Síntese, caracterização e cinética da decomposição térmica dos materiais cerâmicos PrMO3 (M = Ni ou Co)

In this work have been studied the preparation, characterization and kinetic study of decomposition of the polymerizing agent used in the synthesis under non-isothermal condition ceramics PrMO3 of general formula (M = Co and Ni). These materials were obtained starting from the respective metal nitrates, as a cations source, and making use of gelatin as polymerizing agent. The powders were calcined at temperatures of 500°C, 700°C and 900°C and characterized by X-ray Diffraction (XRD), Thermogravimetric Analysis (TG / DTG/ DTA), Infrared Spectroscopy (FTIR), Temperature Programmed Reduction (TPR) and Scanning Electron Microscopy (SEM). The perovskite phase was detected in all the X-rays patterns. In the infrared spectroscopy observed the oxide formation as the calcination temperature increases with the appearance of the band metal - oxygen. The images of SEM revealed uniform distribution for the PrCoO3 and particles agglomerated as consequence of particle size for PrNiO3. From the data of thermal analysis, the kinetics of decomposition of organic matter was employed using the kinetics methods called Model Free Kinetics and Flynn and Wall, in the heating ratios 10, 20 and 30° C.min-1 between room temperature and 700°C. Finally, been obtained the values of activation energy for the region of greatest decomposition of organic matter in samples that were determined by the degree of conversion (α)

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.

Conversão térmica e termocatalítica à baixa temperatura do óleo de girassol para obtenção de bio-óleo

The use of biofuels remotes to the eighteenth century, when Rudolf Diesel made the first trials using peanut oil as fuel in a compression ignition engine. Based on these trials, there was the need for some chemical change to vegetable oil. Among these chemical transformations, we can mention the cracking and transesterification. This work aims at conducting a study using the thermocatalytic and thermal cracking of sunflower oil, using the Al-MCM-41 catalyst. The material type mesoporous Al-MCM-41 was synthesized and characterized by Hydrothermical methods of X-ray diffraction, scanning electron microscopy, nitrogen adsorption, absorption spectroscopy in the infrared and thermal gravimetric analysis (TG / DTG).The study was conducted on the thermogravimetric behavior of sunflower oil on the mesoporous catalyst cited. Activation energy, conversion, and oil degradation as a function of temperature were estimated based on the integral curves of thermogravimetric analysis and the kinetic method of Vyazovkin. The mesoporous material Al-MCM-41 showed one-dimensional hexagonal formation. The study of the kinetic behavior of sunflower oil with the catalyst showed a lower activation energy against the activation energy of pure sunflower oil. Two liquid fractions of sunflower oil were obtained, both in thermal and thermocatalytic pyrolisis. The first fraction obtained was called bio-oil and the second fraction obtained was called acid fraction. The acid fraction collected, in thermal and thermocatalytic pyrolisis, showed very high level of acidity, which is why it was called acid fraction. The first fraction was collected bio-called because it presented results in the range similar to petroleum diesel

Avaliação térmica dos resíduos da destilação atmosférica das blendas - biodiesel/diesel

The worldwide concern regarding the use of sustainable energy and preserving the environment are determining factors in the search for resources and alternative sources of energy and therefore fuel less aggressive nature. In response to these difficulties Biodiesel has emerged as a good solution because it is produced from renewable sources, produces burns cleaner and is easily reproducible. This work was synthesized with biodiesel oil, sunflower via homogeneous catalysis in the presence of KOH, with and without the use of BHT and subsequently added to the blends BX (a proportion of biodiesel X = 5, 10, 15 and 20 %). Atmospheric distillation of the analysis, performed in blends with and without BHT were collected residue generated by each sample and performed a study heat from the thermogravimetric analysis at a heating rate of 10 °C*min-1, nitrogen atmosphere and heating to 600 °C. According to the specifications of Resolution N 7/2008 for biodiesel, it was found that the synthesized material was in accordance with the specifications. For blends showed that the samples are in accordance with the Resolution of ANP N 42/2009. From the TG / DTG curves of the samples of biodiesel, blends and waste can be seen that these show a single loss of thermal decomposition concerning constituents present in each sample. The blends without BHT with ratios of 5%, 10% and 15% biodiesel showed a lower amount of waste (1,07%; 1,09% e 1,10%) to mineral diesel (1,15%). Therefore, it is concluded that the addition of biodiesel with diesel mineral can improve some physico-chemical parameters, but also, depending on the added amount, decreasing the amount of waste generated. This fact is of great importance because the carbonaceous residue can cause problems in mechanical equipment and parts for vehicles, causing more frequent maintenance, and this is not desirable

Estudo de pré-formulação para dose fixa combinada dos tuberculostáticos rifampicina, isoniazida, pirazinamida e etambutol (4 em 1)

According to the global framework regarding new cases of tuberculosis, Brazil appears at the 18th place. Thus, the Ministry of Health has defined this disease as a priority in the governmental policies. As a consequence, studies concerning treatment and prevention have increased. Fixed-dose combination formulations (FDC) are recognized as beneficial and are recommended by WHO, but they present instability and loss on rifampicin bioavailability. The main purpose of this work was to carry out a pre-formulation study with the schedule 1 tuberculosis treatment drugs: rifampicin, isoniazid, pyrazinamide and ethambutol and pharmaceutical excipients (lactose, cellulose, magnesium stearate and talc), in order to develop an FDC product (150 mg of rifampicin + 75 mg of isoniazid + 400 mg of pyrazinamide + 250 mg of ethambutol). The studies consisted of the determination of particle size and distribution (Ferret s diameter) and shape through optical microscopy, as well as rheological and technological properties (bulk and tapped densities, Hausner Factor, Carr s Index, repose angle and flux rate) and interactions among drugs and drug excipient through thermal analysis (DSC, DTA, TG and your derivate). The results showed that, except isoniazid, the other drugs presented poor rheological properties, determined by the physical characteristics of the particles: small size and rod like particles shape for rifampicin; rectangular shape for pyrazinamide and ethambutol, beyond its low density. The 4 drug mixture also not presented flowability, particularly that one containing drug quantity indicated for the formulation of FDC products. In this mixture, isoniazid, that has the best flowability, was added in a lower concentration. The addition of microcrystalline cellulose, magnesium stearate and talc to the drug mixtures improved flowability properties. In DSC analysis probable interactions among drugs were found, supporting the hypothesis of ethambutol and pyrazinamide catalysis of the rifampicin-isoniazid reaction resulting in 3- formylrifamycin isonicotinyl hydrazone (HYD) as a degradation product. In the mixtures containing lactose Supertab® DSC curves evidenced incompatibility among drugs and excipient. In the DSC curves of mixtures containing cellulose MC101®, magnesium stearate and talc, no alterations were observed comparing to the drug profiles. The TG/DTG of the binary and ternary mixtures curves showed different thermogravimetrics profiles relating that observed to the drug isolated, with the thermal decomposition early supporting the evidences of incompatibilities showed in the DSC and DTA curves

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

Obtenção e caracterização de complexos de inclusão binários e ternários com praziquantel

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior

Desenvolvimento de um compósito de espuma rígida de poliuretana de mamona e fibras de sisal para isolação térmica

The search for sustainable technologies that can contribute to reduce energy consumption is a great challenge in the field of insulation materials. In this context, composites manufactured from vegetal sources are an alternative technology. The principal objectives of this work are the development and characterization of a composite composed by the rigid polyurethane foam derived from castor oil (commercially available as RESPAN D40) and sisal fibers. The manufacture of the composite was done with expansion controlled inside a closed mold. The sisal fibers where used in the form of needlepunched nonwoven with a mean density of 1150 g/m2 and 1350 g/m2. The composite characterization was performed through the following tests: thermal conductivity, thermal behavior, thermo gravimetric analysis (TG/DTG), mechanical strength in compression and flexural, apparent density, water absorption in percentile, and the samples morphology was analyzed in a MEV. The density and humidity percentage of the sisal fiber were also determined. The thermal conductivity of the composites was higher than the pure polyurethane foam, the addition of nonwoven sisal fibers will become in a higher level of compact foam, reducing empty spaces (cells) of polyurethane, inducing an increase in k value. The apparent density of the composites was higher than pure polyurethane foam. In the results of water absorption tests, was seen a higher absorption percent of the composites, what is related to the presence of sisal fibers which are hygroscopic. From TG/DTG results, with the addition of sisal fibers reduced the strength to thermal degradation of the composites, a higher loss of mass was observed in the temperature band between 200 and 340 °C, related to urethane bonds decomposition and cellulose degradation and its derivatives. About mechanical behavior in compression and flexural, composites presented a better mechanical behavior than the rigid polyurethane foam. An increase in the amount of sisal fibers induces a higher rigidity of the composites. At the thermal behavior tests, the composites were more mechanically and thermally resistant than some materials commonly used for thermal insulation, they present the same or better results. The density of nonwoven sisal fiber had influence over the insulation grade; this means that, an increaser in sisal fiber density helped to retain the heat

Investigação da estabilidade térmica e das propriedades elétricas do TiO2 em função da dopagem com Ce(SO4)2

The metalic oxides have been studies due to differents applications as materials semiconductor in solar cells, catalysts, full cells and, resistors. Titanium dioxide (TiO2) has a high electric conductivity due to oxygen vacancies. The Ce(SO4)2.2H2O doped samples TiO2 and TiO2 pure was obtained sol-gel process, and characterized by X-ray diffractometry,thermal analysis, and impedance spectroscopy. The X-ray diffraction patterns for TiO2 pure samples shows at 700°C anatase phase is absent, and only the diffraction peaks of rutile phase are observed. However, the cerium doped samples only at 900°C rutile in the phase present with peaks of cerium dioxide (CeO2). The thermal analysis of the TiO2 pure and small concentration cerium doped samples show two steps weight loss corresponding to water of hydration and chemisorbed. To larger concentration cerium doped samples were observed two steps weight loss in the transformation of the doped cerium possible intermediate species and SO3. Finally, two steps weight loss the end products CeO2 and SO3 are formed. Analyse electric properties at different temperatures and concentration cerium doped samples have been investigated by impedance spectroscopy. It was observed that titanium, can be substituted by cerium, changing its electric properties, and increased thermal stability of TiO2 anatase structure

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

Uso do pó da palha de carnaúba em compósitos de quitosana

In this work a biodegradable composite using the carnauba straw s powder as reinforcement on chitosan matrix polymeric were manufactured. Firstly, were carried out the chemistry characterization of the carnauba straw s powder before and after treatments with NaOH and hexane. Goering and Van Soest method (1970), flotation test, moisture absorption, FTIR, TG/DTG, DSC and SEM have also being carried out. Composites were developed with variations in granulometry and in powder concentrations. They were characterized by TG/DTG, SEM and mechanicals properties. The results of chemical composition showed that the carnauba straw s powder is composed of 41% of cellulose; 28,9% of hemicellulose and 14% of lignin.The flotation test have indicated that the chemical treatment with NaOH decreased the powder s hidrophilicity.The thermal analysis showed increased of thermal stability of material after treatments. The results of FTIR and SEM revealed the removal of soluble materials from the powder (hemicelluloses and lignin), the material became rougher and clean. The composites obtained showed that the mechanicals properties of the composites were decreased in respect at chitosan films, and the composites with the powder at 150 Mesh showed less variation in the modulus values. The speed test of 10 mm/min showed the better reproducibility of the results and is in agreement to the standard ASTM D638. The SEM analysis of fracture showed the low adhesion between the fiber/matrix. The increase of volume of powder in the composite caused a decrease in values of stress and strain for the samples with untreated powder and treated with hexane. The composite with 50% of the powder s treated in NaOH didn t have significant variation in the values of stress and strain as compared with the composites with 10% of the powder, showing that the increase in the volume of fiber didn t affect the stress and strain of the composite. Thereby, it is concluded that the manufacture of polymeric composites of chitosan using carnauba straw s powder can be done, without need for pre-treatment of reinforcement, become the couple of carnauba straw s powder-chitosan a good alternative for biodegradable composites

Complexos metálicos de cobalto, níquel e cobre com a Pirazina-2-carboxamida e 4- hidrazida ácida piridincarboxílica: síntese e caracterização

This work involved the synthesis, characterization and proposing the molecular structure of coordination compounds involving ligands pyrazine-2-carboxamide (PZA) and 4- hydrazide acidic pyridine carboxylic (INH) and metals of the first transition series (M = Co2+, Ni2+ and Cu2+). For the characterization of the compounds used were analytical techniques such as infrared absorption spectroscopy average (FT-IR) molar conductivity measurements, CHN elemental analysis, EDTA Complexometric, measurement of melting point, X-ray diffraction by powder method, Thermogravimetry (TG) and Differential Thermal Analysis (DTA) and Simultaneous Differential Scanning Calorimetry (DSC). The absorption spectra in the infrared region suggested that the ligand coordination to the metal center occurs through the carbonyl oxygen atom and nitrogen alpha pyrazine ring to those complexes formed with PZA. For INH complexes with metal-ligand coordination is through the carbonyl oxygen and nitrogen of the terminal hydrazide grouping. The conductivity measurements of the complexes in aqueous solution they suggest to all behavior of the type 1:2 electrolytes, and conduct of non-electrolytes in acetonitrile. The results obtained by CHN elemental analysis and EDTA Complexometric allowed to infer the stoichiometry of the compounds synthesized. For all of the complexes obtained was possible to record the melting points, neither of which melted near the melting temperature of the free ligands. The X-ray diffraction showed that the complexes of pyrazinamide exhibited diffraction lines, suggesting that these compounds are crystalline, while compounds of isoniazid, with the exception of cobalt, exhibited diffraction lines, indicating that they are crystalline. The results from the TG-DTA and DSC allowed information regarding the dehydration and thermal decomposition of these complexes

Trissoralen um medicamento de baixa dosagem: estudos termoanalíticos da compatibilidade do fármaco-excipientes e determinação de parâmetros de qualidade para cápsulas magistrais

The trioxsalen (Tri) is a low-dose drug used in the treatment of psoriasis and other skin diseases. The aim of the study was applying the thermal analysis and complementary techniques for characterization, evaluation of the trioxsalen stability and components of manipulated pharmaceutical formulations. The thermal behavior of the Tri by TG/DTG-DTA in dynamic atmosphere of synthetic air and nitrogen showed the same profile with a melting peak followed by a volatilization-related event. From the curves TG / DTG is observed a single stage of mass loss. By heating the drug in the stove at temperatures of 80, 240 and 260 °C, it had no change in chemical structure through the techniques of XRD, HPLC, MIR, OM and SEM. From the non-isothermal and isothermal TG kinetic studies was possible to calculate the activation energy and reaction order for the Tri. The drug showed good thermal stability. Studies on drug-excipient compatibility showed interaction of trissoralen with sodium lauryl sulfate 1:1. There was no interaction with aerosol, pregelatinized starch, sodium starch glycolate, cellulose, croscarmellose sodium, magnesium stearate, lactose and mannitol.The characterization of three trioxsalen formulations at concentrations of 2.5, 5, 7.5, 10, 12.5 and 15 mg was performed by DSC, TG / DTG, XRD, NIR and MIR. The PCA classification method based on spectral data from the NIR and MIR of trissoralen formulations allows successful differentiation into three groups. The formulation 3 was the one that best showed analytical profile with the following composition of aerosil excipients, pre-gelatinized starch and cellulose. The activation energy of the volatilization process of the drug was determined in binary mixtures and formulation 3 through fitting and isoconversional methods. The binary mixture with sodium starch glycolate and lactose showed differences in kinetic parameters compared to the drug isolated. The thermoanalytical techniques (DSC and TG / DTG) were shown to be promising methodologies for quantifying trioxsalen obtained by the linearity, selectivity, no use solvents, without sample preparation, speed and practicality.