Host-guest system of 4-nerolidylcatechol in 2-hydroxypropyl-beta-cyclodextrin: preparation, characterization and molecular modeling

The interaction of 4-nerolidylcatechol (4-NRC), a potent antioxidant agent, and 2-hydroxypropyl-beta-cyclodextrin (HP-beta-CD) was investigated by the solubility method using Fourier transform infrared (FTIR) methods in addition to UV-Vis, (1)H-nuclear magnetic resonance (NMR) spectroscopy and molecular modeling. The inclusion complexes were prepared using grinding, kneading and freeze-drying methods. According to phase solubility studies in water a B(S)-type diagram was found, displaying a stoichiometry complexation of 2:1 (drug:host) and stability constant of 6494 +/- A 837 M(-1). Stoichiometry was established by the UV spectrophotometer using Job`s plot method and, also confirmed by molecular modeling. Data from (1)H-NMR, and FTIR, experiments also provided formation evidence of an inclusion complex between 4-NRC and HP-beta-CD. 4-NRC complexation indeed led to higher drug solubility and stability which could probably be useful to improve its biological properties and make it available to oral administration and topical formulations.

Wear of coated and uncoated PCBN cutting tool used in turning and milling

This licentiate thesis has the main focus on evaluation of the wear of coated and uncoated polycrystalline cubic boron nitride cutting tool used in cutting operations against hardened steel. And to exam the surface finish and integrity of the work material used. Harder work material, higher cutting speed and cost reductions result in the development of harder and more wear resistance cutting tools. Although PCBN cutting tools have been used in over 30 years, little work have been done on PVD coated PCBN cutting tools. Therefore hard turning and hard milling experiments with PVD coated and uncoated cutting tools have been performed and evaluated. The coatings used in the present study are TiSiN and TiAlN. The wear scar and surface integrity have been examined with help of several different characterization techniques, for example scanning electron microscopy and Auger electron spectroscopy.   The results showed that the PCBN cutting tools used displayed crater wear, flank wear and edge micro chipping. While the influence of the coating on the crater and flank wear was very small and the coating showed a high tendency to spalling. Scratch testing of coated PCBN showed that, the TiAlN coating resulted in major adhesive fractures. This displays the importance of understanding the effect of different types of lapping/grinding processes in the pre-treatment of hard and super hard substrate materials and the amount and type of damage that they can create. For the cutting tools used in turning, patches of a adhered layer, mainly consisting of FexOy were shown at both the crater and flank. And for the cutting tools used in milling a tribofilm consisting of SixOy covered the crater. A combination of tribochemical reactions, adhesive wear and mild abrasive wear is believed to control the flank and crater wear of the PCBN cutting tools. On a microscopic scale the difference phases of the PCBN cutting tool used in turning showed different wear characteristics. The machined surface of the work material showed a smooth surface with a Ra-value in the range of 100-200 nm for the turned surface and 100-150 nm for the milled surface. With increasing crater and flank wear in combination with edge chipping the machined surface becomes rougher and showed a higher Ra-value. For the cutting tools used in milling the tendency to micro edge chipping was significant higher when milling the tools steels showing a higher hard phase content and a lower heat conductivity resulting in higher mechanical and thermal stresses at the cutting edge.

Estudo sobre a potencialidade de uso das escórias de aciaria como adição ao concreto

A geração de resíduos tem se mostrado um problema de preocupação mundial crescente. Muitos rejeitos, sejam industriais ou urbanos, muitas vezes acabam por poluir o meio-ambiente, causando problemas de armazenagem de certos materiais. Além disso, materiais alternativos a partir desses rejeitos podem ser mais baratos, apresentando muitas vezes características de desempenho melhores que os materiais convencionais. As siderúrgicas, em nível mundial, vêm enfrentando um problema comum, que consiste no que fazer para que a totalidade da escória gerada no refino do aço em aciarias elétricas ou à oxigênio tenha uma solução de aproveitamento melhor do que vem sendo feito atualmente. Na fabricação do aço as escorias são geradas em duas etapas: a primeira provém do chamado refino oxidante (forno elétrico a arco ou convertedor à oxigênio) e a segunda do refino redutor em processos de metalurgia na panela (forno-panela). Este trabalho tem como objetivo principal o de apontar potencialidades de uso da escória de aciaria elétrica, com destaque para a proveniente do forno-panela (escória do refino redutor), na indústria da construção civil através de testes em que a escória é utilizada, após moagem, como adição ao cimento Portland comum. Inicialmente foram realizados ensaios de viabilização para se testar a pozolanicidade, resistência à compressão, expansibilidade e profundidade de carbonatação de concretos gerados com diversas adições de escórias de aciaria elétrica. Comprovada a sua viabilidade partiu-se para os ensaios complementares do trabalho utilizando-se somente uma escória do refino redutor. Nesta segunda etapa foram realizados ensaios de caracterização de todos materiais estudados, ensaios de expansibilidade, ensaios mecânicos e de durabilidade dos concretos gerados com esta escória e ensaios de microscopia eletrônica de varredura e de difração de raios X do material. Após o estudo realizado comprovou-se ser perfeitamente viável a utilização de até 10% da escória do refino redutor (forno-panela- FP) como adição ao cimento para produção de concretos. Inclusive, independente do tempo de estocagem da escória, pode-se constatar melhorias no concreto produzido.

Contribuição ao beneficiamento de finos de fosfatos

Foram estudadas as características de floculação da hidro-xiapatita, calcita e quartzo com poliacrilamidas aniônicas. Tanto as suspensões de hidroxiapatita como a calcita foram completamente floculadas enquanto que o quartzo foi refratário a floculação com esses polimeros. Entretanto, observou-se que a floculação da calcita foi impedida com a utilização de um poliacrilato de sódio, enquanto que a hidroxiapatita continuou a ser floculada pela poliacrilamida num intervalo de concentração de O a 1000 g/ton de poliacrilato. Estes resultados permitiram estabelecer condições para a floculação seletiva de hidroxiapatita em misturas sintéticas com quartzo e calcita. Nestes sistemas foram estudados diversos parâmetros operacionais, tais como tipo de separação, efeito do teor da alimentação, e influência da moagem. Onde a separação estagiada apresentou melhor resultado, uma moagem adicional no sistema não favoreceu a seletividade. Por outro lado, o teor de P205 no concentrado é proporcional ao teor presente na alimentação. A hidroxiapatita, em estudo, de alta pureza (de acordo com técnicas de análise química, espectrofotometria de infravermelho e difração de raios X) apresentou um parto de carga zero em pH 6,77 na presença de diversos eletrólitos. A aplicação do sistema de floculação seletiva a fraçoes ultrafinas industriais foi estudada em detalhe e comparada com processos de flotação e floco-flatação. 0s resultados obtidos mostraram que a floculação seletiva somente foi eficiente nos sistemas sintéticos. A flotação, embora o minério apresente uma granulometria muito fina, foi mais eficiente que a floculação seletiva e a floco-flotação nos sistemas reais, em termos de taxa de enriquecimento e percentual de rejeição de massa. Entretanto com a floco-flotação foi possivel obter altas recuperações(-90%) para os minérios de Araxá e Itataia. Para o minério de Tapira, um aumento do teor de P2O5 foi obtido com a flotação da fração seletivamente floculada. As taxas de enriquecimento obtidas foram baixas (entre 1,35 e 2,101 em função das associações entre a apatita do minério com óxido de ferro e argila, o que revelou a caracterização mineralógica. Conclue-se que a concentração de minerios fosfatados de baixo teor é uma operação onerosa, onde o fator predominante é a absorção seletiva de reagentes e atransferência não específica de material de ganga nos respectivos concentrados.

Caracterização de compósitos Nb-20%cu obtidos por moagem de alta energia e sinterizados por fase líquida

In this work, was studied the formation of a composite of the refractory metal niobium with copper, through the process of high-energy milling and liquid phase sintering. The HEM can be used to synthesize composite powders with high homogeneity and fine size particle distribution. It may also produce the solid solubility in immiscible systems such as Nb-Cu, or extend the solubility of systems with limited solubility. Therefore, in the immiscible system Cu-Nb, the high-energy milling was successfully used to obtain the composite powder particles. Initially, the formation of composite particles during the HEM and the effect of preparation technique on the microstructure of the material was evaluated. Four loads of Nb and Cu powders containing 20%wt Cu were synthesized by MAE in a planetary type ball mill under different periods of grinding. The influence of grinding time on the metal particles is evaluated during the process by the withdrawal of samples at intermediate times of milling. After compaction under different forces, the samples were sintered in a vacuum furnace. The liquid phase sintering of these samples prepared by HEM produced a homogeneous and fine grained. The composite particles forming the sintered samples are the addition of a hard phase (Nb) with a high melting point, and a ductile phase (Cu) with low melting point and high thermal and electrical conductivities. Based on these properties, the Nb-Cu system is a potential material for many applications, such as electrical contacts, welding electrodes, coils for generating high magnetic fields, heat sinks and microwave absorbers, which are coupled to electronic devices. The characterization techniques used in this study, were laser granulometry, used to evaluate the homogeneity and particle size, and the X-ray diffraction, in the phase identification and to analyze the crystalline structure of the powders during milling. The morphology and dispersion of the phases in the composite powder particles, as well the microstructures of the sintered samples, were observed by scanning electron microscopy (SEM). Subsequently, the sintered samples are evaluated for density and densification. And finally, they were characterized by techniques of measuring the electrical conductivity and microhardness, whose properties are analyzed as a function of the parameters for obtaining the composite

Estudo sobre o efeito dos parâmetros de processamento dos pós e sinterização do aço inox 316l reforçado com NbC

This masther dissertation presents a contribution to the study of 316L stainless steel sintering aiming to study their behavior in the milling process and the effect of isotherm temperature on the microstructure and mechanical properties. The 316L stainless steel is a widely used alloy for their high corrosion resistance property. However its application is limited by the low wear resistance consequence of its low hardness. In previous work we analyzed the effect of sintering additives as NbC and TaC. This study aims at deepening the understanding of sintering, analyzing the effect of grinding on particle size and microstructure and the effect of heating rate and soaking time on the sintered microstructure and on their microhardness. Were milled 316L powders with NbC at 1, 5 and 24 hours respectively. Particulates were characterized by SEM and . Cylindrical samples height and diameter of 5.0 mm were compacted at 700 MPa. The sintering conditions were: heating rate 5, 10 and 15◦C/min, temperature 1000, 1100, 1200, 1290 and 1300◦C, and soaking times of 30 and 60min. The cooling rate was maintained at 25◦C/min. All samples were sintered in a vacuum furnace. The sintered microstructure were characterized by optical and electron microscopy as well as density and microhardness. It was observed that the milling process has an influence on sintering, as well as temperature. The major effect was caused by firing temperature, followed by the grinding and heating rate. In this case, the highest rates correspond to higher sintering.

Desenvolvimento e caracterização de um compósito matriz metálica (CMM): aço EUROFER97 reforçado com Carbeto de Tântalo - TaC

Steel is an alloy EUROFER promising for use in nuclear reactors, or in applications where the material is subjected to temperatures up to 550 ° C due to their lower creep resistance under. One way to increase this property, so that the steel work at higher temperatures it is necessary to prevent sliding of its grain boundaries. Factors that influence this slip contours are the morphology of the grains, the angle and speed of the grain boundaries. This speed can be decreased in the presence of a dispersed phase in the material, provided it is fine and homogeneously distributed. In this context, this paper presents the development of a new material metal matrix composite (MMC) which has as starting materials as stainless steel EUROFER 97, and two different kinds of tantalum carbide - TaC, one with average crystallite sizes 13.78 nm synthesized in UFRN and another with 40.66 nm supplied by Aldrich. In order to improve the mechanical properties of metal matrix was added by powder metallurgy, nano-sized particles of the two types of TaC. This paper discusses the effect of dispersion of carbides in the microstructure of sintered parts. Pure steel powders with the addition of 3% TaC UFRN and 3% TaC commercial respectively, were ground in grinding times following: a) 5 hours in the planetary mill for all post b) 8 hours of grinding in the mill Planetary only for steel TaC powders of commercial and c) 24 hours in the conventional ball mill mixing the pure steel milled for 5 hours in the planetary mill with 3% TaC commercial. Each of the resulting particulate samples were cold compacted under a uniaxial pressure of 600MPa, on a cylindrical matrix of 5 mm diameter. Subsequently, the compressed were sintered in a vacuum furnace at temperatures of 1150 to 1250 ° C with an increment of 20 ° C and 10 ° C per minute and maintained at these isotherms for 30, 60 and 120 minutes and cooled to room temperature. The distribution, size and dispersion of steel and composite particles were determined by x-ray diffraction, scanning electron microscopy followed by chemical analysis (EDS). The structures of the sintered bodies were observed by optical microscopy and scanning electron accompanied by EDS beyond the x-ray diffraction. Initial studies sintering the obtained steel EUROFER 97 a positive reply in relation to improvement of the mechanical properties independent of the processing, because it is obtained with sintered microhardness values close to and even greater than 100% of the value obtained for the HV 333.2 pure steel as received in the form of a bar

Formulação de massas cerâmicas para porcelanas elétricas utilizando resíduos oriundos de corpos de fusíveis

The power industry generates as waste ceramic bodies of electrical fuses that are discarded after use. The formulation of ceramic bodies for porcelain electrical insulators using waste from the bodies fuse allocation promotes environmentally appropriate, through the reuse of the material. This work evaluated the technical feasibility of using waste for use in electrical porcelains with formulations containing the residue, feldspar and kaolinite. The raw materials were processed through grinding and sieving to 200 mesh. The ceramic material obtained from the proposed formulations with 25%, 30%, 34% and 40% of the residue went through a vibratory mill for grinding and homogenization, and then were sieved at 325 mesh. The samples were shaped in a uniaxial press, with the application of 25 MPa and sintered at 1100° C, 1150°C, 1200°C, 1225°C and 1250°C, at levels of 20 and 45 minutes. Were also developed bodies of evidence with reference formulations obtained without residue, to establish a comparison on physical, mechanical and electrical. The tests were conducted and technology: linear shrinkage, porosity, water absorption, resistance to bending to three points, measuring insulation resistance electrical resistivity of the material, X-ray diffraction and X-ray fluorescence Waste characterizations pointed to the existence of two phases: mullite and quartz phases are of great importance in the microstructure of the ceramic and this fact reveals a possibility for reuse in electrical porcelains. The mullite is an important constituent because it is a phase that makes it possible to increase the mechanical strength in addition to the body allows the use at high temperatures. The use of ceramic bodies residue fuses, proved feasible for application in electrical porcelain and the most significant results were obtained by the formulations with 25% waste and sintering at 1200°C

Efeito da adição de microfibras de lã de vidro na tenacidade à ruptura de pastas de cimento para poços de petróleo

Although there are a wide variety of additives that act in fresh state, to adjust the properties of cement, there is also a search by additions that improve the tenacity of the cement in the hardened state. This, in turn, can often be increased by inserting fibers, which act on the deflection of microcracks. This study aimed to use a microfiber glass wool (silica-based) as an additive reinforcing the cement matrix, improving the rupture tenacity, in order to prevent the propagation of microcracks in the cement sheath commonly found in oil wells submitted to high temperatures. The fibers were added at different concentrations, 2 to 5% (BWOC) and varied average sizes, grinding for 90 s, 180 s, 300 s, 600 s. The cement slurries were made with a density of 1,90 g/ cm3 (15,6 lb/gal), using Portland cement CPP- Special Class as the hydraulic binder and 40% silica flour. The characterization of the fiber was made by scanning electron microscopy (SEM), particle size by sieving, X-ray fluorescence (XRF), X-ray diffraction (XRD) and thermogravimetry (TG / DTG). Were performed technological tests set by the API (American Petroleum Institute) by rheology, stability, free water, compressive strength, as well as testing rupture energy, elastic modulus and permeability. The characterization results showed good thermal stability of the microfiber glass wool for application in oil wells submitted to steam injection and, also, that from the particle size data, it was possible to suggest that microfibers milled up to 300 s, are ideal to act as reinforcement to the cement slurries. The rheological parameters, there was committal of plastic viscosity when larger lengths were inserted of microfiber (F90). The values obtained by free water and stability were presented according to API. The mechanical properties, the incorporation of microfiber to the cement slurries gave better rupture tenacity, as compared to reference cement slurries. The values of compressive strength, elastic modulus and permeability have been maintained with respect to the reference cement slurries. Thus, cement slurries reinforced with microfiber glass wool can ensure good application for cementing oil wells submitted to steam injection, which requires control of microcracks, due to the thermal gradients

Influência da adição de cinza do bagaço de cana calcinada em sistemas de pastas para cimentação de poços petrolíferos

Cementing operation is one of the most important stages in the oil well drilling processes and has main function to form hydraulic seal between the various permeable zones traversed by the well. However, several problems may occur with the cement sheath, either during primary cementing or during the well production period. Cements low resistance can cause fissures in the cement sheath and compromise the mechanical integrity of the annular, resulting in contamination of groundwater and producing zones. Several researches show that biomass ash, in particular, those generated by the sugarcane industry have pozzolanic activity and can be added in the composition of the cementing slurries in diverse applications, providing improvements in mechanical properties, revenue and cement durability. Due to the importance of a low cost additive that increases the mechanical properties in a well cementing operations, this study aimed to potentiate the use of sugarcane bagasse ash as pozzolanic material, evaluate the mechanisms of action of this one on cement pastes properties and apply this material in systems slurries aimed to cementing a well with 800 m depth and geothermal gradient of 1.7 °F/100 ft, as much primary cementing operations as squeeze. To do this, the ash beneficiation methods were realized through the processes of grinding, sifting and reburning (calcination) and then characterization by X-ray fluorescence, XRD, TG / DTG, specific surface area, particle size distribution by laser diffraction and mass specific. Moreover, the ash pozzolanic activity added to the cement at concentrations of 0%, 20% and 40% BWOC was evaluated by pozzolanic activity index with lime and with Portland cement. The evaluation of the pozzolanic activity by XRD, TG / DTG and compressive strength confirmed the ash reactivity and indicated that the addition of 20% in the composition of cement slurries produces improvement 34% in the mechanical properties of the slurry cured. Cement slurries properties evaluated by rheological measurements, fluid loss, free fluid, slurry sedimentation, thickening time and sonic strength (UCA) were satisfactory and showed the viability of using the sugarcane ash in cement slurries composition for well cementing

Influência na qualidade final de metais retificados através da variação da velocidade de mergulho

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Influência da lubrirrefrigeração na qualidade superficial de metais retificados

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Additional steps in mechanical recyling of PET

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Host-guest system of 4-nerolidylcatechol in 2-hydroxypropyl-beta-cyclodextrin: preparation, characterization and molecular modeling

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Construction and demolition waste as a source of PVC for recycling

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)