Síntese e caracterização de argilas pilarizadas com pilares mistos Al/Co

Two pillaring methods were tested to synthesize pillared clays containing mixed Al/Co pillars. Using the first method, based on the traditional procedure, were obtained materials containing different Co concentrations: 10, 25, 50, 75 and 100 % of Co in the pillaring solution. Just the experiments with low concentrations (10 and 25 % of Co) has formed pillared clays, whereas the sample with 25 % of cobalt showed best results compared with the one obtained just using Al as pillaring agent (basal spacing higher than 18 Å and surface area bigger than 300 m²/g). The 27Al NMR results pointed out the formation of mixed Al/Co pillars due to decreased between the intensities of AlVI/AlIV signals, indicating that the AlIV content decreased while Co content increased, suggesting the isomorphic substitution of Al atoms for Co in the Keggin ion structure (pillaring agent). For the samples containing 75 and 100 % of cobalt, it was verified the formation of others materials, which could be identified as hydrotalcite like compounds. The second pillarization method was named mixed layers, because the objective was to intercalate clay layers with hydrotalcite layers. Thus, after calcination, the hydrotalcite layers would dehydroxylate, resulting just in the metals oxides, intercalated between the clay sheets, thus generating, a pillared clay. For this purpose, were tested 4 synthesis procedures: physical mixture, mixture in water, ionic exchange under reflux and in situ synthesis. Of these, the method which showed the best results was the in situ synthesis, in which basal spacings of 14 Å (after calcination) were obtained, indicating that the samples are intercalated with metal oxides (Mg and Al). This procedure was reproduced with a Co-Al LDH (layered double hydroxide) and similar results were obtained, testifying the method reproducibility

Estudo da adição de argila expandida na formulação de concretos leves

Lightweight concrete has been the subject of several studies towards the development of new building materials. Emphasis has been given on the particle size effect and nature of aggregates used as raw materials. The present study includes an analysis of the materials that make this kind of concrete, analyzes of mechanical properties such as compressive and tensile strength, in addition to assessments of the interface concrete aggregate/matrix interface, porosity and absorption profile of chloride ions in lightweight concrete based on expanded clay. The experiments were carried out by molding cylindrical samples 100 mm in diameter and 200 mm in height. The dosage experiments were performed without additives or with the addition of minerals: (T1) 1: 2.01: 1.10: 0.78 (T2) 1: 2.00: 1.32 : 0.62 - (T3) 1 :1.93 :1.54: 0.47 (cement : sand : expanded clay 0500 : expanded clay 1506).The water to cement ratio was set to 0.43. Expanded clay minerals with different average particle sizes were used, i.e., 9.5 mm/0500 and 19 mm/1506. The larger aggregate was coated by a glassy layer, yielding lower water absorption characteristics to the concrete. The results showed that the use of light expanded clay aggregates is a technically interesting solution to the production of lightweight concrete for construction applications

Desevolvimento de nanocompósitos de poli(metacrilato de metila)/argila processados por mistura no estado fundido

Poly(methyl methacrylate)/clay nanocomposites were prepared by melt mixing using a montmorillonite-rich clay (MMT). The clay in natura was treated with acrylic acid to facilitate the dispersion in the polymer matrix. A masterbatch of PMMA/clay was prepared and combined with the pure PMMA and then subjected to extrusion process using singlescrew and twin-screw extruders followed by injection. Nanocomposites were processed with clay contents of 1, 3, 5 and 8 wt.%. The effect of shear processing on the morphology of the nanocomposites was evaluated by XRD, SEM and TEM. Thermal and mechanical properties of the nanocomposites were investigated through TGA, DSC, HDT, VICAT, tensile and impact tests, to evaluate the effect of the addition of clay to the PMMA matrix. Flammability tests were also conducted to investigate the effect of the addition of clay on the flame retardation properties. SEM images of the nanocomposites indicated the presence of clay agglomerates, which resulted in the reduction of properties such as thermal stability, mechanical strength and impact resistance, and increased the rate of burning for materials processed by both extrusion routes

Efeito da adição de feldspato e/ou resíduo de caulin em formulações à base de argila ilítica

The red pottery industry in Piauí state is well developed and stands out at the national context for the technical quality of its products. The floor and wall tile industry, however, is little developed since the state has only one company that produces red clay-based ceramic tiles. This thesis aims at using the predominantly illitic basic mass of the above mentioned industry, with the addition of feldspar and/or kaolin residue in order to obtain products of higher technical quality. Kaolin residue consists basically of kaolinite, muscovite mica and quartz; the feldspar used was potassic. In this experiment, basic mass (MB) was used for experimental control and fifteen formulations codified as follows: F2, F4, F8, F16, F32, FR2, FR4, FR8, FR16, FR32, R2, R4, R8, R16 and R32. All raw materials were dry-milled, classified, formulated and then humidified to 10% water. Thereafter, test samples were produced by unixial pressing process in a rectangular steel matrix (60.0 x 20.0 x 5.0) mm3 at (25 MPa). They were fired at four temperatures: 1080°C, 1120°C, 1160°C, with a heating rate of 10°C/min during up to 10 min in an electric oven, and the last one in an industrial oven with a peak of 1140°C, aim ing to confirm the results found in laboratory and, finally, technological tests were performed: MEA, RL, AA, PA, TRF and PF. The results revealed that the residue under study can be considered a raw material with large potential in the industry of red clay-based ceramic tiles, since the results found both in laboratory and in the industry have shown that the test samples produced from the formulations with up to 4% feldspar and those produced with up to 8% feldspar and residue permitted a reduction in the water absorption rate and an increase in the mechanical resistance while those samples produced with up to 4% residue had an increase in the mechanical resistance when compared to those produced from the basic mass and that the formulation with 2% feldspar and residue presented the best technological properties, lowering the sintering temperature down to 1120°C

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

Efeito da adição de argila expandida e adições minerais na formulação de concretos estruturais leves autoadensáveis

The search for alternative materials with lower density, reduction in heat transfer and propagation of noise associated with the ease of handling and application in concrete structures, represents an enormous challenge in the formulation and knowledge of the performance of self-compacting lightweight concrete, which has technology little known nationally, and appears on the international scene as an innovative material and alternative to conventional concrete. Based on these, this study set out to study self-compacting lightweight concrete made with two distinct grades of expanded clay associated with the addition of plasticizing/superplasticizers additives and mineral additions of metakaolin and bagasse ash of sugar cane. There is also an object of study, evaluation of pozzolanic activity of mineral admixtures and their influence on the durability characteristics of concrete. The rheological, physical, mechanical and microstructural analysis in this study served as basis in the classification of concretes autoadensáveis, targeting the national technical requirements for their classification in the category autoadensável and lightweight structural. The inclusion of mineral admixtures (metakaolin and bagasse ash of sugar cane), partial replacement of cement, pozzolanic activity and demonstrated maintenance of mechanical properties through the filler effect, a reduction of up to 76% of the nitrogen gas permeability in blend with 20% bagasse ash. All concretes had rheology (cohesion and consistency) suitable for self-adensability as well as strength and density inherent structural lightweight concrete without presenting phenomena of segregation and exudation

Adsorção do corante amarelo reativo BF-4G 200% por argila esmectita

This study aimed to evaluate the potential use of smectite clays for color removal of textile effluents. The experiments were performed by testing exploratory/planning method factorial and fractional factorial where the factors and levels are predetermined. The smectite clays were used originating from gypsum hub of the region Araripe-PE, and the dye used was Reactive Yellow BF-4G 200%. The smectite clay was collected and transported to the Laboratory of Soil Physics of UFRPE, where it held its preparation through air drying, lump breaking and classification in sieve to then submit it to the adsorption process. Upon completion of 22 complete factorial design it was concluded that the values of (96, 96,5 and 95,8%) corresponding to the percentage of of removal for "in-kind", chemically and thermally activated, respectively and adsorbed amounts of (4,80, 4,61 and 4,74 mg/g) for three clays. Showed that the activation processes used did not increase the adsorption capacity of smectite clay. The kinetic data were best fitted to the Freundlich isotherm, with an exponential distribution of active sites and that shows above the Langmuir equation for adsorption of cations and anions by clays. The kinetic model that best adapted to the results was the pseudosecond order model. In the factorial design study 24-1, at concentrations up to 500 mg/L obtains high percentage of color removal (92,37, 90,92 and 93,40%) and adsorbed amount (230,94, 227,31 and 233,50 mg/g) for three clays. The kinetic data fitted well to Langmuir and Freundlich isotherms. The kinetic model that best adapted to the results was the pseudosecond order model

Avaliação do comportamento de argila ativada na presença de água destilada, soluções salinas e inibidores de hidratação catiônicos

The clay swelling is today one of the major problems during the well drilling. Nearly 50% of clays that constitute shale expand easily in the presence of water molecules. During the drilling of a geological formation containing swelling clays, when is feasible the use of water base fluids, it is necessary to apply clay inhibitors. This avoids the incorporation of the cutting to the drilling fluid which is responsible for the wall swelling and crumbling. The aim of this work was to evaluate the synergistic behavior that occurs when swelling clay inhibitors are associated to NaCl and KCl salts. Three swelling clay inhibitors samples, INIB A, INIB B and INIB C, were analyzed. Each inhibitor was characterized by the amount of chlorides and active matter content. For the water-clay interaction evaluation in the presence of various fluids, it was used the Capillary Suction Timer (CST, Fann) and Linear Swell Meter (LSM 2000, Fann). For better interpretation of results, a Design of Experiments (DOE, Umetrics MODDE 7.0 TM) through Result Surface Methodology (RSM) was employed, taking into account the type, the swelling inhibitors concentration and the contact time with the clay. The results showed different efficiencies among the inhibitors employed, and the salt-inhibitors mixtures were more efficient than those products alone. However, for field operation, other parameters should be taking into account, as operational cost, environmental requests and time of application for each product

Aplicação de argila branca comercial pura e modificada para adsorção de sulfeto de hidrogênio

In this work were synthesized matrix-based commercial white clay in its composition having large amounts of kaolinite and quartz, with a certain percentage of iron oxide for use as an adsorbent for hydrogen sulfide (H2S). To characterize the effect of initial matrix techniques were used to characterize XRD, FTIR, XRF and TG. The initial clay mineral matrix was placed in contact with 0.1 molar solutions of the salts of Co2+, Ni2+, Cr3+ and a solution 0.1 g / 100ml rhodamine B. During the synthesis process, the solutions were placed in contact with the initial matrix for a period of 48 hours in order to have ion exchange with the clay mineral. To check the amount of exchanged metals, we used the technique of X-ray Fluorescence (XRF). After synthesis was initiated the process of adsorption of H2S, where the arrays were placed in the reactor, then by passing a stream of hydrogen sulfide. The matrix along with the reactor was weighed before and after to measure the amount of gas adsorbed. Based on the gravimetric data the matrix which had the highest performance of the adsorption matrix was exchanged with Ni2+ ions, obtaining a result of 11.13 mg H2S / g matrix, then the matrix coated with rhodamine B which was reached 10.13 mg H2S / g matrix

Uso de resíduos de queima de casca de café e argila da região sul da Bahia na obtenção de isolador elétrico cerâmico

The electrical ceramic insulators industry, uses noble raw materials such as siliceous and aluminous clays of white burning, in order to provide plasticity of the mass and contribute to electrical and mechanical properties required of the product, and feldspar with the flux function In literature references the composition of the masses indicates that the clay participates in percentage between 20 and 32, and feldspar 8 to 35, these materials have significant cost. In this research was performed the total replacement of commercial clay, for white burning clay from Santa Luzia region in southern Bahia and partial replacement of feldspar by ash residue of husk conilon coffee burning, from extreme south of Bahia. The objective of replacement these raw materials is to aver its technical feasibility and call attention for the embryo pole of ceramic industry for the existing in the south and extreme south of Bahia, which has significant reserves of noble raw materials such as clay white burning, kaolin, quartz and feldspar, and generates significant volume of gray husk conilon coffee as alternate flux. Clay Santa Luzia is prima noble material whose current commercial application is the production of white roofing. The residue of coffee husk ash is discarded near of production sites and is harmful to the environment. Phase diagrams and statistic design of experiments, were used for optimization and cost savings in research. The results confirmed the expectations of obtaining electrical ceramic insulators, with white burning clay of Santa Luzia and partial replacement up to 35.4% of feldspar, by treaty residue of conilon ash coffee husk burning. The statistic design that showed best results was for formulation with percentages of: clay 26.4 to 30.4%; kaolin 14.85 to 17.1%; feldspar 12.92 to 16.96%; R2 residue 7.08 to 9.2% and Quartz 32.5 to 38.75%, relative to the total mass of the mixture. The best results indicated; 0.2 to 1.4% apparent porosity , water absorption 0.1 to 0.7%, flexural strength 35 to 45MPa , dielectric strength 35-41 kV/cm , the transverse resistivity 8x109 2.5x1010 Ω.cm and for the dielectric constant ε/ε0 7 to 10.4, specification parameters for manufacturing ceramic electrical insulators of low and medium voltage.

Tratamento de argila montmorilonítica para a produção de nanocompósitos poliméricos com retardo de propagação de chama

Compared to conventional composites, polymer matrix nanocomposites typically exhibit enhanced properties at a significantly lower filler volume fraction. Studies published in the literature indicate t hat the addition of nanosilicate s can increase the resistance to flame propagation in polymers. In this work, a treatment of montmorillonite (MMT) nano clay and the effect of its ad dition o n flame propagation characteristics of vinyl ester were studied. The resea rch was conducted in two stages. The first stage focused on the purification and activation of the MMT clay collected from a natural deposit to improve compatibility with the polymer matrix . Clay modification with sodium acetate was also studied to improve particle dispersion in the polymer. The second step was focused on the effect of the addition of the treated clay on nanocomposites ’ properties. Nanocomposites with clay con tents of 1, 2, 4 wt. % were processed. T he techniques for the characterization of the clay included X - ray fluorescence (XRF), X - r ay d iffraction (XRD), thermogravimetric a nalysis (TGA), d ifferential scanning c alorimetry (DSC) , s urface area (BET) and Fourier transform infrared spectroscopy (FTIR). For t he characterization of the nanocomposites , the techniques used were thermogravimetric a nalysis (TGA) , differential scanning c alorimetry (DSC), Fourier transform infrared spectroscopy (FTIR) , scanning electron mi croscopy (SEM), transmission electron m icroscopy (TEM), and the determination of tensile strength, modulus of elasticity and resistance to flame propagation. According to the results, the purification and activation treatment with freeze - drying used in thi s work for the montmorillonite clay was efficient to promote compatibility and dispersion in the polymer matrix as evidenced by the characterization of the nanocomposite s . It was also observed that the clay modifica tion using sodium acetate did not produce any significant effect to improve compatibilization of the clay with the polymer. The addition of the treated MMT resulted in a reduction of up to 53% in the polymer flame propagation speed and did not affect the mechanical tensile strength and modulus o f elas ticity of the polymer, indicating compatibility between the clay and polymer. The effectiveness in reducing flame propagation speed peaked for nanocomposites with 2 wt. % clay, indicating that this is the optimum clay concentration for this property. T he clay treatment used in this work enables the production of vinylester matrix nanocomposites with flame - retardancy properties .

Estudo de tensoativos na organofilização de argila bentonítica para uso em fluido de perfuração à base de óleo

Due to the great challenges encountered in drilling wells, there is a need to develop fluids with appropriated properties and able to meet all the requirements of drilling operations. The physicochemical and rheological properties must be carefully controlled so that a fluid can exercise all its functions. In perforations sensitive to contact with water and "offshore", it becomes necessary the use of oil based drilling fluids, but the bentonite clay cannot be used without a previous surface modification so that their surfaces become hydrophobic. Lately, the oil companies in Brazil use imported organoclays in the preparation of oil-based drilling fluids. The study aimed to modify a calcium clay to increase the affinity of the same organic phase of oil-based drilling fluids, applying three surfactants (OCS, CTAB and UTM 150) at different concentrations. The results indicated that the surfactants UTM 150 and CTAB showed better results compared to OCS. Considering the type of surfactant and concentration as variables used in the statistical analysis, the results indicated that only the surface tension and concentration of calcium oxide in response to organophilization process showed statistically significant effects. The organophilizated clay has potential for application in oil-based drilling fluids.

Estudo da adição de argila expandida na formulação de concretos leves

Lightweight concrete has been the subject of several studies towards the development of new building materials. Emphasis has been given on the particle size effect and nature of aggregates used as raw materials. The present study includes an analysis of the materials that make this kind of concrete, analyzes of mechanical properties such as compressive and tensile strength, in addition to assessments of the interface concrete aggregate/matrix interface, porosity and absorption profile of chloride ions in lightweight concrete based on expanded clay. The experiments were carried out by molding cylindrical samples 100 mm in diameter and 200 mm in height. The dosage experiments were performed without additives or with the addition of minerals: (T1) 1: 2.01: 1.10: 0.78 (T2) 1: 2.00: 1.32 : 0.62 - (T3) 1 :1.93 :1.54: 0.47 (cement : sand : expanded clay 0500 : expanded clay 1506).The water to cement ratio was set to 0.43. Expanded clay minerals with different average particle sizes were used, i.e., 9.5 mm/0500 and 19 mm/1506. The larger aggregate was coated by a glassy layer, yielding lower water absorption characteristics to the concrete. The results showed that the use of light expanded clay aggregates is a technically interesting solution to the production of lightweight concrete for construction applications

Desevolvimento de nanocompósitos de poli(metacrilato de metila)/argila processados por mistura no estado fundido

Poly(methyl methacrylate)/clay nanocomposites were prepared by melt mixing using a montmorillonite-rich clay (MMT). The clay in natura was treated with acrylic acid to facilitate the dispersion in the polymer matrix. A masterbatch of PMMA/clay was prepared and combined with the pure PMMA and then subjected to extrusion process using singlescrew and twin-screw extruders followed by injection. Nanocomposites were processed with clay contents of 1, 3, 5 and 8 wt.%. The effect of shear processing on the morphology of the nanocomposites was evaluated by XRD, SEM and TEM. Thermal and mechanical properties of the nanocomposites were investigated through TGA, DSC, HDT, VICAT, tensile and impact tests, to evaluate the effect of the addition of clay to the PMMA matrix. Flammability tests were also conducted to investigate the effect of the addition of clay on the flame retardation properties. SEM images of the nanocomposites indicated the presence of clay agglomerates, which resulted in the reduction of properties such as thermal stability, mechanical strength and impact resistance, and increased the rate of burning for materials processed by both extrusion routes

Efeito da adição de feldspato e/ou resíduo de caulin em formulações à base de argila ilítica

The red pottery industry in Piauí state is well developed and stands out at the national context for the technical quality of its products. The floor and wall tile industry, however, is little developed since the state has only one company that produces red clay-based ceramic tiles. This thesis aims at using the predominantly illitic basic mass of the above mentioned industry, with the addition of feldspar and/or kaolin residue in order to obtain products of higher technical quality. Kaolin residue consists basically of kaolinite, muscovite mica and quartz; the feldspar used was potassic. In this experiment, basic mass (MB) was used for experimental control and fifteen formulations codified as follows: F2, F4, F8, F16, F32, FR2, FR4, FR8, FR16, FR32, R2, R4, R8, R16 and R32. All raw materials were dry-milled, classified, formulated and then humidified to 10% water. Thereafter, test samples were produced by unixial pressing process in a rectangular steel matrix (60.0 x 20.0 x 5.0) mm3 at (25 MPa). They were fired at four temperatures: 1080°C, 1120°C, 1160°C, with a heating rate of 10°C/min during up to 10 min in an electric oven, and the last one in an industrial oven with a peak of 1140°C, aim ing to confirm the results found in laboratory and, finally, technological tests were performed: MEA, RL, AA, PA, TRF and PF. The results revealed that the residue under study can be considered a raw material with large potential in the industry of red clay-based ceramic tiles, since the results found both in laboratory and in the industry have shown that the test samples produced from the formulations with up to 4% feldspar and those produced with up to 8% feldspar and residue permitted a reduction in the water absorption rate and an increase in the mechanical resistance while those samples produced with up to 4% residue had an increase in the mechanical resistance when compared to those produced from the basic mass and that the formulation with 2% feldspar and residue presented the best technological properties, lowering the sintering temperature down to 1120°C