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The development of hydroxyapatite (HAp) and polyether ether ketone (PEEK) biocomposites has been extensively studied for bone repair applications due to the synergistic properties of the involved materials. In this study, we aimed to develop HAp/PEEK biocomposites using high-energy ball milling, with HAp concentrations (20%, 40%, and 60% w/v) in PEEK, to evaluate their physicochemical, mechanical, cytotoxicity, and antimicrobial properties for potential applications in Tissue Engineering (TE). The biocomposites were characterized by structure, morphology, apparent porosity, diametral compression strength, cytotoxicity, and antimicrobial activity. The study results demonstrated that the HAp/PEEK biocomposites were successfully synthesized. The C2 biocomposite, containing 40% HAp, stood out due to the optimal distribution of HAp particles in the PEEK matrix, resulting in higher compression strength (246 MPa) and a homogeneous microstructure. It exhibited antimicrobial activity against Staphylococcus aureus, Pseudomonas aeruginosa, and Escherichia coli, with no cytotoxicity observed. These properties make the C2 biocomposite promising for regenerative medicine applications, combining mechanical strength, bioactivity, and biocompatibility.
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Styrene-butadiene rubber (SBR) waste from the shoe industry was repurposed to produce polypropylene (PP)-based compounds, with the aim of evaluating their antistatic potential. Styrene-ethylene-propylene (SEP) was added as a compatibilizing agent, while carbon nanotubes (MWCNT) were incorporated as a conductive nanofiller. The polymer compounds were processed in an internal mixer, and injection molded. The properties evaluated included torque rheometry, melt flow index (MFI), impact strength, tensile strength, Shore D hardness, electrical conductivity, heat deflection temperature (HDT), and differential scanning calorimetry (DSC), along with scanning electron microscopy (SEM) for morphology analysis. The production of the PP/SBR/SEP (60/30/10 wt%) compound resulted in a ductile material, enhancing impact strength and elongation at break to 161.2% and 165.2%, respectively, compared to pure PP. The addition of SEP improved the compatibility of the PP/SBR system, leading to an increase in the torque curve and a reduction in the MFI. Furthermore, the SBR/SEP combination in PP accelerated the crystallization process and increased the degree of crystallinity, suggesting a nucleating effect. Carbon nanotubes, in concentrations ranging from 0.5 to 2 phr (parts per hundred resin), were added to the PP/SBR/SEP system. Only the PP/SBR/SEP/MWCNT compound with 2 phr of MWCNT was suitable for antistatic applications, exhibiting an electrical conductivity of 4.52 × 10-07 S/cm. This was due to the greater distribution of MWCNT in the PP matrix, as demonstrated by SEM. In addition, remains tough at room temperature, with a 166% increase in impact strength compared to PP. However, there was a reduction in elastic modulus, tensile strength, Shore D hardness, and HDT due to increased flexibility. SBR waste can be reintegrated into the production chain to produce antistatic polymeric compounds, obtaining a tough material at room temperature.
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The study aimed to utilize MoO3 catalysts, produced on a pilot scale via combustion reaction, to produce biodiesel from residual oil. Optimization of the process was conducted using a 23 experimental design. Structural characterization of the catalysts was performed through X-ray diffraction, fluorescence, Raman spectroscopy, and particle size distribution analyses. At the same time, thermal properties were examined via thermogravimetry and differential thermal analysis. Catalytic performance was assessed following process optimization. α-MoO3 exhibited a monophasic structure with orthorhombic phase, whereas α/h-MoO3 showed a biphasic structure. α-MoO3 had a larger crystallite size and higher crystallinity, with thermal stability observed up to certain temperatures. X-ray fluorescence confirmed molybdenum oxide predominance in the catalysts, with traces of iron oxide. Particle size distribution analyses revealed polymodal distributions attributed to structural differences. Both catalysts demonstrated activity under all conditions tested, with ester conversions ranging from 93% to 99%. The single-phase catalyst had a long life cycle and was reusable for six biodiesel production cycles. The experimental design proved to be predictive and significant, with the type of catalyst being the most influential variable. Optimal conditions included α-MoO3 catalyst, oil/alcohol ratio of 1/15, and a reaction time of 60 min, resulting in high biodiesel conversion rates and showcasing the viability of MoO3 catalysts in residual oil biodiesel production.
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The development of polymeric biocomposites containing natural fibers has grown over the years due to the properties achieved and its eco-friendly nature. Thus, biocomposites involving a polymer from a renewable source (Biopolyethylene (BioPE)) and babassu fibers (BFs), compatibilized with polyethylene grafted with maleic anhydride (MA) and acrylic acid (AA) (PE-g-MA and PE-g-AA, respectively) were obtained using melt mixing and injection molded into tensile, impact, and HDT specimens. Babassu fiber was characterized with Fourier transform infrared spectroscopy (FTIR), thermogravimetry (TGA), and scanning electron microscopy (SEM). The biocomposites were characterized using torque rheometry, TGA, tensile strength, impact strength, thermomechanical properties, Shore D hardness, and SEM. The data indicate that the torque during the processing of compatibilized biocomposites was higher than that of BioPE/BF biocomposites, which was taken as an indication of a possible reaction between the functional groups. Compatibilization led to a substantial improvement in the elastic modulus, tensile strength, HDT, and VST and a decrease in Shore D hardness. These results were justified with SEM micrographs, which showed babassu fibers better adhered to the surface of the biopolyethylene matrix, as well as an encapsulation of these fibers. The system investigated is environmentally sustainable, and the results are promising for the technology of polymeric composites.
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In this work, polyhydroxybutyrate (PHB) was maleic anhydride (MA)-grafted in the molten state, using dicumyl peroxide (DCP) as a reaction initiator. Tin(II) 2-ethylhexanoate (Sn(Oct)2) and styrene monomer (St.) were used to maximize the maleic anhydride grafting degree. When PHB was modified with MA/DCP and MA/DCP/Sn(Oct)2, viscosity was reduced, suggesting chain scission in relation to pure PHB. However, when the styrene monomer was added, the viscosity increased due to multiple grafts of MA and styrene into the PHB chain. In addition, the FTIR showed the formation of a new band at 1780 cm-1 and 704 cm-1, suggesting a multiphase copolymer PHB-g-(St-co-MA). The PHB (MA/DCP) system showed a grafting degree of 0.23%; however, the value increased to 0.39% with incorporating Sn(Oct)2. The highest grafting efficiency was for the PHB (MA/DCP/St.) system with a value of 0.91%, while the PHB (MA/DCP/St./Sn(Oct)2) hybrid mixture was reduced to 0.73%. The chemical modification process of PHB with maleic anhydride increased the thermal stability by about 20 °C compared with pure PHB. The incorporation of 0.5 phr of the Sn(Oct)2 catalyst increased the efficiency of the grafting degree in the PHB. However, the St./Sn(Oct)2 hybrid mixture caused a deleterious effect on the maleic anhydride grafting degree.
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Anidridos Maleicos , Estireno , Polímeros , Fenômenos QuímicosRESUMO
In this work, blends based on poly (lactic acid) (PLA)/acrylonitrile-butadiene-styrene (ABS) compatibilized with maleic anhydride-grafted (SEBS-g-MA) were prepared in a co-rotational twin-screw extruder by varying the concentrations of the compatibilizing agent. The influence of the compatibilizing agent on the morphology, mechanical, thermal, thermomechanical, and rheological properties of the prepared materials was analyzed. The effect of annealing on the properties of the blends was also investigated using injection-molded samples. The X-ray diffraction (XRD) results proved that the increments in crystallinity were an effect of annealing in the PLA/ABS/SEBS-g-MA blends, resonating at higher heat deflection temperatures (HDTs). The impact strength of the PLA/ABS blends compatibilized with 10 wt% SEBS-g-MA was significantly increased when compared to the PLA/ABS blends. However, the hardness and elastic modulus of the blends decreased when compared to neat PLA. The refined morphology shown in the scanning electron microscopy (SEM) analyses corroborated the improved impact strength promoted by SEBS-g-MA. The torque rheometer degradation study also supported the increased compatibility between SEBS-g-MA, PLA, and ABS. The TGA results show that the PLA/ABS and PLA/ABS/SEBS-g-MA blends are more thermally stable than the neat PLA polymer at higher temperatures. The results showed that the ideal composition is the heat-treated PLA/ABS/SEBS-g-MA (60/30/10 wt%), given the high impact strength and HDT results. The results of this work in terms of mechanical improvement with the use of compatibilizers and annealing suggest that the PLA/ABS/SEBS-g-MA system can be used in the production of 3D-printing filaments.
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Nylon 6/acrylonitrile-butadiene-styrene nanocomposites were prepared by mixing in a molten state and injection molded for application in electromagnetic interference shielding and antistatic packaging. Multi-wall carbon nanotubes (MWCNT) and maleic anhydride-grafted ABS compatibilizer were incorporated to improve the electrical conductivity and mechanical performance. The nanocomposites were characterized by oscillatory rheology, Izod impact strength, tensile strength, thermogravimetry, current-voltage measurements, shielding against electromagnetic interference, and scanning electron microscopy. The rheological behavior evidenced a severe increase in complex viscosity and storage modulus, which suggests an electrical percolation phenomenon. Adding 1 to 5 phr MWCNT into the nanocomposites produced electrical conductivities between 1.22 × 10-6 S/cm and 6.61 × 10-5 S/cm. The results make them suitable for antistatic purposes. The nanocomposite with 5 phr MWCNT showed the highest electromagnetic shielding efficiency, with a peak of -10.5 dB at 9 GHz and a value around -8.2 dB between 11 and 12 GHz. This was possibly due to the higher electrical conductivity of the 5 phr MWCNT composition. In addition, the developed nanocomposites, regardless of MWCNT content, showed tenacious behavior at room temperature. The results reveal the possibility for tailoring the properties of insulating materials for application in electrical and electromagnetic shielding. Additionally, the good mechanical and thermal properties further widen the application range.
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Acrilonitrila , Nanocompostos , Nanotubos de Carbono , Butadienos , Caprolactama/análogos & derivados , Condutividade Elétrica , Polímeros , EstirenoRESUMO
In this work, polyamide 6 (PA6) properties were tailored and improved using a maleic anhydride-grafted acrylonitrile-butadiene-styrene terpolymer (ABS-MA). The PA6/ABS-MA blends were prepared using a co-rotational twin-screw extruder. Subsequently, the extruded pellets were injection-molded. Blends were characterized by torque rheometry, the Molau test, Fourier transform infrared spectroscopy (FTIR), impact strength, tensile strength, Heat Deflection Temperature (HDT), Differential Scanning Calorimetry (DSC), Thermogravimetry (TG), Contact Angle, Scanning Electron Microscopy (SEM), and water absorption experiments. The most significant balance of properties, within the analyzed content range (5, 7.5, and 10 wt.%), was obtained for the PA6/ABS-MA (10%) blend, indicating that even low concentrations of ABS-MA can improve the properties of PA6. Significant increases in impact strength and elongation at break have been achieved compared with PA6. The elastic modulus, tensile strength, HDT, and thermal stability properties of the PA6/ABS-MA blends remained at high levels, indicating that maleic anhydride interacted with amine end-groups of PA6. Torque rheometry, the Molau test, and SEM analysis suggested interactions in the PA6/ABS-MA system, confirming the high properties obtained. Additionally, there was a decrease in water absorption and the diffusion coefficient of the PA6/ABS-MA blends, corroborating the contact angle analysis.
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Poly(ethylene-octene) grafted with glycidyl methacrylate (POE-g-GMA) and ethylene elastomeric grafted with glycidyl methacrylate (EE-g-GMA) were used as impact modifiers, aiming for tailoring poly(lactic acid) (PLA) properties. POE-g-GMA and EE-g-GMA was used in a proportion of 5; 7.5 and 10%, considering a good balance of properties for PLA. The PLA/POE-g-GMA and PLA/EE-g-GMA blends were processed in a twin-screw extruder and injection molded. The FTIR spectra indicated interactions between the PLA and the modifiers. The 10% addition of EE-g-GMA and POE-g-GMA promoted significant increases in impact strength, with gains of 108% and 140%, respectively. These acted as heterogeneous nucleating agents in the PLA matrix, generating a higher crystallinity degree for the blends. This impacted to keep the thermal deflection temperature (HDT) and Shore D hardness at the same level as PLA. By thermogravimetry (TG), the blends showed increased thermal stability, suggesting a stabilizing effect of the modifiers POE-g-GMA and EE-g-GMA on the PLA matrix. Scanning electron microscopy (SEM) showed dispersed POE-g-GMA and EE-g-GMA particles, as well as the presence of ligand reinforcing the systems interaction. The PLA properties can be tailored and improved by adding small concentrations of POE-g-GMA and EE-g-GMA. In light of this, new environmentally friendly and semi-biodegradable materials can be manufactured for application in the packaging industry.
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The aim of the present work is to evaluate the effect of NaOH solution as a stress cracking agent on the thermal and tensile properties of PET and PET/ZnO composites. The solutions were applied during tensile testing and the effects were monitored by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and testing the actual mechanical properties. The rate of crystallization was increased when the samples were exposed to NaOH, as observed by both cold and melt crystallization; this is possibly due to the reduction in molar mass of the PET molecules caused by NaOH. During melting, the DSC peaks became more complex, which is probably due to the distinct macromolecular mass, as well as crystallites with different sizes and levels of perfection. According to TGA analyses, no drastic changes were observed on the thermal stability of PET due to the action of NaOH. The tensile properties were shown to decrease drastically upon exposure to NaOH, which is the main symptom of stress cracking, leading to increased fragility, as also observed in the scanning electron microscopy (SEM) images. The presence of ZnO improved PET crystallization and provided some protection against the harmful effects of NaOH.