Síntese e impregnação de peneiras moleculares Fe MCM-41 derivada de sílica da casca do arroz

The mesoporous molecular sieves of the MCM-41 and FeMCM-41 type are considered promissory as support for metals used as catalysts in oil-based materials refine processes and as adsorbents for environmental protection proposes. In this work MCM-41 and FeMCM41 were synthesized using rice husk ash - RHA as alternative to the conventional silica source. Hydrothermal synthesis was the method chosen to prepare the materials. Pre-defined synthesis parameters were 100°C for 168 hours, later the precursor was calcinated at 550°C for 2 hours under nitrogen and air flow. The sieves containing different proportions of iron were produced by two routes: introduction of iron salt direct synthesis; and a modification post synthesis consisting in iron salt 1 % and 5% impregnation in the material followed by thermal decomposition. The molecular sieves were characterized by X ray diffraction XRD, Fourier transform infrared spectroscopy FT-IR, X ray fluorescence spectroscopy XFR, scanning electronic microscopy SEM, specific surface area using the BET method, Termogravimetry TG. The kinetic model of Flynn Wall was used with the aim of determining the apparent activation energy of the surfactant remove (CTMABr) in the MCM- 41 porous. The analysis made possible the morphology characterization, identifying the presence of hexagonal structure typical for mesoporous materials, as well as observation of the MCM41 and iron of characteristic bands.

Controle feedback de nível baseado em sensor de imagem aplicado ao equipamento misturador-decantador à inversão de fases (MDIF®)

The treatment of wastewaters contaminated with oil is of great practical interest and it is fundamental in environmental issues. A relevant process, which has been studied on continuous treatment of contaminated water with oil, is the equipment denominated MDIF® (a mixer-settler based on phase inversion). An important variable during the operation of MDIF® is the water-solvent interface level in the separation section. The control of this level is essential both to avoid the dragging of the solvent during the water removal and improve the extraction efficiency of the oil by the solvent. The measurement of oil-water interface level (in line) is still a hard task. There are few sensors able to measure oil-water interface level in a reliable way. In the case of lab scale systems, there are no interface sensors with compatible dimensions. The objective of this work was to implement a level control system to the organic solvent/water interface level on the equipment MDIF®. The detection of the interface level is based on the acquisition and treatment of images obtained dynamically through a standard camera (webcam). The control strategy was developed to operate in feedback mode, where the level measure obtained by image detection is compared to the desired level and an action is taken on a control valve according to an implemented PID law. A control and data acquisition program was developed in Fortran to accomplish the following tasks: image acquisition; water-solvent interface identification; to perform decisions and send control signals; and to record data in files. Some experimental runs in open-loop were carried out using the MDIF® and random pulse disturbances were applied on the input variable (water outlet flow). The responses of interface level permitted the process identification by transfer models. From these models, the parameters for a PID controller were tuned by direct synthesis and tests in closed-loop were performed. Preliminary results for the feedback loop demonstrated that the sensor and the control strategy developed in this work were suitable for the control of organic solvent-water interface level

Automação de um sistema rotatório para secagem do rejeito de maracujá

The rotary dryer is one of the most used equipments in processing industries. Its automatic control mode of operation is important specially to keep the moisture content of the final product in the desired value. The classical control strategies, like PID (proportional integral derivative) control, are largely used in the industrial sector because of its robustness and because they are easy to be implemented. In this work, a data acquisition system was implemented for monitoring the most relevant process variables, like: both inlet and outlet drying air temperature, dryer rotation, outlet air speed and humidity, and mass of the final product. Openloop tests were realized to identify a mathematical model able to represent the drying process for the rotary system. From this model, a PID controller was tuned using a direct synthesis method, assuming a first order trajectory. The PID controller was implemented in the system in order to control the inlet drying air temperature. By the end, closedloop tests (operating in automatic mode) were realized to observe the controller performance, and, after setting the best tune, experiments were realized using passion fruit seeds as raw material. The experiments realized in closedloop showed a satisfactory performance by the implemented control strategy for the drying air temperature of the rotary system

Síntese e caracterização de niobiosilicatos para produção de biocombustível

The mesoporous materials has been an special attention, among them was discovered in the 1990´s the mesoporous molecular sieve of SBA-15 type. The good features of the SBA- 15 makes this material very promising in catalysis, however, due to the absence of native active sites, it has low catalytic activity. In this way, different metals and oxides have been included in this molecular sieve as a means of introducing active sites and increase its catalytic activity. Among the oxides that are being researched, there is the niobium oxide, which presents strong acid sites and exists in abundance. Brazil is the largest producer of the mineral. On the other hand, the production of biofuels has been desired, but it requires the development of new catalysts for this purpose. The aim of this work was to develop silicate of niobium by impregnation and by new synthesis method for application in the cracking of moringa oil. The methodology consisted of inserting the niobium oxide either by postsynthesis process using wet impregnation and direct insertion. For direct insert a new method was developed for pH adjustment, being tested different pH, and the pH 2.2 was used different ratios of Si/Nb. The materials were characterized by different techniques such as: XRD, N2 adsorption, SEM, EDS, UV-visible, TG/DTG, DSC, TEM, acidity by thermodesorption of n-butilamine and FTIR. After this part of the catalysts developed by the two methods were tested in the thermocatalytic cracking of moringa oil, being used a simple distillation. All silicates of Niobium obtained showed a highly ordered structure, having high specific areas, good distribution of pore diameters, beyond present a morphology in the form of fibers. In the catalysts after synthesis was observed that the niobium inserted has so as octahedrally and tetrahedrally coordinated, demonstrating that there were also oxides formed on the external surface of SBA-15. The materials obtained in the direct synthesis are only tetrahedrally coordinated. The new synthesis method of pH adjusting by using the buffer solution for it, proved to be very efficient for the production of such materials, because the materials obtained showed characteristics and structures similar to the molecular sieve of SBA-15 type. Among the pH tested the material that presented better characteristics was synthesized at pH 2.2. The application of these materials in catalytic cracking showed a higher formation of organic liquids when compared to thermal cracking, in addition to significantly reducing the acidity and residues formed, demonstrating that the use of silicates of Niobium increases both the conversion and the selectivity of the products.

Síntese e impregnação de peneiras moleculares Fe MCM-41 derivada de sílica da casca do arroz

The mesoporous molecular sieves of the MCM-41 and FeMCM-41 type are considered promissory as support for metals used as catalysts in oil-based materials refine processes and as adsorbents for environmental protection proposes. In this work MCM-41 and FeMCM41 were synthesized using rice husk ash - RHA as alternative to the conventional silica source. Hydrothermal synthesis was the method chosen to prepare the materials. Pre-defined synthesis parameters were 100°C for 168 hours, later the precursor was calcinated at 550°C for 2 hours under nitrogen and air flow. The sieves containing different proportions of iron were produced by two routes: introduction of iron salt direct synthesis; and a modification post synthesis consisting in iron salt 1 % and 5% impregnation in the material followed by thermal decomposition. The molecular sieves were characterized by X ray diffraction XRD, Fourier transform infrared spectroscopy FT-IR, X ray fluorescence spectroscopy XFR, scanning electronic microscopy SEM, specific surface area using the BET method, Termogravimetry TG. The kinetic model of Flynn Wall was used with the aim of determining the apparent activation energy of the surfactant remove (CTMABr) in the MCM- 41 porous. The analysis made possible the morphology characterization, identifying the presence of hexagonal structure typical for mesoporous materials, as well as observation of the MCM41 and iron of characteristic bands.