Moreover, the steam explosion process is an ecofriendly method to modify cellulose fibers by inducing fibrillation, allowing the production of nanofibers. Fibrillation of microcrystalline cellulose using steam explosion process as the only cellulose treatment process was not yet studied in the literature. In the present work, steam explosion process was applied to commercial microcrystalline cellulose and the obtained fibers were characterized and employed in composites with polypropylene for evaluation of the thermal, mechanical, and morphological properties in relation to the matrix. The results showed that this process promoted partial fibrillation to nanosized diameter, and an increase in crystalline degree and thermal stability of the original fiber. As for the polypropylene/cellulose composites in the absence of compatibilizer, there was an increase of thermal degradation temperature and mechanical properties measured by dynamic-mechanical analysis in comparison with pure polypropylene.
Abstract. Three-component catalytic systems based on 2,6-bis(imino) pyridine iron(II) chloride were synthesized from different ligands, which provided new alternative catalysts for polymerization of ethylene. The synthesized catalysts were characterized by Fourier transform infrared spectroscopy (FTIR), and the lack of absorption bands was observed in the region related to the carbonyl, as well as the presence of bands in the region of imino groups corresponding to C=N bonds. Coordination with Fe was also carried out. The structure of the ligands and the new catalysts were confirmed by the elemental analysis (CHN), and 1 H-and 13 C-nuclear magnetic resonance spectroscopy. In ethylene polymerization with methylaluminoxane as a cocatalyst, the activity of catalyst C1 was high. Although this catalyst structure contains sterically bulky ligands, the metal center was not sufficiently protected allowing transfer reactions, producing polyethylene with a low molar mass and melting temperature.
This work deals with synthesis, characterization and evaluation of post-metallocene complexes based on silica-supported bis(imino)pyridine iron, containing amino groups in ethylene polymerizations. The reaction of these complexes and methylaluminoxane generated active species in heterogeneous ethylene polymerization. The absence of substituents at the orthoposition of the phenyl rings near the metal site was not compensated by the steric hindrance of the silica surface, negatively affecting the catalytic activity and the molar mass of the produced polymer. The catalyst C1, with the most bulkier ligand, presented the best performance, showing high catalytic activity not only in homogeneous system, but also in supported systems due to the chemical bond between the functionalized complex and the support surface, which led to polyethylene particles with good morphology, spherical tendency, filled pores and the decrease in bulk density compared to the particles produced through homogeneous catalyst.
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