Aproveitamento da fibra do epicarpo do coco babaçu em compósito com matriz epóxi: estudo do efeito do tratamento da fibra

Nowadays the environmental issues are increasingly highlighted since the future of humanity is dependent on the actions taken by man. Major efforts are being expended in pursuit of knowledge and alternatives to promote sustainable development without compromising the environment. In recent years there has been a marked growth in the development of reinforced composite fiber plants, as an alternative for economic and ecological effects, especially in the substitution of synthetic materials such as reinforcement material in composites. In this current study the chemical- physical or (thermophysics )characteristics of the babassu coconut fiber, derived from the epicarp of the fruit (Orbignyda Phalerata), which the main constituents of the fiber: Klason lignin, insoluble, cellulose, holocellulose, hemicellulose and the content of ash and moisture will be determined. A study was conducted about the superficial modification of the fibers of the epicarp babassu coconut under the influence of chemical treatment by alkalinization, in an aqueous solution of NaOH to 2.5% (m/v) and to 5.0% to improve the compatibility matrix / reinforcement composite with epoxy matrix. The results of the changes occurred in staple fibers through the use of the techniques of thermogravimetric analyses (TG) and differential scanning calorimetry (DSC). The results found on thermal analysis on samples of fiber without chemical treatment (alkalinities), and on fiber samples treated by alkalinization show that the proposed chemical treatment increases the thermal stability of the fibers and provides a growth of the surface of area fibers, parameters that enhance adhesion fiber / composite. The findings were evaluated and compared with published results from other vegetable fibers, showing that the use of babassu coconut fibers has technical and economic potential for its use as reinforcement in composites

O efeito do tratamento da atapulgita no desenvolvimento de compósito com o polietileno reciclado

The study aimed at the treatment of attapulgite for the development and characterization of composite recycled low density polyethylene - PEBD_rec embedded with natural attapulgite - ATP_NAT, sifted - ATP_PN and attapulgite treated with sulfuric acid - ATP_TR in different compositions (1, 3 and 5%) and compared with the PEBD_rec. The atapulgitas, natural, screened and treated, were characterized by X-ray diffraction (XRD), X-ray fluorescence (XRF), particle size analysis, scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and determining the area specific surface (BET). The composites were characterized by thermogravimetry (TG), differential scanning calorimetry (DSC), Xray diffraction (XRD), torque rheometry, scanning electron microscopy (SEM) and traction. The composite PEBD_rec / ATP (natural, sieved and treated) were produced by mixing in the molten state in a single screw extruder matrix wire with subsequent reprocessing matrix tape. It was found that the screening of attapulgite not reduce the quantity of quartz and the acid treatment completely extracted dolomite aggregate impurities of the channels attapulgite, and increase their surface area. The addition of attapulgite in PEBD_rec acts as a catalyst, reducing the thermal stability of the polymer. The increased concentration of attapulgite, increases resistance and reduces the elongation at break and modulus of elasticity of the composite PEBD_rec / attapulgite

Desenvolvimento e caracterização de compósitos poli(tereftalato de etileno) reciclado (PET reciclado) com flocos de vidro.

The growing concern with the solid residues management, observed in the last decade, due to its huge amount and impact, has motivated the search for recycling processes, where these residues can be reprocessed to generate new products, enlarging the cycle of materials and energy which are present. Among the polymeric residues, there is poly (ethylene terephthalate) (PET). PET is used in food packaging, preferably in the bottling of carbonated beverages. The reintegration of post-consumer PET in half can be considered a productive action mitigation of environmental impacts caused by these wastes and it is done through the preparation of several different products at the origin, i.e. food packaging, with recycling rates increasing to each year. This work focused on the development and characterization mechanical, thermal, thermo-mechanical, dynamic mechanical thermal and morphology of the pure recycled PET and recycled PET composites with glass flakes in the weight fraction of 5%, 10% and 20% processed in a single screw extruder, using the following analytical techniques: thermogravimetry (TG), differential scanning calorimetry (DSC), tensile, Izod impact, Rockwell hardness, Vicat softening temperature, melt flow rate, burn rate, dynamic mechanical thermal analysis (DMTA) and scanning electron microscopy (SEM). The results of thermal analysis and mechanical properties leading to a positive evaluation, because in the thermograms the addition of glass flakes showed increasing behavior in the initial temperatures of thermal decomposition and melting crystalline, Furthermore was observed growing behavior in the mechanical performance of polymer composites, whose morphological structure was observed by SEM, verifying a good distribution of glass flakes, showing difference orientation in the center and in the surface layer of test body of composites with 10 and 20% of glass flakes. The results of DMTA Tg values of the composites obtained from the peak of tan ä showed little reductions due to poor interfacial adhesion between PET and recycled glass flakes.

Síntese e caracterização do poli(ácido láctico) para potencial uso em sistemas de liberação controlada de fármacos

With the advances in medicine, life expectancy of the world population has grown considerably in recent decades. Studies have been performed in order to maintain the quality of life through the development of new drugs and new surgical procedures. Biomaterials is an example of the researches to improve quality of life, and its use goes from the reconstruction of tissues and organs affected by diseases or other types of failure, to use in drug delivery system able to prolong the drug in the body and increase its bioavailability. Biopolymers are a class of biomaterials widely targeted by researchers since they have ideal properties for biomedical applications, such as high biocompatibility and biodegradability. Poly (lactic acid) (PLA) is a biopolymer used as a biomaterial and its monomer, lactic acid, is eliminated by the Krebs Cycle (citric acid cycle). It is possible to synthesize PLA through various synthesis routes, however, the direct polycondensation is cheaper due the use of few steps of polymerization. In this work we used experimental design (DOE) to produce PLAs with different molecular weight from the direct polycondensation of lactic acid, with characteristics suitable for use in drug delivery system (DDS). Through the experimental design it was noted that the time of esterification, in the direct polycondensation, is the most important stage to obtain a higher molecular weight. The Fourier Transform Infrared (FTIR) spectrograms obtained were equivalent to the PLAs available in the literature. Results of Differential Scanning Calorimetry (DSC) showed that all PLAs produced are semicrystalline with glass transition temperatures (Tgs) ranging between 36 - 48 °C, and melting temperatures (Tm) ranging from 117 to 130 °C. The PLAs molecular weight characterized from Size Exclusion Chromatography (SEC), varied from 1000 to 11,000 g/mol. PLAs obtained showed a fibrous morphology characterized by Scanning Electron Microscopy (SEM)

Síntese e caracterização do líquido iônico tetrafluoroborato de 1-metil-3-(2,6-(S)-dimetiloct-2-eno)-imidazol como eletrólito para produção de hidrogênio via eletrólise da água

Ionic liquids (ILs) are organic compounds liquid at room temperature, good electrical conductors, with the potential to form as a means for electrolyte on electrolysis of water, in which the electrodes would not be subjected to such extreme conditions demanding chemistry [1]. This paper describes the synthesis, characterization and study of the feasibility of ionic liquid ionic liquid 1-methyl-3(2,6-(S)-dimethyloct-2-ene)-imidazole tetrafluoroborate (MDI-BF4) as electrolyte to produce hydrogen through electrolysis of water. The MDI-BF4 synthesized was characterized by thermal methods of analysis (Thermogravimetric Analysis - TG and Differential Scanning Calorimetry - DSC), mid-infrared spectroscopy with Fourier transform by method of attenuated total reflectance (FTIR-ATR), nuclear magnetic resonance spectroscopy of hydrogen (NMR 1H) and cyclic voltammetry (CV). Where thermal methods were used to calculate the yield of the synthesis of MDI-BF4 which was 88.84%, characterized infrared spectroscopy functional groups of the compound and the binding B-F 1053 cm-1; the NMR 1H analyzed and compared with literature data defines the structure of MDI-BF4 and the current density achieved by MDI-BF4 in the voltammogram shows that the LI can conduct electrical current indicating that the MDI-BF4 is a good electrolyte, and that their behavior does not change with the increasing concentration of water

Avaliação da argila atapulgita para potencial uso como excipiente farmacêutico em formas sólidas

Clays are natural materials that have great potential for use as excipients for solid dosage forms. Palygorskite is a type of clay that has hydrophilic properties as well as a large surface area, which could contribute to the dissolution of drugs. Thus, the present study aims to evaluate the use of palygorskite clay, from Piaui (Northeast region of Brazil), as a pharmaceutical excipient for solid dosage forms, using rifampicin and isoniazid as the model drugs. The former is a poorly soluble drug often associated with isoniazid for tuberculosis treatment. Palygorskite was characterized by X-ray diffraction (XRD), X-ray fluorescence (XRF), particle size, transmission electron microscopy (TEM), scanning electron microscopy (SEM) and specific surface area (BET). The rheological and technological properties of palygorskite were determined and compared to those of talc, magnesium stearate and Aersosil 200. Mixtures between drugs and palygorskite were analyzed by differential scanning calorimetry (DSC), thermogravimetric analysis (TG) combined with thermal analysis (DTA) and Fourier Transform Infrared Spectroscopy (FT-IR), where the results were compared with those of the individual compounds. In addition, dissolution studies of solid dispersions and capsules containing the drugs, mixed with either palygorskite or a mixture of talc and magnesium stearate, were performed. The results showed that palygorskite has small particles with a high surface area. Its rheological characteristics were better than those of others commonly used glidants and lubricants. There was no interaction between palygorskite and the drugs (rifampicin and isoniazid). Among the dispersions studied, the mixture with palygorskite (5%) showed the highest drug dissolution when compared to other excipients. The dissolution of the rifampicin capsules containing palygosrkite was faster in higher concentrations. However, these differences were statistically different only in the first minutes of the dissolution experiment. The dissolution profile of isoniazid was also statistically different on the initial part of the experiment. The formulations prepared with isoniazid and palygorskite showed higher drug dissolution, but it was in descending order of concentration. According to these results, the palygorskite clay used in this study has great potential for application as an excipient for solid dosage forms

Dispersões sólidas de sinvastatina: preparação, caracterização, no estado sólido utilizando técnicas emergentes e estudo de estabilidade

This thesis aimed to assess the increase in solubility of simvastatin (SINV) with solid dispersions using techniques such as kneading (MA), co-solvent evaporation (ES), melting carrier (FC) and spray dryer (SD). Soluplus (SOL), PEG 6000 (PEG), PVP K-30 (PVP) e sodium lauryl sulphate (LSS) were used as carriers. The solid dispersions containing PEG [PEG-2(SD)], Soluplus [SOL-2(MA)] and sodium lauryl sulphate [LSS-2(ES)] were presented with a greater increase in solubility (5.02, 5.60 and 5.43 times respectively); analyses by ANOVA between the three groups did not present significant difference (p<0.05). In the phase solubility study, the calculation of the Gibbs free energy (ΔG) revealed that the spontaneity of solubilisation of SINV occurred in the order SOL>PEG >PVP 75%>LSS, always 80%. The phase diagrams of PEG and LSS presented solubilization stoichiometry of type 1:1 (type AL). The diagrams with PVP and SOL tend to 1:2 stoichiometry (type AL + AP). The stability coefficients (Ks) of the phase diagrams revealed that the most stable reactions occurred with LSS and PVP. The solid dispersions were characterized by Fourier transform infrared (FTIR), differential scanning calorimetry (DSC), scanning electron microscopy (SEM), particle size distribution (PSD), near-infrared spectroscopy imaging (NIR-CI) and X-ray diffraction of the powder using the Topas software (PDRX-TOPAS). The solid dispersion PEG-2(SD) presented the greatest homogeneity and the lowest degree of crystallinity (18.2%). The accelerated stability study revealed that the solid dispersions are less stable than SINV, with PEG-2(SD) being the least stable, confirmed by FTIR and DSC. The analyses by PDRX-TOPAS revealed the amorphous character of the dispersions and the mechanism of increasing solubility

Eletrofiação e caracterização de membranas biopoliméricas a base de quitosana extraídas dos exoesqueletos de crustáceos

Chitin and chitosan are nontoxic, biodegradable and biocompatible polymers produced by renewable natural sources with applications in diverse areas such as: agriculture, textile, pharmaceutical, cosmetics and biomaterials, such as gels, films and other polymeric membranes. Both have attracted greater interest of scientists and researchers as functional polymeric materials. In this context, the objective of this study was to take advantage of the waste of shrimp (Litopenaeus vannamei and Aristeus antennatus) and crabs (Ucides cordatus) from fairs, beach huts and restaurant in Natal/RN for the extraction of chitin and chitosan for the production of membranes by electrospinning process. The extraction was made through demineralization, deproteinization, deodorization and deacetylation. Morphological analyzes (SEM and XRD), Thermal analysis (TG and DTG), Spectroscopy in the Region of the Infrared with Transformed of Fourier (FTIR) analysis Calorimetry Differential Scanning (DSC) and mechanical tests for traction were performed. In (XRD) the semicrystalline structure of chitosan can be verified while the chitin had higher crystallinity. In the thermal analysis showed a dehydration process followed by decomposition, with similar behavior of carbonized material. Chitosan showed temperature of maximum degradation lower than chitin. In the analysis by Differential Scanning Calorimetry (DSC) the curves were coherent to the thermal events of the chitosan membranes. The results obtained with (DD) for chitosan extracted from Litopenaeus vannamei and Aristeus antennatus shrimp were (80.36 and 71.00%) and Ucides cordatus crabs was 74.65%. It can be observed that, with 70:30 solutions (v/v) (TFA/DCM), 60 and 90% CH3COOH, occurred better facilitate the formation of membranes, while 100:00 (v/v) (TFA/DCM) had formation of agglomerates. In relation to the monofilaments diameters of the chitosan membranes, it was noted that the capillary-collector distance of 10 cm and tensions of 25 and 30 kV contributed to the reduction of the diameters of membranes. It was found that the Young s modulus decreases with increasing concentration of chitosan in the membranes. 90% CH3COOH contributed to the increase in the deformation resulting in more flexible material. The membranes with 5% chitosan 70:30 (v/v) (TFA/DCM) had higher tensile strength

Avaliação tribológica dos polímeros NBR, PTFE e PTFE gravitado em contato com aço AISI 52100

Low cost seals are made of NBR, Nitrile Butadiene Rubber, a family of unsaturated copolymers that is higher resistant to oils the more content of nitrile have in its composition, although lower its flexibility. In Petroleum Engineering, NBR seal wear can cause fluid leakage and environmental damages, promoting an increasing demand for academic knowledge about polymeric materials candidate to seals submitted to sliding contacts to metal surfaces. This investigation aimed to evaluate tribological responses of a commercial NBR, hardness 73 ± 5 Sh A, polytetrafluoroethylene (PTFE), hardness 60 ± 4 HRE and PTFE with graphite, 68 ± 6 HRE. The testings were performed on a sliding tribometer conceived to explore the tribological performance of stationary polymer plane coupons submitted to rotational cylinder contact surface of steel AISI 52100, 20 ± 1 HRC Hardness, under dry and lubricated (oil SAE 15W40) conditions. After screening testings, the normal load, relative velocity and sliding distance were 3.15 N, 0.8 m/s and 3.2 km, respectively. The temperatures were collected over distances of 3.0±0.5 mm and 750±50 mm far from the contact to evaluate the heating in this referential zone due to contact sliding friction by two thermocouples K type. The polymers were characterized through Thermogravimetric Analysis (TGA), Differential Scanning Calorimetry (DSC) and Dynamic Mechanical Analysis (DMA). The wear mechanisms of the polymer surfaces were analyzed by Scanning Electron Microscopy (SEM) and EDS (Energy-Dispersive X-ray Spectroscopy). NBR referred to the higher values of heating, suggesting higher sliding friction. PTFE and PTFE with graphite showed lower heating, attributed to the delamination mechanism

Mecanismos de desgaste de poliuretano em ensaios de microabrasão

Wear mechanisms and thermal history of two non-conforming sliding surfaces was investigated in laboratory. A micro-abrasion testing setup was used but the traditional rotative sphere method was substituted by a cylindrical surface of revolution which included seven sharp angles varying between 15o to 180o. The micro-abrasion tests lead to the investigation on the polyurethane response at different contact pressures. For these turned counterfaces with and without heat treatment. Normal load and sliding speeds were changed. The sliding distance was fixed at 5 km in each test. The room and contact temperatures were measured during the tests. The polyurethane was characterized using tensile testing, hardness Shore A measurement, Thermogravimetric Analysis (TGA), Differential Scanning Calorimetry (DSC) and Thermomechanical Analyze (TMA). The Vickers micro-hardness of the steel was measured before and after the heat treatment and the metallographic characterization was also carried out. Worn surface of polyurethane was analysed using Scanning Electron Microscope (SEM) and EDS (Electron Diffraction Scanning) microanalyses. Single pass scratch testing in polyurethane using indenters with different contact angles was also carried out. The scar morphology of the wear, the wear mechanism and the thermal response were analyzed in order to correlate the conditions imposed by the pressure-velocity pair to the materials in contact. Eight different wear mechanisms were identified on the polyurethane surface. It was found correlation between the temperature variation and the wear scar morphology.

Estudo da incorporação de resíduo industrial polimérico ao CAP

This work presents the incorporation of an industrial polymeric waste into a petroleum asphalt cement with penetration grade 50-60 (CAP 50-60). The main goal of this research is the development of a polymer-modified asphalt, with improvements in its physical properties, in order to obtain a more resistant material to the traffic loads. Furthermore, the use of this polymeric waste will result in economic and environmental benefits. The CAP 50-60 used in this research was kindly supplied by LUBNOR Lubrificantes e Derivados de Petróleo do Nordeste (produced in Fazenda Belém Aracati - Ceará) and the industrial polymeric waste was provided by a button manufacturer industry, located in Rio Grande do Norte state. This polymeric waste represents an environmental problem due to its difficulty in recycling and disposal, being necessary the payment by the industry to a landfill. The difficulty in its reuse is for being this material a termofixed polymer, as a result, the button chips resulting from the molding process cannot be employed for the same purpose. The first step in this research was the characterization of the polymeric waste, using Differential Scanning Calorimetry (DSC) Infrared spectroscopy (IR spectroscopy), and Thermogravimetric analysis (TGA). Based on the results, the material was classified as unsaturated polyester. After, laboratory experiments were accomplished seeking to incorporate the polymeric waste into the asphalt binder according to a 23 experimental factorial design, using as main factors: the polymer content (2%, 7% and 14%), the temperature of the mixture (140 and 180 oC) and the reaction time (20 and 60 minutes). The characterization of the polymer-modified asphalt was accomplished by traditional tests, such as: penetration, ring and ball softening point, viscosity, ductility and flash point temperature. The obtained results demonstrated that the addition of the polymeric waste into the asphalt binder modified some of its physical properties. However, this addition can be considered as a feasible alternative for the use of the polymeric waste, which is a serious environmental and technological problem.

Extração de ferro da cera de carnaúba utilizando sistemas microemulsionados

The constant search for biodegradable materials for applications in several fields shows that carnauba wax can be a viable alternative in the manufacturing of biolubricants. Carnauba wax is the unique among the natural waxes to have a combination of properties of great importance. In previous studies it was verified the presence of metals in wax composition that can harm the oxidative stability of lubricants. Considering these factors, it was decided to develop a research to evaluate iron removal from carnauba wax, using microemulsion systems (Me) and perform the optimization of parameters, such as: extraction pH, temperature, extraction time, among others. Iron concentration was determined by atomic absorption and, to perform this analysis, sample digestion in microwave oven was used, showing that this process was very efficient. It was performed some analysis in order to characterize the wax sample, such as: attenuated total reflectance infrared spectroscopy (ATR-IR), thermogravimetry (TG), differential scanning calorimetry (DSC), energy dispersive X-ray fluorescence (EDXRF), scanning electron microscopy (SEM) and melting point (FP). The microemulsion systems were composed by: coconut oil as surfactant, n-butanol as cosurfactant, kerosene and/or heptanes as oil phase, distilled water as water phase. The pH chosen for this study was 4.5 and the metal extraction was performed in finite experiments. To evaluate Me extraction it was performed a factorial design for systems with heptane and kerosene as oil phase, also investigating the influence of temperature time and wax/Me ratio, that showed an statistically significant answer for iron extraction at 95% confidence level. The best result was obtained at 60°C, 10 hours contact time and 1: 10 wax/Me ratio, in both systems with kerosene and heptanes as oil phase. The best extraction occurred with kerosene as oil phase, with 54% iron removal

Preparação de poliuretana à base de óleo de mamona

Polyurethanes are very versatile macromolecular materials that can be used in the form of powders, adhesives and elastomers. As a consequence, they constitute important subject for research as well as outstanding materials used in several manufacturing processes. In addition to the search for new polyurethanes, the kinetics control during its preparation is a very important topic, mainly if the polyurethane is obtained via bulk polymerization. The work in thesis was directed towards this subject, particularly the synthesis of polyurethanes based castor oil and isophorone diisocianate. As a first step castor oil characterized using the following analytical methods: iodine index, saponification index, refraction index, humidity content and infrared absorption spectroscopy (FTIR). As a second step, test specimens of these polyurethanes were obtained via bulk polymerization and were submitted to swelling experiments with different solvents. From these experiments, the Hildebrand parameter was determined for this material. Finally, bulk polymerization was carried out in a differential scanning calorimetry (DSC) equipment, using different heating rates, at two conditions: without catalyst and with dibutyltin dilaurate (DBTDL) as catalyst. The DSC curves were adjusted to a kinetic model, using the isoconversional method, indicating the autocatalytic effect characteristic of this class of polymerization reaction

Estudo da estabilidade térmica de adoçantes naturais e artificiais

Sweeteners provide a pleasant sensation of sweetness that helps the sensory quality of the human diet, can be divided into natural sweeteners such as fructose, galactose, glucose, lactose and sucrose, and articial sweeteners such as aspartame, cyclamate and saccharin. This work aimed to study the thermal stability of natural and artificial sweeteners in atmospheres of nitrogen and syntetic air using thermogravimetry (TG), derivative thermogravimetry (DTG), Differential Thermal Analysis (DTA) and Differential Scanning Calorimetry (DSC). Among the natural sweeteners analyzed showed higher thermal stability for the lactose and sucrose, which showed initial decomposition temperatures near 220 ° C, taking advantage of the lactose has a higher melting point (213 ° C) compared to sucrose (191 ° C). The lower thermal stability was observed for fructose, it has the lowest melting point (122 °C) and the lower initial decomposition temperature (170 °C). Of the artificial sweeteners studied showed higher thermal stability for sodium saccharin, which had the highest melting point (364 ° C) as well as the largest initial decomposition temperature (466 ° C under nitrogen and 435 ° C in air). The lower thermal stability was observed for aspartame, which showed lower initial decomposition temperature (158 ° C under nitrogen and 170 ° C under air). For commercial sweeteners showed higher thermal stability for the sweeteners L and C, which showed initial temperature of thermal decomposition near 220 ° C and melting points near 215 ° C. The lower thermal stability was observed for the sweetener P, which showed initial decomposition temperature at 160 ° C and melting point of 130 °C. Sweeteners B, D, E, I, J, N and O had low thermal stability, with the initial temperature of decomposition starts near 160 °C, probably due to the presence of aspartame, even if they have as the main constituent of the lactose, wich is the most stable of natural sweeteners. According to the results we could also realize that all commercial sweeteners are in its composition by at least a natural sweeteners and are always found in large proportions, and lactose is the main constituent of 60% of the total recorded

Estudo termoanalítico de medicamentos de referência, genérico e similar

This study aimed to apply, thermogravimetriy /derivative Thermogravimetriy (TG/DTG), differential scanning calorimetry (DSC), Differential Thermal Analysis (DTA), to conduct a comparative study on drug reference, generic and whose active principles are similar captopril hydrochlorothiazide, ampicillin, paracetamol, aspirin and mebendazole sold in local pharmacies. Samples of the active ingredients and dosage forms were also characterized by absorption infrared spectroscopy (IR), X-ray diffraction (XRD) and microscopy scanning electron (SEM). The TG / DTG curves showed a general similarity in the thermal behavior of the samples, but also showed the influence of excipients on the thermal stability. The DSC curve of the generic base hydrochlorothiazide showed no peak on the fusion of the drug due to interference of lactose as a diluent, which causes interaction with the active principle causing their degradation before the merger. The DSC curves of the drugs consisting of paracetamol showed reproducibility at the melting point of the active and the other thermal events. The DSC result of binary mixtures involving captopril / magnesium stearate and mebendazole/magnesium stearate showed possible interactions or incompatibilities evidenced by the displacement of the melting point of both drugs. The other mixtures showed no change. The infrared spectra presented were very similar, indicating the presence of functional groups characteristic of the constituents of the samples. The X-ray diffraction showed peaks indicative of crystalline structure of the active ingredients as well as some of the ingredients in the formulation of the drug and the micrographs indicate a general heterogeneity in the size distribution of particles in the samples