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

Análise do efeito do tempo da moagem de alta energia no tamanho de cristalito e microdeformação da rede cristalina do WC-Co

Hard metals are the composite developed in 1923 by Karl Schröter, with wide application because high hardness, wear resistance and toughness. It is compound by a brittle phase WC and a ductile phase Co. Mechanical properties of hardmetals are strongly dependent on the microstructure of the WC Co, and additionally affected by the microstructure of WC powders before sintering. An important feature is that the toughness and the hardness increase simultaneously with the refining of WC. Therefore, development of nanostructured WC Co hardmetal has been extensively studied. There are many methods to manufacture WC-Co hard metals, including spraying conversion process, co-precipitation, displacement reaction process, mechanochemical synthesis and high energy ball milling. High energy ball milling is a simple and efficient way of manufacturing the fine powder with nanostructure. In this process, the continuous impacts on the powders promote pronounced changes and the brittle phase is refined until nanometric scale, bring into ductile matrix, and this ductile phase is deformed, re-welded and hardened. The goal of this work was investigate the effects of highenergy milling time in the micro structural changes in the WC-Co particulate composite, particularly in the refinement of the crystallite size and lattice strain. The starting powders were WC (average particle size D50 0.87 μm) supplied by Wolfram, Berglau-u. Hutten - GMBH and Co (average particle size D50 0.93 μm) supplied by H.C.Starck. Mixing 90% WC and 10% Co in planetary ball milling at 2, 10, 20, 50, 70, 100 and 150 hours, BPR 15:1, 400 rpm. The starting powders and the milled particulate composite samples were characterized by X-ray Diffraction (XRD) and Scanning Electron Microscopy (SEM) to identify phases and morphology. The crystallite size and lattice strain were measured by Rietveld s method. This procedure allowed obtaining more precise information about the influence of each one in the microstructure. The results show that high energy milling is efficient manufacturing process of WC-Co composite, and the milling time have great influence in the microstructure of the final particles, crushing and dispersing the finely WC nanometric order in the Co particles

Obtenção de placas cerâmico a partir de formulações de massas triaxiais de resíduos de caulim, chamote de telha e cinza vegetal

The production of red ceramic is an industrial activity that causes an intense impact. The manufacture of its products considerably increases the demand for natural resources, mainly with the extraction of raw material. The ceramic material produced generates waste, such as ash firewood and chamote. The residue from the beneficiation of kaolin is deposited in a poor, degrades the environment and contaminate water sources and soil, constituting in this manner, ecological disasters. The main objective of this work is to develop the formulation of a ceramic product consisting solely of industrial solid wastes, from ceramic tiles, (chamote) residue of kaolin and ash firewood. It is assumed that this product made in the laboratory can be used in coatings, wall and floor. The aim is to facilitate the replacement of the raw material of original composition of a ceramic body, for waste, while the process of production equal to the conventionally used, so that the properties of the product are reproduced. This work is characterized waste as its chemical composition, analysis of particle size, X-ray diffraction and thermal behavior. Several formulations were studied. The mass of waste was prepared by dry process, pressed to 25 MPa, and then burned in muffle type oven to 850, 950, 1050 and 1150 °C. The results showed that it is technically possible to produce porous tiles only with waste. It was found that the formulations of bodies play a key role in the properties of the final product, as well as the sintering temperature and heating rates. RN in the waste of kaolin is estimated at 15,000 t/month, about 3,000 gray t/month and chamote with 10 million pieces/month damaged. The presence of carbonates of calcium and magnesium at 1050 ° C results in an appropriate porosity and mechanical strength. The formulation M3JE, composed of 69% waste of kaolin, 7.7% and 23.3% of chamote of gray, became suitable for porous materials with the strength and absorption within the level of national and international standards

Estudo da formulação de massas cerâmicas provenientes da região do Seridó-RN para fabricação de telhas

This work has for objective study compared the characteristics and technological properties of ceramic bodies from the region of Seridó-RN. The region under study has identified 23 cities where they were 80 ceramics industries. To define the universe of search, there was a survey of pottery that are part of APL Seridó next to the IEL. The characteristics and operating conditions of ceramics industries of the region were identified through a socio-economic questionnaire applied locally, which addressed issues such as: profiles of companies, production process etc. The analysis of information collected from 24 companies identified in seven cities shows that the vast majority of industries is small, with family structure, obsolete equipment and labo, little qualified. Most of the pottery works with low technical knowledge, poor control of the production process and product technology. The raw collected were submitted to analysis of X ray diffraction, chemical composition, termical analysis, particle size distribution and plasticity. Then were produced five formulations and made by uniaxial pressure at 25 MPa for firing in temperatures varying from 850 to 1050 °C. The firing technological properties evaluated were: mass loss to fire, lineal shrinkage, apparent density, apparent porosity, water absorption and flexural strength (3 points). The results indicated that the raw materials from the region have significant similarities in the composition chemical and mineralogical. Furthermore, it indicates the possibility of the use of cycles of firing faster and efficient than the current, limited to some clay mass burning of certain conditions

Estudo e caracterização de matérias-primas para o desenvolvimento de blocos sílico-calcários

The types of products manufactured calcium silicate blocks are very diversified in its characteristics. They include accessory bricks, blocks, products in dense material, with or without reinforcements of hardware, great units in cellular material, and thermal insulating products. The elements calcium silicate are of great use in the prefabricated construction, being formed for dense masses and hardened by autoclaving. This work has for objective develop formulations that make possible the obtaining of calcium silicate blocks with characteristics that correspond the specifications technical, in the State of the Rio Grande of the North, in finality of obtaining technical viability for use in the civil construction. The work studied the availability raw materials from convenient for the production of calcium silicate blocks, and the effect of variations of the productive process on the developed products. The studied raw materials were: the quartz sand from the city of São Gonçalo do Amarante/RN, and two lime, a hydrated lime and a pure lime from the city of Governador Dix-Sept Rosado/RN. The raw materials collected were submitted a testes to particle size distribution, fluorescence of X rays, diffraction of X rays. Then were produced 8 formulations and made body-of-test by uniaxial pressing at 36 MPa, and cured for 7 hours at about 18 kgf/cm2 pressing and temperature of approximately 180 °C. The cure technological properties evaluated were: lineal shrinkage, apparent density, apparent porosity, water absorption, modulus of rupture flexural (3 points), resistance compression, phase analysis (XRD) and micromorphological analysis (SEM). From the results presented the technological properties, was possible say that utilization of hydrated lime becomes more viable its utilization in mass limestone silica, for manufacture of calcium silicate blocks

Estudo de formulação de massa para aplicação em placas cerâmicas

The sector of civil construction is strongly related to the red ceramic industry. This sector uses clay as raw material for manufacturing of various products such as ceramic plates. In this study, two types of clay called clay 1 and clay 2 were collected on deposit in Ielmo Marinho city (RN) and then characterized by thermogravimetric analysis (TG/DTG), differential thermal analysis (DTA), X-ray diffraction (XRD), X-ray fluorescence (XRF), rational analysis and particle size distribution and dilatometric analyses. Ceramic plates were manufactured by uniaxial pressing and by extrusion. The plates obtained by pressing were produced from the four formulations called 1, 2, 3 and 4, which presented, respectively, the following proportions by mass: 66.5% clay 1 and 33.5% clay 2, 50% clay 1 and 50% clay 2, 33.5% clay 1 and 66.5% clay 2, 25% clay 1 and 75% clay 2. After firing at 850, 950 and 1050 °C with heating rate of 10 °C/min and soaking time of 30 minutes, the following technological properties were determined: linear firing shrinkage, water absorption, apparent porosity, apparent specific mass and tensile strength (3 points). The formulation containing 25% clay 1 produced plates with most satisfactory results of water absorption and mechanical resistance, because of that it was chosen for manufacturing plates by extrusion. A single firing cycle was established for these plates, which took place as follow: heating rate of 2 °C/min up to 600 ºC with soaking time of 60 minutes, followed by heating using the same rate up to 1050 ºC with soaking time of 30 minutes. After this cycle, the same technological properties investigated in the plates obtained by pressing were determined. The results indicate (according to NRB 13818/1997) that the plates obtained by pressing from the mixture containing 25 wt% clay 1, after firing at 1050 °C, reach the specifications for semi-porous coating (BIIb). On the other hand, the plates obtained by extrusion were classified as semi-stoneware (group AIIa)

Síntese citrato-hidrotermal e caracterização eletroquímica de LSCF para aplicação como catodo em célula a combustível de temperatura intermediária

The lanthanum strontium cobalt iron oxide (La1-xSrxCo1-yFeyO3 LSCF) is the most commonly used material for application as cathode in Solid Oxide Fuel Cells (SOFCs), mainly due to their high mixed ionic electronic conductivity between 600 and 800ºC. In this study, LSCF powders with different compositions were synthesized via a combination between citrate and hydrothermal methods. As-prepared powders were calcined from 700 to 900°C and then characterized by X-ray fluorescence, X-ray diffraction, thermal analyses, particle size analyses, nitrogen adsorption (BET) and scanning electronic microscopy. Films of composition La0,6Sr0,4Co0,2Fe0,8O3 (LSCF6428), powders calcined at 900°C, were screen-printed on gadolinium doped ceria (CGO) substrates and sintered between 1150 and 1200°C. The effects of level of sintering on the microstructure and electrochemical performance of electrodes were evaluated by scanning electronic microscopy and impedance spectroscopy. Area specific resistance (ASR) exhibited strong relation with the microstructure of the electrodes. The best electrochemical performance (0.18 ohm.cm2 at 800°C) was obtained for the cathode sintered at 1200°C for 2 h. The electrochemical activity can be further improved through surface activation by impregnation with PrOx, in this case the electrode area specific resistance decreases to values as low as 0.12 ohm.cm2 (800°C), 0.17 ohm.cm2 (750°C) and 0.31 ohm.cm2 (700°C). The results indicate that the citrate-hydrothermal method is suitable for the attainment of LSCF particulates with potential application as cathode component in intermediate temperature solid oxide fuel cells (IT-SOFCs)

Estudo da viabilidade técnica do uso das argilas da região do agreste potiguar para produção de peças cerâmicas: caracterização e formulação

In recent decades, ceramic products have become indispensable to the technological development of humanity, occupying important positions in scientific production and consequently in industrial production. One area of the economy that continues to absorb large amounts of the products of this sector is Construction. Among the branches of the ceramic industry, there are the red ceramic industry which is traditionally the basis of that economic sector. Among the reasons for which the red ceramic industry became popular in the country, and specifically in Rio Grande do Norte, is the abundance of this raw material, easily found throughout the national territory. However, it appears that the red ceramic industry has deficiencies in technology and skilled labor, resulting in the production of ceramic goods with low added value. Among the factors that determine the quality of the ceramic products red has the proper formulation of the ceramic mass, the conformation and the firing temperature. Thus, the overall goal of this work is to study the mineralogical and technological properties, two clays from the region of the Wasteland Potiguar industrial ceramist. Therefore, the raw materials were characterized by analysis of Xray diffraction (XRD) analysis, X-ray fluorescence (XRF), particle size analysis (FA), scanning electron microscopy (SEM), optical microscopy (OM ), plasticity index (PI), thermal gravimetric analysis (TGA) and differential thermal analysis (DTA). The technological properties of the material were analyzed by water absorption tests (AA%) porosity (% PA), the linear shrinkage (RT%), apparent density (MEA), loss on ignition (PF%) and flexural strength three points (TRF)

Desenvolvimento de um secador spray para obtenção de pós finos de precursores de nióbio

This work presents a spray-dryer designed to oxalate-niobate precursors and suitable for the production of Niobium Carbide. The dryer was intended to produce powders of controlled particle size. First, the precursor is dissolved in water to produce a solution of known concentration and then it is atomized on the spray-dryer to produce the powder. This equipment consists of a 304 stainless steel chamber, 0.48 m x 1.9 m (diameter x length), with a conical shape at the lower portion, which is assembled on a vertical platform. The chamber is heated by three 4 kW electrical resistances. In this process, drying air is heated as it flows inside a serpentine surrounding the chamber, in contrary to more traditional processes in which the hot drying air is used to heat the component. The air enters the chamber at the same temperature of the chamber, thus avoiding adherence of particles on the internal surface. The low speed flow is concurrent, directed from the top to the bottom portion of the chamber. Powders are deposited on a 0.4 m diameter tray, which separates the cylindrical portion from the conical portion of the chamber. The humid air is discharged though a plug placed underneath the collecting tray. A factorial experimental planning was prepared to study the influence of five parameters (concentration, input flow, operation temperature, drying air flow and spray air flow) on the characteristics of the powders produced. Particle size distribution and shape were measured by laser granulometry and scanning electronic microscopy. Then, the powders are submitted to reaction in a CH4 / H2 atmosphere to compare the characteristics of spray-dried powders with powders synthetizided by conventional methods

Aplicação da parafina e do óleo de linhaça como hidrofobizantes da vermiculita, para remoção de derivados de óleo diesel resentes em água produzida sintética

Produced water has lately aroused interest due to their high degree of salinity, suspended oil particles, chemicals added in various manufacturing processes, heavy metals and radioactivity sometimes. Along with oil and due to its high volume production, water production is one of the pollutants of most concern in the process of oil extraction. PAHs due to their ubiquity and their characteristics carcinogenic or mutagenic and teratogenic even have attracted the attention of every scientific society. Formed from the incomplete combustion of organic matter may be natural or anthropogenic. Some materials have been researched with the goal of cleaning up environmental matrices that may be contaminated by hydrocarbons. Among these materials researched various clays have been employed, of which highlights the vermiculite. The family of phyllosilicates, vermiculite for its potential and its high hydrophobic surface area has been a tool widely used in the decontamination of water in processes of oil spills. However, when it loses its capacity expanded hydrophobic having the necessity of using a hidrofobizante to make it organophilic. Among the numerous hidrofobizantes researched and used the linseed oil was the pioneer. In this study sought to evaluate the capacity of removal of PAHs using the vermiculite hydrofobized with linseed oil and wax also, for it was made use of the 24 full factorial design as the main tool for the experiments. We also evaluated the clay grain size (-20 +48 and -48 +80 #), the percentage of hidrofobizante applied (5 and 10%) and salinity of the water produced synthesized in our laboratory (35,000 and 55,000 ppm). The molecular fluorescence spectroscopy due to its sensitivity and speed was used to verify the adsorption capacity of clay, as well as gas chromatography served as an auxiliary technique to identify and quantify the PAHs in solution. In order to characterize the vermiculite was made use of X-ray fluorescence and X-ray diffraction. The infrared and thermogravimetry were essential to note hydrophobization and the amount of coating of clay. According to the fluorescence analysis showed that the test 12 was the best result in about 98% adsorption of fluorescent compounds, however the high salinity, the smallest particle size, the highest percentage of hidrofobizante and the use of linseed oil showed greater efficiency in the removal capacity of these hydrocarbons, in accordance with the trend followed by the analysis of the major factors of the factorial design. To verify the adsorption capacity of clay using a fixed volume of water produced synthetically, used as the test base 12, at their respective levels and factors. Thus, it was observed that after adding about 1 ½ liters of water solution produced synthetically, about 300 times its volume in mass, the vermiculite was able to adsorb 80% of fluorescent species present in solution

Caracterização dos eletrocatalisadores LaMnO3, LaFeO3, LaFe0,2Mn0,8O3 E La0,5Fe0,5MnO3 preparados por autocombustão assistida por microondas para cátodos de células a combustível do tipo SOFC

Materials consisting of perovskite-type oxides (ABO3) have been developed in this work for applications in fuel cell cathodes of solid oxide type (SOFC). These ceramic materials are widely studied for this type of application because they have excellent electrical properties, conductivity and electrocatalytic. The oxides LaMnO3, LaFeO3, LaFe0.2Mn0.8O3 e La0.5Fe0.5MnO3 were synthesized by the method of microwave assisted combustion and after sintering at 800°C in order to obtain the desired phases. The powders were characterized by thermogravimetry (TG), X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron microscopy (SEM) and voltammetric analysis (cyclic voltammetry and polarization curves). The results obtained by XRF technique showed that the microwave synthesis method was effective in obtaining doping oxides with values near stoichiometric. In general, powders were obtained with particle size less than 0.5 μm, having a porous structure and uniform particle size distribution. The particles showed spherical form, irregular and crowded of varying sizes, according to the analysis of SEM. The behavior of the oxides opposite the thermal stability was monitored by thermogravimetric curves (TG), which showed low weight loss values for all samples, especially those of manganese had its structure. By means of Xray diffraction of the samples sintered at 800°C was possible to observe the formation of powders having high levels of crystallinity. Furthermore, undesirable phases such as La2O3 and MnOx were not identified in the diffractograms. These phases block the transport of oxygen ions in the electrode/electrolyte interface, affecting the electrochemical activity of the system. The voltammetric analysis of the electrocatalysts LF-800, LM-800, LF2M8-800 e L5F5M-800 revealed that these materials are excellent electrical conductors, because it increased the passage of electrical current of the working electrode significantly. Best performance for the oxygen reduction reaction was observed with iron-rich structures, considering that the materials obtained have characteristics suitable for use in fuel cell cathodes of solid oxide type

Desenvolvimento de uma rota química alternativa de síntese de SrCo0,8Fe0,2O3- e LaNi0,3Co0,7O3- para aplicação na reação de oxidação do CO

This thesis focuses on the coprecipitation synthesis method for preparation of ceramic materials with perovskite structure, their characterization and application as catalytic material in the reaction of converting CO to CO2 developing a methodological alternative route of synthesis from the middle via oxalate coprecipitation material SrCo0,8Fe0,2O3-d. In order to check the influence of this method, it was also synthesized using a combined citrate - EDTA complexing method. The material was characterized by: X-ray diffraction (XRD), Rietveld refinement method, thermogravimetry and differential thermo analysis (TG / DTA), scanning (SEM) and transmission (TEM) electron microscopy, particle size distribution and surface analysis method BET. Both methods led to post-phase synthesis, with pH as a relevant parameter. The synthesis based on the method via oxalate coprecipitation among particles led to the crystalline phase as those obtained using a combined citrate - EDTA complexing method under the same conditions of heat treatment. The nature of the reagent used via oxalate coprecipitation method produced a material with approximately 80 % lower than the average size of crystallites. Moreover, the via oxalate coprecipitation method precursors obtained in the solid state at low temperature (~ 26 oC), shorter synthesis, greater thermal stability and a higher yield of around 90-95 %, maintaining the same order of magnitude the crystallite size that the combined citrate - EDTA complexing method. For purposes of comparing the catalytic properties of the material was also synthesized by the using a combined citrate - EDTA complexing method. The evaluation of catalytic materials SrCo0,8Fe0,2O3-d LaNi0,3Co0,7O3-d was accompanied on the oxidation of CO to CO2 using a stainless steel tubular reactor in the temperature range of 75-300 oC. The conversion CO gas was evaluated in both materials on the results shaved that the firm conversion was loves for the material LaNi0,3Co0,7O3-d