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In this research, palm oil and soy oil were used as a natural polyol to prepare novel poly(silyl ether)s. Palm oil and soy oil were first converted to monoglyceride by one step via alcoholysis process in the presence of 0.1% CaO as a catalyst. The monoglycerides were characterized by Fourier transform infrared spectrometer (FT-IR), nuclear magnetic resonance (NMR) and iodine test. The novel poly(silyl ether)s were prepared via polycondensation reaction between dimethyldichlorosilane with monoglycerides based on palm and soy oils, respectively. FT-IR, NMR and silicone-29 (29Si NMR) were used to confirm and determine the presence of silicone in the synthesized polymers. Thermal behavior was studied by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). Antibacterial activity of the polymers was screened against three different strains of bacteria, namely Escherichia coli E266, Staphylococcus aureus S276 and Salmonella choleeraesuis 10708.

In the present work, the depolymerization of polyethylene terephthalate (PET) was performed by the method of glycolysis with ethylene glycol. The process was carried out using a factorial design in the Box-Behnken optimization model, using a response surface methodology (RSM) in which three factors (time, temperature and mass ratio of ethylene glycol) were studied in three levels of variation (- 1, 0, +1) with two replicates of the center point, totalizing 15 experiments for which the yield of bis (2-hydroxyethyl) terephthalate (BHET) monomers formed in the process was chosen as response. In parallel, the Arrhenius kinetic test was used to determine the apparent activation energy (Ea) for the 1-butyl-3-methylimidazole trichlorozincate ([Bmin]ZnCl3) - catalyst used in the depolymerization process. The products of glycolysis obtained were characterized by spectroscopic techniques (FTIR), (1 H and 13C NMR), thermal analyses (TGA) and (DSC) and Mass Spectrometry LC-MS/MS hybrid Quadrupole-Orbitrap.

Advanced fabric reinforced polymer composites find extensive applications in aerospace and structural fields due to their high mechanical properties. A novel stamp forming technique finds extensive use in the hemispherical forming of thermoplastic composites. This study investigates the influence of stamp forming parameters on the formability of thermoplastic composite using Taguchi’s robust design and grey relational analysis. Taguchi’s orthogonal array was used for designing the forming experiments. Responses such as forming ratio and logarithmic thickness strain were considered for the assessment of sheet formability through single and multi-response optimization. Analysis of variance was used for the determination of the contribution of each parameter on formability and it was identified that the die temperature acts as a prominent factor, followed by blank holder force and blank temperature. The confirmation test was conducted at optimum parameter levels and the obtained experimental grade was seen within the confidence interval of the predicted value.

Core-shell magnetic polymer particles were synthesized by seeded suspension polymerization. The core was made of poly(methyl methacrylate-co-divinylbenzene) and a mixture of magnetite, maghemite and goethite (P(MMA-co-DVB)-M). The shell was composed of poly(glycidyl methacrylate-co-divinylbenzene) (P(GMA-co-DVB)). These particles were characterized by infrared spectrometry (FTIR), thermal analysis (TG), scanning electron microscopy (SEM), dynamic light scattering (DLS) and vibrating sample magnetometry (VSM). The results showed the formation of core-shells with good magnetic properties (≈7.1 emu/g) and good thermal resistance (≈300 ºC). The light scattering experiments showed that the particle size of these materials changed from 5-90 microns (core) to 5-120 microns (core-shell). Scanning electron microscopic images were useful to show the formation of P(GMA-co-DVB) shells on P(MMA- co-DVB)-M cores. The materials synthesized in this work have potential to be modified and employed in magnetic separation processes in the biotech and environmental fields.

This study investigated the effects of low concentrations of sericin (≤ 1.5 wt%) in starch- poly(butylene-adipate-co-terephthalate) (PBAT) films. The films were produced by blown extrusion and mechanical, barrier and structural properties were determined. Films containing 1.0 and 1.5 wt% sericin showed higher tensile strength (6.41 and 6.59 MPa) and Young's modulus (90.88 and 132.71 MPa) compared with film without sericin (4.76 MPa and 18.64 MPa). When 0.5 wt% of sericin was used, the elongation was reduced by 62%. The addition of sericin in a concentration of 1.5% (w/w) decreased the water vapor permeability of films from 7.55 to 5.94 g (m s Pa)-1, likely due to the formation of a more homogeneous and compact matrix. Based on these results, a mechanism of action is proposed, whereby sericin acts at the interface of the polymers (starch and PBAT), reducing the interfacial tension and enhancing compatibility.

Electrospun nanofibers from gelatin (G), chitosan (CS), and chitosan-polyvinyl alcohol (CS-PVA) were developed by electrospinning process. Mechanical properties were determined by the tensile test, the elastic modulus values of the nanofibers were G (15.418-34.34 MPa) and CS-PVA (17.44-126.427 MPa). The morphological characterization by SEM revealed that the systems with 15% G and 6% CS-PVA showed morphological homogeneity. Structural characterization by FTIR indicated an interaction among some functional groups of the component. Thermal analysis by DSC and TGA showed degradation temperatures for G (330 °C), CS (210 °C to 370 °C), and PVA (310 °C to 420 °C). The contact angles values denoted the hydrophilic nature of the material. Finally, the antimicrobial assay proved that both 15% G and 7% PVA on the CS-PVA system presented the best antimicrobial effect. The results indicate that the electrospun nanofibers fabricated with G or CS-PVA can be used as wound healing dressings.

The purpose of this study was to characterize, isolate and chemically modify tiger nut ( Cyperus sculentus L.) starch with octenyl succinic anhydride. The efficiency of the chemical modification was 0.04. Chemical composition, particle morphology (SEM), particle size, X-ray diffraction, infrared analysis, thermogravimetric analysis, differential scanning calorimetry and swelling and solubility power were determined for characterization of the native and modified starch. Both showed similar chemical composition and amylose and amylopectin contents, as well as absorption spectra in the infrared region without modification of the molecular structure and A-type crystalline pattern. The particles of both had an oval and spherical shape. The modified starch was more resistant to temperature and the gelatinization process occurred at 67.52 °C. These results suggest that tiger nut starch has a great industrial potential.

Sulfonated poly(indene) (SPInd), with 35% and 45% degree of sulfonation, was blended with Nafion to prepare blended membranes with 10, 15 and 20 wt.% of SPInd. Membranes were evaluated by infrared spectroscopy, thermogravimetric analysis, differential scanning calorimetry, scanning electron microscopy and X-ray diffraction. Water uptake (WU), ion exchange capacity (IEC) and through-plane proton conductivity were measured. The membranes presented similar thermal stability to Nafion. WU was slightly higher for Nafion/SPInd membranes (19-21% at RT and 40-44% at 90 °C) compared with recast Nafion (16% and 34%, respectively), and IEC values showed a similar trend. Blended Nafion membranes had increased proton conductivity of 2.41 x 10-2 and 2.37 x 10-2 Scm-1 (20 wt. % of SPInd 35% and 45%, respectively), compared with 1.16 x 10-2 Scm-1 for recast Nafion. The results show that the addition of SPInd to Nafion is a potential route towards improving the performance of Nafion in proton conductivity for use in fuel cells devices.

Made available in DSpace on 2018-11-29T23:48:17Z (GMT). No. of bitstreams: 0 Previous issue date: 2018-07-01. Added 1 bitstream(s) on 2019-10-09T18:28:11Z : No. of bitstreams: 1 S0104-14282018000300220.pdf: 1620072 bytes, checksum: bd4cff020a71e368122646a260a87503 (MD5) Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP) Prope Atom-Transfer Radical Copolymerization (ATRP) of methyl methacrylate (MMA) and ethyl methacrylate (EMA) under different reaction conditions was conducted using Grubbs 1st (1) and 2nd (2) generation catalysts. Initially, the study focused on the reactivity of the catalysts in ATRP of EMA individually, then the syntheses of poly(MMA-co-EMA) were also conducted in different mixtures of monomers ([MMA]/[EMA] = 100/200 and [MMA]/[EMA] = 200/100). Conversion and semilogarithmic kinetic plots as a function of time were related to the different catalysts and reaction conditions. The values of M-n and PDI also changed when different catalysts were used in the presence of Al(OiPr)(3), and more controlled polymerizations were achieved using 1. In the syntheses of poly(MMA)-co-(EMA), conversion of 60% was reached for both catalysts at different [MMA]/[EMA] ratios for 16 h; however, for shorter time, 4 h, better conversion values were obtained using 1 as catalyst for both [MMA]/[EMA] = 100/200 or 200/100. Univ Estadual Paulista, UNESP, FCT, Presidente Prudente, SP, Brazil Univ Estadual Piaui UESPI, Dept Quim, Nucleo Interinst Estudo & Geracao Novas Tecnol GE, Teresina, PI, Brazil Univ Estadual Paulista, UNESP, FCT, Presidente Prudente, SP, Brazil FAPESP: 2013/10002-0 Prope: 2180/002/14-PROPe/CDC

The effects of disinfection by microwave irradiation and immersion in peracetic acid on the physical-mechanical properties of a microwave-activated acrylic resin were evaluated. Specimens of acrylic resin were divided into a control group (specimens not disinfected) and 2 test groups subjected to one disinfection method: microwave irradiation at 850 W for 1 minute or immersion in 50 mL of 0.2% peracetic acid for 5 minutes. Specimens were submitted to Knoop hardness, flexural strength, flexural modulus, Izod impact, water sorption and solubility, glass transition temperature, and degree of conversion tests. Microwave disinfection significantly increased the mean Knoop hardness, Izod impact strength, water sorption, water solubility and glass transition temperature, whereas the flexural properties remained unaffected. Microwave disinfection increased the degree of conversion. Peracetic acid disinfection showed no changes in any properties. Both disinfection techniques did not adversely affect the evaluated properties.

The use of silica based bagasse fiber ash (BFA) as a reinforcing filler in polylactic acid (PLA) biocomposites was examined. The effects of surface-treated BFA on the rheological, swelling behavior, and mechanical properties and water absorption of biocomposites were studied. BFA was treated using a silane coupling agent (Bis-[3-(triethoxysilyl)-propy]-tetrasulfide). Composites with BFA were varied from 5 to 25wt.%. The PLA/BFA composite melts were pseudoplastic non -Newtonion fluid and exhibited a shear thinning behavior. The viscosity of the surface-treated BFA biocomposites was higher than that of the untreated. The viscosity of the composites decreased with increasing BFA content and shear rate. The extrudate swell of the composites increased with increasing shear rate, whereas it decreased with increasing BFA content and die temperature. The extrudate swell tended to be suppressed when surface-treated BFA was used. Silane treated BFA composites showed improvement in their mechanical properties, and exhibited significantly reduced water absorption.

Chitosan (CT) is a polysaccharide with the ability to adsorb metals on its surface. In this work, CT-based nanoparticles (NPs) are produced by complex formation with gum arabic (GA) to increase their adsorbent potential for removal of heavy metals in aqueous medium. Adsorption efficiency is evaluated as a function of NP composition and polysaccharide concentration. NPs are sized from 250 to 375 nm at a zeta potential up to -25 mV, suggesting stability to adsorb metals. In particular, CTGA56 and CTGA80 NPs adsorbed a substantially higher amount of copper ions than pure CT. Adsorption kinetics studies showed that the reaction process followed a pseudo second-order model and the adsorption isotherm results fit a Langmuir model, highlighting the monolayer adsorption process with prominent adsorption capacity. These findings indicate the adsorbent potential of CTGA NPs and suggest that these particles can be used for removal of metal ions from contaminated water sources.

It is a well-established fact that rubber accelerator is essential to provide solution in different sectors. However, there is a reversal process which can reduce the material performance. Sulfur accelerators donors and organic peroxides have been presented as a solution to the problem. The methodology development that can separate or characterize those components is a challenge and still allows gaps, explained by the application of conventional technique to reach this goal. This study aimed at contributing to the use of off-line coupling of thin layer chromatography (TLC)/infrared spectroscopy (IR) by Universal Attenuated Total Reflection (UATR) for analysis of N-cyclohexyl-2-benzotiazolsulfenamide (CBS), tetraethylthiuram disulfide (TMTD) and dicumyl peroxide (DCP), in natural poly-cis-isoprene (NR) formulations, containing naphthenic oil. The best results were obtained for the plasticizer and DCP, in formulations that had a greater proportion of these compounds. The separation of CBS and TMTD was made with less effectiveness, due to bands overlapping.

This work aims to evaluate the performance of anticorrosive thermoplastic coatings in cold rolled steel sheets. Two types of thermoplastic coatings were studied: polystyrene (PS) and cornstarch. These types of coatings are applied for protection against corrosion during transport and storage of steel plates after cold rolling until delivery to stamping or other processing. The good performance for these coatings is suitably standardized to ABNT NBR 5915-2: 2013 and ASTM A1008 / A1008M-2016. According to corrosion tests carried out in saline chamber, the coatings were satisfactory in different degrees of guarantee of corrosion protection on ASTM 1080 steel, in accordance with standards mentioned.

The aim of this work was to study the relationship of chain size of partially hydrolyzed PVA blended with starch in properties of biodegradable sheets produced by thermoplastic extrusion. It was also studied the effect of extrusion temperature profile to determine the better PVA chain size and temperature profile to produce biodegradable sheets through a factorial design. The processability and the mechanical, thermal, optical, and microstructural properties of the biodegradable sheets were adequate, indicating that PVA/cassava starch blends have potential to replace conventional non-biodegradable polymers. Tensile strength and Young’s modulus ranges from 1.0 to 2.6 and 3.0 to 6.9 MPa respectively, the elongation at break ranges from 42 to 421%. It was not possible to state a conclusive relationship between PVA molecular weight and the materials properties, but in general, PVA with medium molecular weight and high extrusion temperature profile promote an increase of mechanical properties of the sheets.

Made available in DSpace on 2018-11-26T16:04:38Z (GMT). No. of bitstreams: 0 Previous issue date: 2018-07-01. Added 1 bitstream(s) on 2019-10-09T18:25:30Z : No. of bitstreams: 1 S0104-14282018000300246.pdf: 2790991 bytes, checksum: 22303ed164be852f3c0654500f3e3219 (MD5) Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP) This work evaluated polyurethane (Polyquil (R)) as a graft for treatment of bone defects. Bone defects of 1.5 x 0.5 cm were made in the calvaria of 16 rabbits. Eight animals had their defects treated with Polyurethane (Treated) and 8 of them had their defects filled with blood clot (Control). In the second experiment, segmental defects of 0.5 cm were performed at the zygomatic arch of 16 rabbits. Eight animals were treated by guided bone regeneration, using a latex membrane, associated to grafting of polyurethane while the others were not treated (Control). The bone tissue morphometry in the craniotomy experiment resulted in a higher bone volume in the Treated group at 60 days (p < 0.05, t student test). Microscopic and radiographic images demonstrate the formation of a bone bridge in the segmental defect, 60 and 120 days after surgery in the Treated group, different from the Control group with incomplete healing. Univ Sagrado Coracao, PRPPG, Bauru, SP, Brazil Univ Sao Paulo, Fac Odontol Bauru, Bauru, SP, Brazil Univ Estadual Paulista UNESP, Fac Ciencias, Bauru, SP, Brazil Univ Estadual Paulista UNESP, Fac Ciencias, Bauru, SP, Brazil

There are few studies about Moringa oleifera derivates in polymer developments where vegetable oil was used as a plasticizer and a biodegrading agent. The polymerization of moringa oil (MO) was carried out assisted by microwaves without catalysts presence. There aren’t studies about the polymerization of MO using microwaves technology. Moringa’s oil and its polymer (PMO) were used as a biodegrading agent for mixtures of low density polyethylene (LDPE) with poly(butylene adipate-co-terephthalate)/poly(lactic acid) (PBAT/PLA). The mixtures producted films that were characterized and submitted to biodegradation analysis in order to discuss the influence of moringa components. Results showed that both moringa components improved thermal properties and reduced the crystalline phase of the mixture. The addition of PMO had improved the biodegradation capacity up to five times while MO had improved it up to three times. The results showed the greatest influence of moringa components on biodegradation of mixtures with cited polymers.

Fungal chitosan is a polymer that has been discussed and studied since 1859 in the world with great advances occurring over the years. Due to its global importance, this review aims to expose the history of the production and application of fungal chitosan in Brazil. Data collection was done at the Scielo, Sciencedirect and Pubmed databases, considering the period of the last 50 years. The inclusion criteria were articles on pure or associated chitosan and, in particular, fungal chitosan produced or applied by Brazilian research groups. At the end of the review, it was noticed a fungal chitosan very studied in different continents, and in Brazil is still used in specific and small groups. With the present work, it is expected that the diffusion of the studies will be accelerated and that potential research groups for fungal chitosan may grow through interaction with the existing ones.

A polymeric adsorbent based on sodium alginate (SAG) grafted with polyacrylamide (PAM) (SAG- g-PAM) was synthesized using an ultrasound-assisted method. The addition polymerization was carried out with ammonium persulfate as the initiator, at different acrylamide (AM) concentrations. The SAG-g-PAM copolymers were evaluated by FTIR and 13C NMR spectroscopies, thermogravimetric analysis, grafting efficiency (%GE) and intrinsic viscosity in NaCl solution at 25 °C. Graft copolymers could be obtained in reaction lasting until 10 min by using ultrasound energy with grafting efficiency above 75%. The decolorization efficiency and adsorption capacity of the SAG- g-PAM copolymers were investigated in the adsorption of methylene blue (MB). The dye adsorption was pH dependent, and adsorption capacity (69.13 mg/g) maxima was at pH 10. All the graft copolymers have shown the same decolorization efficiency (99%), and the best one for MB removing is the SAG-g-PAM6 (%GE = 75%), since lower acrylamide content is required in the synthesis.

Fuel Cells based in polymers are an alternative for the conventional energetic matrices. However, materials currently available still present disadvantages to overcome. Membranes of polycarbonate (PC)/sulfonated polycarbonate (PCs) blend/sepiolite nanocomposites have previously been studied by the authors, resulting in good mechanical properties and promising properties of vapor transmission and ionic migration resistance. However, their production in large scale is still a challenge. The aim of this work was the development further the formulation and processing of the previously studied material. Films of PC/PCs blends (50/50 wt%) with different content of sepiolite clay, with and without chemical modification, have been prepared in an extruder and evaluated by FTIR, XRD, DSC, TGA, DMA, tension strength and water vapor transmission (WVT). Even after two processing steps, the blend-based nanocomposites keep good thermal and mechanical properties. However, changes in WVT were observed with respect to data obtained in previous studies.

The compatibilization of recycled PP/PET blend with high and low concentration (20 and 5 phr) of elastomer functionalized by maleic anhydride (SEBS-g-MA) was achieved. Recycled polypropylene from plastic industry and recycled PET from post-consumer bottles was used. PP/PET blends: 80:20 w/w, 50:50 w/w and 20:80 w/w were prepared in an internal mixer for mechanical properties, thermal properties, morphology and rheological properties. SEBS-g-MA promoted compatibilization of the PP/PET blends and improved their properties. With an increasing compatibilization level, the refinement of morphology was observed in the PET rich blend. Compatibilized blends showed negative deviation in the PET glass transition temperature related to neat PET, demonstrating that compatibilization was very successful. PET crystallization was accelerated in the blends due to PP presence that enhanced nucleation. It was found that the 50/50/20 blend showed huge potential for textile fiber application and that of 80/20/20 showed more intermediary properties than neat polymers.

This paper presents the outcomes of an exploratory research carried out in companies, which are located in Brazil. They are FSSC-22000-certified food plastic packaging manufacturers. In order to identify the key aspects of the implementation process and certification, a questionnaire was developed and sent to twenty certified organizations. Out of them, eleven of which participating companies responded in a collaborative way. Based on the data obtained, improving competitiveness and customer retention were the reasons, which led the companies to seek the certification. However, the greatest difficulties were related to personnel, which presented technical and behavioral issues. In addition, it was noted that an overall satisfaction, derived from after-certification benefits, has been arisen in the companies. For instance, enhanced employee awareness, improved company's image and winning new customers, significantly contributing to their competitiveness, are some of the benefits found in this process.

Biodiesel has been considered a suitable substitute for petroleum diesel, but their chemical composition differs greatly. For this reason, biodiesel interacts differently than petroleum diesel with various materials, including rubbers. Therefore, the resistance of some elastomers should be thoroughly evaluated, specifically those which are commonly used in automotive industry. Nitrile rubber (NBR) is widely used to produce vehicular parts that are constantly in contact with fuels. This paper aimed to assess the resistance of carboxylated nitrile rubber (XNBR) with 28% of acrylonitrile content to soybean biodiesel in comparison with non-carboxylated nitrile rubber samples, with high and medium acrylonitrile content (33 and 45%). NBR with medium acrylonitrile content showed little resistance to biodiesel. However, carboxylated nitrile rubber even with low acrylonitrile content had similar performance to NBR with high acrylonitrile content.

When using Fourier transform infrared spectroscopy (FT-IR) under the qualitative aspect for characterization of polymer blends, often a simple identification of each one of the existing polymers in the blend does not justify the material failure since different amounts of each component may result in different mechanical properties, which should be a possible cause for of material failure when applied to an automotive part. Thus, seeking for a better justification in the understanding of material failure analysis, a new quantitative FT-IR methodology was developed in the mid-infrared region (MIR), using the transmission techniques and universal attenuated reflectance for the determination of Acrylonitrile Butadiene Styrene (ABS) and polycarbonate (PC). Transmission mode was more suitable. The relative band (A831 /A2237) was chosen for the preparation of the calibration curve that showed a 0.99% error methodology, which is within the FT-IR spectrometer accuracy limit (≤ 2%); therefore, it is accurate for the analysis of the system.

Composites Films were produced using Poly (Vinyl Alcohol) as the soft material and reinforced with Chitin Nanowhiskers(NWCH) as the rigid material. The present work studies the reinforcing mechanisms of NWCH in PVA films, made through a solvent casting technique and characterized for their calorimetric, swelling and mechanical properties. DSC tests revealed a sharp increase of 45 °C in glass transition temperatures with only 1.5% NWCH, while melting temperature had a small increases suggesting an anti-plasticizing effect. Swelling tests revealed decreasing hygoscopy when NWCH volume fraction increases. Estimates for elastic tensile modulus using a model that predicts the formation of a percolating network were not consistent with the experimental data of tensile tests suggesting that contrary to the reinforcement with cellulose nanowhiskers the percolating network is not primarily responsible for the reinforcement of the films. By adjusting the Halpin-Tsai equations, modified by Nielsen it was found that the mechanical properties were mainly influenced by the packing of the NWCH.

In this study, the chemical interaction between functionalized carbon nanotuboes with carboxyl groups (CNT-f) and the subsequent addition of furfuryl alcohol (FA) and mixture with poly(furfuryl alcohol) (PFA) resin was evaluated. The FA with CNT-f was mixed in PFA resin to facilitate the chemical interaction of CNTs. The morphological and chemical interaction were studied by Transmission Electron Microcopies (MET), FTIR analyses, Raman Spectroscopy, viscosimetry and X-ray photoelectron spectroscopy (XPS). It was observed that a chemical interaction occurs through the opening of the hydroxyl polymer chain with a subsequent output of one water molecule. This interaction was evident from the FTIR and XPS data of the PFA composites. In this way, the mixture of functionalized carbon nanotubes with carboxyl groups in the FA, before adding this reinforcement into the PFA resin, can be considered a good procedure in order to obtain an appropriate chemical interaction between the CNT and PFA resin.

The Dynamic mechanical behavior of chemically treated and untreated hemp fiber reinforced composites was investigated. The morphology of the composites was studied to understand the interaction between the filler and polymer. A series of dynamic mechanical tests were performed by varying the fiber loading and test frequencies over a range of testing temperatures. It was found that the storage modulus (E’) recorded above the glass transition temperature (Tg) decrease with increasing temperature. The loss modulus (E”) and damping peaks (Tan δ) values were found to be reduced with increasing matrix loading and temperature. Morphological changes and crystallinity of Composites were investigated using scanning electron microscope (SEM) and XRD techniques. The composites with Alkali and Benzoyl treated fibers has attributed enhanced DMA Results. In case of XRD studies, the composites with treated fibers with higher filler content show enhanced crystallinity.

Different polymeric matrices have been investigated for use in the development of biodegradable films. The incorporation of cellulose nanocrystals in such films has particularly attracted attention because of the potential for achieving improved properties of starch nanocomposites. In the present study, cellulose nanocrystals were extracted from coconut fibers and incorporated in cassava and potato starch films at different concentrations. The properties of the different nanobiocomposite films were comparatively evaluated, including their barrier and mechanical properties. All the films, regardless of the nanocrystal concentration, were found to exhibit low solubility in water, with increased moisture content particularly observed in the films with higher nanocrystal concentrations. The potato starch film with the lowest nanocrystal concentration was found to exhibit the best mechanical properties. The observations of this study indicated that the source of the starch and the nanocrystal concentration determined the properties of the nanobiocomposite films.

The vinyl ester resins and natural composites have emerged as a suitable alternative in tribological application due to mechanical behavior, which relates to the conversion of the double bonds. During tribological test the permanent contact between polymeric sample and counterpart can increase the temperature affecting the crosslinking of the samples. These variations have direct implications in the curing rate and the global conversion. In this work, the FTIR evaluation is used to evaluate possible changes on the global conversion of vinyl ester and their composites reinforced with Musaceae fiber bundles and cured using two hardeners, after a specific tribological test. Increments around 15% on global conversion of styrene double bonds were observed for neat matrix and composites using both hardeners, suggesting that during tribology test some alterations on resin structure takes place. These results open alternatives to manipulate the curing conditions in order to control the tribological behavior.

Packages are essential for the food processing industry. Among the innovative alternatives there is antimicrobial packaging, which aims to reduce or inhibit microbial growing on the food surface. One potential to produce this type of package is poly(3-hydroxybutyrate)-PHB additivated with canola oil. In this work, films of PHB additivated with canola oil were produced in different compositions. Mid-infrared records, tensile mechanical testing and thermal analyses were performed on the films. The results of the mechanical tests indicated that the addition of canola oil to the polymeric matrix of PHB increases the material flexibility. The thermal analyses results showed that the addition of canola oil changes the thermal properties of PHB, such as the melting and crystallization temperatures, maximum crystallization rate and relative crystallinity. The knowledge of these properties is fundamental for the manufacturing process of polymeric materials, due to the specifications required for these materials in the intended applications.

Core-shell particles were produced on seeded suspension polymerization by using polystyrene (PS) as polymer core, or seed, and methyl methacrylate (MMA) as the shell forming monomer. Two synthesis routes were evaluated by varying the PS seed conversion before MMA addition. The main purpose of this work was to investigate the influence of synthesis routes on the morphology and chemical resistance of the resulting particles. 1H NMR spectroscopy showed that the use of PS seeds with lower conversion led to the formation of higher amount of poly(styrene-co-MMA). The copolymer acted as a compatibilizer, decreasing the interfacial energy between both homopolymers. As a consequence, a larger amount of reduced PMMA cluster were formed, as was revealed by TEM measurements. Samples in this system showed enhanced resistance to cyclohexane attack compared with pure PS, with a PS extraction of only 37% after 54 hours test.

Graphical Abstract Abstract Polymers are a class of soft materials with numerous and versatile mechanical and chemical properties that can be tuned specific to their application. Agriculture is an expanding area due to the requirement for indispensable food to meet the demands of a growing global population. Consequently, development of technology to improve the quality of the soil and agriculture manages is still under development. Intelligent agricultural supplies (controlled or slow release agrochemicals and superabsorbents) and biosorbents contribute to an expanding niche using technology from polymers. This review elucidates the state-of-the-art and will discuss some important aspects of using polymers in intelligent fertilizers, as well as superabsorbent, biosorbent and biodegradation processes in agriculture that are environmentally, technically, socially, and economically sustainable.

Made available in DSpace on 2018-12-11T17:34:54Z (GMT). No. of bitstreams: 0 Previous issue date: 2017-09-01. Added 1 bitstream(s) on 2021-07-15T15:04:23Z : No. of bitstreams: 1 S0104-14282017000300183.pdf: 1650034 bytes, checksum: 2cb2c66cd4146051c0f244e73c39a02d (MD5) Polyvinylidene fluoride (PVDF) is valued for its properties of transparency to light, lightness, flexibility, mechanical strength, chemical stability, ease of processing, and low-cost production. Ceramics have low mechanical strength and poor processability, but have excellent piezo- and pyroelectric characteristics. The deficiencies of ceramics can be minimized by combining them with polymers. Accordingly, PVDF samples with different percentages of bentonite or LiNbO3 were used to obtain composites via “casting,” and the modulus of elasticity (E) of the composites was studied using a specially designed system. The method used to obtain E took into account the strain energy and the strength of the materials. Based on the results, E decreased with an increased percentage of bentonite and, in the case of LiNbO3, for the percentages of 30% and 35% increases. Department of Physics Faculty of Science Universidade Estadual Paulista Julio de Mesquita Filho – UNESP Department of Physics Chemistry and Biology Faculty of Science and Technology Universidade Estadual Paulista Julio de Mesquita Filho UNESP Department of Physics Faculty of Science Universidade Estadual Paulista Julio de Mesquita Filho – UNESP Department of Physics Chemistry and Biology Faculty of Science and Technology Universidade Estadual Paulista Julio de Mesquita Filho UNESP

Silica was extracted from rice husk ash (RHA) by a sequence of reactions to produce nanosilica. Two laboratory routes, co-coagulation and spray drying, were used to incorporate the nanosilica into the rubber matrix. Samples were characterized regarding filler incorporation efficiency, thermal stability, rheological behavior and morphology. Thermogravimetric analysis showed that spray-drying was the most efficient filler incorporation process and also the presence of silica increased the thermal resistance of the rubber compound when compared to the unfilled rubber. The rheological behavior showed that NBR filled with silica presented higher elastic torque (S’), storage modulus (G’) and complex viscosity (η*) than unfilled rubber. The Payne effect was also observed for the composites produced by spray-drying. In addition, the thermal behavior and Payne effect results were supported by the comparison of morphology observed by FEG-SEM analysis.

This work shows the fractographic study of fractured surfaces resulted from tensile tests of thermoplastic composites based on poly(propylene-co-ethylene) (PP-PE) and modified PP-PE copolymers reinforced with continuous carbon fibers (CF). The PP-PE matrix was modified with two agents called AM1 (based on maleic anhydride) and AM2 (containing an elastomeric agent), respectively. Three different laminates - CF/PP-PE, CF/PP-PE(AM1) and CF/PP-PE(AM2) - were manufactured. The best tensile strength and elastic modulus results were determined for the CF/PP-PE(AM1) laminate (507.6 ± 11.8 MPa and 54.7 ± 2.4 GPa, respectively). These results show that the AM1 agent contributed to increase the physicochemical interaction between the CF and the PP-PE matrix. This condition provided a better loading transfer from matrix to the reinforcement. Scanning electron microscopy analyses of the fracture surfaces show the fractographic aspects of the samples and allow evaluating the fiber/matrix-interfacial adhesion. Poor adhesion is observed for the CF/PP-PE and CF/PP-PE(AM2) laminates with the presence of fiber impressions on the polymer rich regions and fiber surfaces totally unprotected of polymer matrix. On the other side, a more consistent adhesion is observed for the CF/PP-PE(AM1) laminate. This result is in agreement with the tensile test data and show the presence of a good interaction between the laminate constituents. The correlation of the mechanical and fractographic results with the curves of complex viscosity versus temperature of the studied polymer matrices shows that the matrix viscosity did not affect the wettability of the reinforcement.

This paper investigates the application of the luminescence spectroscopy technique in steady–state to study the moisture influence in glass fiber/epoxy prepreg and their laminates. The studies were monitored by intrinsic luminescence comparing the results with gravimetric analysis and near infrared with Fourier transform. Samples are cured and submitted to humidity controlled at 60 and 80 °C until 90 days. It is verified that the decrease in the maximum emission of the samples is directly related to the material moisture content. However, for very short periods, there is an increase in the relative intensity and blue shift of the emission band for all samples treated at 60 °C, which is related to an increase of the rigidity of the polymeric matrix. The results in this paper have a great significance because it brings a wide discussion on the interaction of water in epoxy composites materials.

The objective of this study was to assess the chemical, physical, morphological, crystalline and thermal properties of starch from two non-traditional vegetables, yam and taro. The analyses included proximate composition percent, amylose and mineral content, water absorption capacity, absolute density, morphological properties, X-ray diffractometry, thermal properties, pasting properties and infrared spectrum. The extracted starch exhibited a high purity level with low lipid, fiber and ash contents. The electron micrographs suggested that the taro starch granules were smaller than the yam starch granules. The results for the experimental conditions used in this study indicated that the studied starches differed, especially the amylose content, granule size and crystallinity degree and the pattern of the starches. Due to the high amylose content of yam starch, this type of starch can be used for film preparation, whereas the taro starch can be used as a fat substitute due to its small granule size.

Resumo A extração de poli(3-hidroxibutirato) (P(3HB)) com a utilização de solventes tóxicos e voláteis é contraditória à ideia do emprego destes biopolímeros para minimizar as agressões ambientais causadas pelos polímeros petroquímicos. O carbonato de propileno (CP) possui baixa toxicidade e alto ponto de ebulição, o que garante baixo risco de perdas por evaporação e alto rendimento de recuperação, podendo assim ser reutilizado. O objetivo deste trabalho foi verificar o efeito da reutilização do CP, recuperado do processo de extração de P(3HB) produzido por Cupriavidus necator, no rendimento e pureza do biopolímero e avaliar as perdas de solvente durante as etapas do processo de extração. Verificou-se a possibilidade de recuperar 80% do CP ao longo do processo. O solvente recuperado foi reutilizado onze vezes sem perder sua eficiência no rendimento e na pureza do produto. Desta forma, o presente estudo propõe a reutilização do CP, no processo de extração de P(3HB), contribuindo assim para a redução dos custos de produção deste biopolímero. Abstract Poly(3-hydroxybutyrate) (P(3HB)) extraction using toxic volatile solvents is contradictory to the idea of using this biopolymer to minimize environmental aggressions caused by petrochemical polymers. Propylene carbonate (PC) has low toxicity and high boiling point, which ensure a low risk of losses due to evaporation and high recovery performance, allowing for reuse. The aim of this study was to investigate the effect of reusing PC recovered the process of extraction of P(3HB) produced by Cupriavidus necator on the performance and purity of the biopolymer and evaluate the amount of solvent loss during the stages of the extraction process. It was observed that 80% of PC could be recovered throughout the process. The recovered solvent was reused eleven times without losing its efficiency in terms of product performance and purity. Hence, the present study proposes to reuse PC in the process of P(3HB) extraction, thus contributing to reduce the costs for the production of this biopolymer.

Resumo O presente artigo apresenta a aplicação e adequação dos modelos de percolação elétrica em trabalhos experimentais e teóricos da literatura para compósitos poliméricos condutores. Foi realizado um levantamento das publicações referentes aos modelos estudados para os diferentes tipos de cargas condutoras mais aplicadas na preparação destes compósitos, tais como pós metálicos, grafite, negro de fumo, nanofibras e nanotubos de carbono. A discussão está apresentada quanto à adequação dos modelos ao comportamento dos compósitos na influência das cargas nas propriedades elétricas de matrizes poliméricas.

In this work, low density polyethylene (LDPE)/plasticized starch (TPS) blends were prepared. The TPS employed in this study was obtained by plasticization of tapioca starch with a hyperbranched polyester polyol. Differential scanning calorimetry analysis showed that the melting temperature increased with the TPS content. The opposite effect was exhibited in the crystallization temperature and additional changes were not observed during the heating. X-ray diffraction analysis showed a reduction in intensity of the peak at Bragg’s angle 17.5°, proving a diminution on A type crystallinity with the increasing amount of LDPE. Micrographs obtained by scanning electron microscopy exhibited starch granules without destructure. TPS acted as a filler to LDPE, since the mechanical properties (Young’s modulus and tensile strength) improved ostensibly. The Young’ modulus and tensile strength decreased with the amount of LDPE, however, the elongation at break exhibited an opposite behavior.

Shrimp shells are a raw material rich in chitin, a precursor of chitosan biopolymer. The variables of processing (demineralization, deproteination and deacetylation) can be manipulated to determine the main characteristics of chitosan, the degree of deacetylation (DD), and average molar mass. This study evaluated the influence of one of the unit operations of shrimp shell physical processing, the milling, on the final product characteristic, chitosan. After different milling conditions, the raw material was subjected to standard chemical processing for chitin extraction, followed by deacetylation to obtain chitosan, which is characterized by 1H NMR, SEM, XRD, N2 physisorption (BET) and viscometry. The results indicated that the milling time of the raw material can be manipulated to increase the material depolymerization, significantly influencing the molecular weight reduction of chitosan a desirable feature for many applications of this biopolymer, and usually obtained by complex chemical and enzymatic methods.

N-isopropylacrylamide / itaconic acid hydrogels were prepared in this study, varying the proportion of itaconic acid in the pregel mixture. The kinetics of the hydrogel swelling at 4 °C was determined, obtaining the kintetic patameters, in accordance with the second-order kinetic model. Similarly, the capacity to absorb water in terms of temperature was determined, along with the transition temperature of the samples. The influence of temperature on the capacity of the hidrogels to absorb nickel from aqueous solutions at 5% of NiCl2 and its subsequent recuperation was determined.

The aim of this study was to evaluate the properties of nanocomposite films of protein isolates from mechanically deboned chicken meat with organoclay (montmorillonite). For the film development, a 23 experimental design was performed with three levels, protein isolate (2, 3.5, 5 g.100 mL-1 of solution), montmorillonite (0.3, 0.5, 0.7 g.100mL-1 of solution) and glycerol (25, 30, 35 g.100 mL-1 CPI). The tensile strength varied between 6.7 and 9.1 MPa, elongation to break from 26-66%, opacity of 13.1 to 35.7 and solubility from 38.5% to 81.8%. Assessing the structural properties, interleaving of the isolate and montmorillonite can be noted. The results obtained in the experimental design indicate that 2.0 g of CPI.100 g-1 of solution, 0.8 g of MMT.100 g-1of solution and 0.2 g of glicerol.100 g-1CPI are the ideal parameters for preparing nanocomposite films.

Resumo Neste trabalho foram desenvolvidas espumas flexíveis de poliuretano com a adição de celulose de Pinus nas concentrações de 0,5; 1 e 2% (m/m). A celulose foi submetida ao processo de fibrilação mecânica e posterior secagem por aspersão (spray dry) sendo caracterizada quanto a sua morfologia por MEV e MET. As espumas foram produzidas pelo método de batelada (one-shot) com a adição e mistura da fibra junto ao poliol. As espumas foram caracterizadas por MEV, densidade aparente e resistência à compressão. Os principais resultados indicam que a fibrilação mecânica promove a obtenção de fibras em escala nanométrica, porém durante a secagem, ocorre aglomeração ocasionando aumento para escala micrométrica. As propriedades mecânicas da espuma obtiveram acréscimos de 40 e 50% na resistência à compressão com a adição de 0,5 e 1% de celulose, respectivamente, evidenciando seu potencial como aditivo alternativo para o desenvolvimento de espumas de poliuretano. Abstract In this work, flexible polyurethane foams were developed with the addition of Pinus cellulose at concentrations of 0.5; 1 and 2 wt%. The cellulose was subjected to mechanical fibrillation process and subsequent dried by spray dry process. It was characterized morphologically by SEM and TEM. The foams were produced by one-shot method by adding and mixing the fiber with the polyol. The foams were characterized by SEM, apparent density and compression strength. The main results indicate that the mechanical fibrillation promotes the obtainment of nanoscale fibers, but during the drying process, agglomeration occurs causing an increase reaching the micrometer scale. The mechanical properties of the foam increased by 40 and 50% in compressive strength with the addition of 0.5% and 1% of cellulose, respectively, showing its potential as an alternative additive for the development of polyurethane foams.

Made available in DSpace on 2018-12-11T17:32:49Z (GMT). No. of bitstreams: 0 Previous issue date: 2017-01-01. Added 1 bitstream(s) on 2021-07-15T15:04:18Z : No. of bitstreams: 1 S0104-14282017000700056.pdf: 1341788 bytes, checksum: d856bd72b662f0aff65ce5ae78099fbf (MD5) In this work, dynamic mechanical properties and viscosity of multiwalled carbon nanotubes reinforced poly (phenylene sulfide) nanostructured composites obtained by melt mixing techinique were investigated. The storage modulus (E') and the glass transition temperature (Tg) showed increases up to 130% and 11 °C for concentrations of 2.0 wt% compared to neat PPS. In Addition, it was observed for concentrations above 1.0 wt% an increment of complex viscosity (η∗), suggesting the formation of an interconnected nanotube structure within the polymeric matrix. Departamento de Materiais e Tecnologia Universidade Estadual Paulista 'Júlio de Mesquita Filho' - UNESP Departamento de Materiais e Tecnologia Universidade Estadual Paulista 'Júlio de Mesquita Filho' - UNESP

Resumo Nesse trabalho foi desenvolvido filme de PHB/quitosana com aplicação promissora em embalagens de alimentos e medicamentos. Esses filmes foram preparados via casting solution e após esterilização térmica ou radiolítica suas propriedades foram avaliadas a partir da microscopia eletrônica de varredura, ensaio de tração, calorimetria exploratória diferencial e análise termogravimétrica. Foram constatadas alterações na morfologia dos filmes de PHB/quitosana após os processos de esterilização. As propriedades mecânicas da blenda se mantiveram aproximadamente constantes após esterilização térmica. Porém, após irradiação as blendas apresentaram-se quebradiças. As propriedades térmicas da blenda foram alteradas apenas para as doses de 50 e 75 kGy, em que foi observado uma redução no valor da entalpia de cristalização, grau de cristalinidade, cristalinidade relativa e taxa de cristalização da blenda. Foi observado que a degradação térmica dos filmes de PHB e das blendas, antes e após os processos de esterilização apresentaram um único estágio (250-300 °C). Abstract In this work was developed PHB/chitosan film with promising application in food and medicine packaging. These films were prepared by the casting solution and after radiolytic or thermal sterilization their properties were evaluated by scanning electron microscopy, tensile testing, differential scanning calorimetry and thermogravimetric analysis. PHB/chitosan films changed their morphology after sterilization processes. Mechanical properties of the blend remained approximately constant after thermal sterilization. But, after irradiation the blends presented brittle. Thermal properties of the blend were changed only for the doses of 50 and 75 kGy, in which case was observed a reduction in the crystallization enthalpy value, the degree of crystallinity, relative crystallinity and crystallization rate of the blend. It was observed thermal degradation of the PHB films and blends, before and after sterilization processes presented a single stage (250-300 °C).

Resumo A Engenharia de Tecidos envolve o desenvolvimento de novos materiais ou dispositivos capazes de interações específicas com os tecidos biológicos, buscando a utilização de materiais biocompatíveis que devem servir como arcabouço para o crescimento de células in vitro, organizando e desenvolvendo o tecido que posteriormente será implantado no paciente. Uma variedade de arcabouços como hidrogéis poliméricos, sintéticos e naturais, têm sido investigados para a expansão de condrócitos in vitro, visando o reparo da cartilagem lesionada. Um hidrogel de interesse particular na regeneração de cartilagem é o ácido hialurónico (AH). Trata-se de um biopolímero atraente para a fabricação de arcabouços artificiais para Engenharia de Tecidos por ser biocompatível e biodegradável. A biocompatibilidade do AH deve-se ao fato de estar presente na matriz extracelular nativa, deste modo, cria-se um ambiente propício que facilita a adesão, proliferação e diferenciação celular, além da existência de sinalização celular específica, o que contribui para a regeneração do tecido. O uso de hidrogel composto de ácido hialurónico e quitosana (QUI) também tem sido investigado em aplicações de Engenharia de Tecidos de cartilagem, com resultados promissores. Baseando-se nestas informações, o objetivo este trabalho foi investigar as alternativas disponíveis para regeneração tecidual da cartilagem e conhecer mais detalhadamente as relações entre células e biomateriais. Abstract Tissue Engineering involves the development of new materials or devices capable of specific interactions with biological tissues, searching the use of biocompatible materials as scaffolds for cell growth in vitro, organizing and developing tissue that is subsequently implanted into the patient. A variety of scaffolds such as polymeric hydrogels, natural and synthetic, have been investigated for the expansion of chondrocytes in vitro in order to repair the damaged cartilage. A hydrogel of particular interest in cartilage regeneration is hyaluronic acid (HA). HA are attractive biopolymers for manufacturing artificial scaffolds for Tissue Engineering, it is biocompatible and biodegradable. The biocompatibility of HA is due to the fact that it is present in native extracellular matrix, thus creates an environment, which facilitates the adhesion, proliferation and differentiation, in addition to the existence of specific cell signaling, which contributes to tissue regeneration. The use of hydrogel composed of hyaluronic acid and chitosan (CHI) has also been investigated for applications in Tissue Engineering of soft tissues, like cartilage, with promising results. Based on this information, this study aims to investigate the alternatives available for cartilage tissue regeneration and meet more detail the relationships between cells and biomaterials.

The life cycle of a product depends to a great extent on its reuse and ease of recycling. This work had developed of composite materials of reprocessed polypropylene composites with rice husk ash (RHA) and sugarcane bagasse ash (SBA) through the coextrusion and injection processes as main purpose. The polymeric matrix was reprocesed until six generations by the injection technique. The reprocessed PP was mixed in 80:20 proportions with respect to filler mineral, using maleic anhydride as coupling agent in a coextrusion machine. The new series of composite materials were analyzed thermal, mechanical, rheological and morphologically. The incorporation of ashes in the PP matrix achieved characteristics of improved tensile strength, conserving the thermal properties. For this reason, this work presents an alternative for the manufacture of composite materials from post-industrial waste.

Industries and the scientific community currently focus on creating new ways to recycle and to reuse polymer waste that leads to serious socio-environmental risks. However, the quality of recycled polyethylenes depends strongly on their purity degree, but the distinction between Low Density Polyethylene (LDPE) and High Density Polyethylene (HDPE) by a fast and consistently good methodology is still an unsolved issue for the current recycling processes. In this study, confocal Raman spectroscopy and Competitive Adaptive Reweighted Sampling - Partial Least Squares (CARS-PLS) linear regression have been successfully applied to quantify the concentration of LDPE/HDPE blends. The effects of several regression parameters (pretreatment method, Monte Carlo sampling runs, k-fold and maximal number of latent variables for cross-validation) on the CARS-PLS model training and prediction performance were analyzed. The CARS-PLS-based models show root-mean-squared prediction error of 4.06 - 8.87 wt% of LDPE for the whole composition range of HDPE/LDPE blend.

The release kinetics of nitrogen and phosphorous of a granulated fertilizer, encapsulated in a κ-carrageenan-based hydrogel (CBH), was evaluated in order to determine its release mechanism given the potential this hydrogel has as coating material for controlled release fertilizers (CFRs). The effect of pH on the release properties was also investigated. The relationship between the NH4+, NO3-, and PO43- release of encapsulated fertilizers and time was determined by short- and long-term laboratory incubations. The mechanism of the release of nutrient ions was determined by comparing the release data with the zero-order, first-order, Higuchi, Hixon-Crowell and Korsmeyer-Peppas kinetic models. The findings showed that the Korsmeyer-Peppas model could be used to describe the release characteristics of the nutrients in the encapsulated fertilizers and that non-Fickian diffusion is the main release mechanism. The experimental hydrogel showed a high water retention capacity able to absorb 300 times its weight water.