Navegando por Orientadores "NEVES, Roberto de Freitas"

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Acesso aberto (Open Access)
Aproveitamento do rejeito de caulim na produção de alumina para cerâmica e sílica de baixa granulometria
(Universidade Federal do Pará, 2000-11-29) FLORES, Silvia Maria Pereira; NEVES, Roberto de Freitas; http://lattes.cnpq.br/9559386620588673
The Amazon region detains 10% of the world reserves of kaolim. Since the seventy's, two great amazonic beds of kaolim are explored, producing kaolim for paper cover. In the beneficiation process, it's generated an elevated volume of polluted industrial residue which is deposited in extensivas and onerous lagoons of sedimentation. Because of the residue is very voluminous, these lagoons become an environmental problem of great proportions, due the extensivas deforested areas used for their constructions ( Barata, 1998). In this work, are suggested altematives of economic utilization of this residue, which is constituted, mainly, by a suspension of the claymineral kaolinite, for the production of pozolane, aluminium sulphate, the synthesis of the ammonium alum and alumina for ceramics utilization. The methodology constitutes in the drying and the calcination of the residue, followed by the extraction of the AI retained by the acid lixiviation H2SO4 ) followed by the ammonium alum crystallisation, for the reaction with the concentrated NH4OH, by means of pH control, and later calcination at 1200°C, getting a-Al2O3, with no sodium and Iow granulometry. From the aluminas obtained, are made bodies of proof smashed and sintered at 1600°C, to the determination of the ceramics properties, which are compared to one of the commercial alumina. After the acid lixiviation for the AI extraction, results as an insoluble material, an amorphous silica, for which it is suggested, as an additional contribution, an economic application, using it as artificial pozolane in building portland cement, making mechanics tests for the evaluation of its performance. The material that were used and synthesized were characterized throught the use of the X ray diffraction, eletronic scanning microscopy, the infra-red spectroscopy, thermogravimetry, differential thermic analisys, particle size analysis, specific area BET, porosity, chemical analisys throught umid means and throught X ray fluorescence.
Acesso aberto (Open Access)
Beneficiamento de uma argila tipo palygorskita da Bacia de São Luis-Grajaú, região de Alcântara (MA) e sua utilização como adsorvente de fósforo.
(Universidade Federal do Pará, 2012-09-04) ARRUDA, Gabriela Monice; NEVES, Roberto de Freitas; http://lattes.cnpq.br/9559386620588673
The estimated contribution of the industry minerals in Brazil is about 70% of National Mineral Production Value. These minerals are important because of its diverse applications. Among them, in clay minerals group, there is palygorskite, which presents the requirements to join special clays group, once their occurrence is restricted. Thus, this new mineral occurrences deserve attention and further study. Adding to this, there is the fact in the Amazon region, as well as in most areas of tropical and temperate zones, the acidity is an important factor in land degradation and represent one of the major problems faced by agriculture. Acid soils have several limitations, which hinders the use of nutrients, requiring the addition of fertilizers, always aiming maximum efficiency. In this context, this study used a sample from the Bacia de São-Luis-Grajaú, Maranhão State, consisting of a mixture which is predominantly palygorskite and dolomite, approaching the existence of this new occurrence, suggesting a processing method and its application as phosphorus adsorbent, once dolomite is a pH soil corrector, while palygorskite has the function of nutrients carrier. First, chemical and mineralogical characterizations were performed, by XRD, XRF, SEM and separation of sand, silt and clay fractions. Sedimentation and phosphorus adsorption experiments were also performed, with determination of kinetic curve. After the analysis of XRD, results shown that the sample consists mainly of palygorskite and dolomite. Illite, chlorite and quartz are also presented. It was also possible to see that the different types of disaggregation used showed no significant differences in the diffractograms of the samples. The sand-silt-clay separation, although only based on the size of the material, showed a reasonable efficiency for material separation, as the sedimentation tests, where it was noticed that after a 24 hours period, dolomite had disappeared from the supernatant. Determination of kinetic curve revealed that the adsorption period of 2 hours is not sufficient for phosphorus adsorption, requiring 24 hours to reach the reaction equilibrium. Sorption tests showed efficiency higher than 91% of the initial phosphorus present in solution, and the maximum quantity adsorbed per gram of sample was 0.607 mg. The correlation with the adsorption isotherm models studied, showed better results for Langmuir-Freundlich isotherm, with correlation coefficient of 0.9993, which can be attributed to the fact that adsorption occurs in more than one layer.
Acesso aberto (Open Access)
Caulim calcinado: estudo cinético da dissolução do alumínio em meio ácido e aplicação como precursor na produção de sílica porosa
(Universidade Federal do Pará, 2016-12-19) LIMA, Paula Elissa Antonio de; NEVES, Roberto de Freitas; http://lattes.cnpq.br/9559386620588673
A kinetic study of metakaolin (calcined kaolin) dissolution was carried out using kaolin for paper coating derived from the Rio Capim region (Pará State, Northern Brazil). The kaolin was calcined at 700ºC for 2 hours, in order to obtain metakaolin, and then leached with sulfuric, hydrochloric and nitric acid at 95ºC, 80ºC and 70ºC ± 3°C. The leachings were performed using excess acid of 5%. Samples were collected every 15 minutes for 3 hours and subjected to aluminum analysis by the EDTA titrimetric method. Final aluminum extraction of 97.42%, 97.99% and 95.9% was obtained with sulfuric, hydrochloric and nitric acid, respectively. Hydrochloric acid was faster than nitric and sulfuric acid, which showed a similar dissolution behavior. Kinetic models of homogeneous (Integral Method, Method of Half-Lives and Method of Initial Rates) and heterogeneous (Shrinking Core Model) reaction were used. The Shrinking Core Model for spherical morphology with a constant size showed better fit. The leaching process is chemically controlled, with leaching reaction of the first order with respect to aluminum from metakaolin, the first order with respect to sulfuric, hydrochloric and nitric acid concentration and activation energies of 87.78 kJ/mol, 90.60 kJ/mol and 91.58 kJ/mol, respectively. Previous research, using excess acid above 50%, are consistent with the data found in this study carried out with only 5% excess acid. The study about the application of calcined kaolin as a precursor in the porous silica production was carried out with the solid obtained in the leaching process with sulfuric acid. The leached material was a microporous solid, with 86.7% of silica, high specific area (297.13m²/g) and humidity adsorption capacity compatible with commercial silica.
Acesso aberto (Open Access)
O caulim duro da região do rio Capim, Pará: mineralogia, geoquímica e avaliação das propriedades cerâmicas
(Universidade Federal do Pará, 2003-02-28) CARNEIRO, Bruno Santana; NEVES, Roberto de Freitas; http://lattes.cnpq.br/9559386620588673
Acesso aberto (Open Access)
Desenvolvimento de processo para obtenção de zeólita do tipo faujasita a partir de caulim de enchimento, caulim duro e tube press: aplicação como adsorvente.
(Universidade Federal do Pará, 2015-03-31) ROCHA JUNIOR, Carlos Augusto Ferreira da; NEVES, Roberto de Freitas; http://lattes.cnpq.br/9559386620588673; 9559386620588673
The main purpose of this work is zeolite synthesis of faujasite type (X and Y) from kaolin from the beneficiation process for paper coating, hard kaolin or Flint (mining of waste), tube press kaolin and filler kaolin. For each process zeolitização kaolin used in a chemical reactor a product of calcination of each material (metakaolin), sodium metasilicate, solid sodium hydroxide and distilled water, subjected at 110 ° C, reaction time 13 h Si / Al ratio of 2, 4 and 6. The products of each zeolite synthesis as well as the starting kaolin were characterized by chemical, physical and mineralogical analyzes such as X-ray diffraction, X-ray fluorescence, electron microscopy scan and thermal analysis. From these tests, it was observed that all the kaolin showed the formation of faujasite zeolite, but with differences in the peak intensities and their associations with other zeolite phases. Hard kaolin showed a lower potential zeolitization into the Si / Al ratio equal to 2 compared with the other two supposedly related to the iron present in its composition, thus made was a removal process of this constituent, by Mehra and Jackson method to verify a possible maximization in the synthesis process. New results indicated a complete modifications to the area and degree of structural order of faujasita phase, now moving into a major phase and there is an increase in the degree of structural order. As this reaction condition for consumption and a lower cost of raw materials and energy for calcination This medium was used as a starting point for an experimental design to evaluate the best reaction conditions. This design was varied some parameters of the synthesis as temperature, reaction time, Si / Al ratio and H2O / Na2O. The results of the statistical design showed the formation of faujasite in 32 points of study, as well as a great region with 8 points of planning, in this region point 13 proved the best reaction conditions. The zeolite synthesized at this point, showed an increase of ammonium adsorption capacity and percentage near 85 % efficiency up to 60 ppm. The Langmuir model was more suitable than the Freundlich and Sips in agreement with experimental data. The thermodynamic parameters showed that adsorption of NH4 + is a spontaneous and exothermic process, in which the temperature rise from 25 to 60 ° C promotes a small decrease in the adsorption capacity.
Acesso aberto (Open Access)
Desenvolvimento de processos de síntese de sodalita a partir de rejeitos de caulins da região Amazônica
(Universidade Federal do Pará, 2013-01-17) SILVA, Liliane Nogueira da; NEVES, Roberto de Freitas; http://lattes.cnpq.br/9559386620588673
In the study of the Sodalite synthesis used two wastes kaolins from two kaolin processing industries for paper coating, located in the Amazon region, operating in the region of Rio Capim (CRC) and Rio Jari (CRJ). Besides this, was also used as a source of silica and alumina to metakaolin, obtained by calcination of kaolin (MRC and MRJ, respectively). Preliminary chemical and mineralogical characterization of kaolin was performed to obtain information of its characteristics. The Sodalite synthesis was performed varying some parameters, such as starting material: kaolinite was used directly as starting material at temperatures of 80, 100, 120 and 150 °C, and, starting with metakaolinite at 95 °C. In order to observe the influence of ions OH, Cl- and CO32-, as well as Na2O/Al2O3 ratio, the syntheses were carried out varying the basic solutions, set temperature at 95 °C for the starting material MRC. Furthermore, the Na2O/Al2O3 ratio were maintained constant and temperature were varied in the reaction mixture to determine the ideal conditions for Sodalite synthesis. The starting materials and the synthesis products were identified and characterized by using XRay Diffraction (XRD) and Scanning Electron Microscopy (SEM) analysis, Thermal Methods (DTA/DTG) and Fourier Transform Infrared Spectrometry (FTIR). The method of synthesis that show best results were used as starting material metakaolin, with NaOH + Na2CO3 solution having Na2O/Al2O3 ratio of 3.89 conducted under stirring at 95 °C, atmospheric pressure and a time of 4 hours, for the two types of kaolin (CRC and CRJ). Using the MRC metakaolin, kaolin from the Rio Capim, under the above conditions was obtained by conversion of 86.5% by weight of sodalite and MRJ metakaolin, kaolin of the Rio Jari, the conversion was 73.6% in sodalite. All products were characterized as mesoporous materials, but starting from the product of metakaolin Rio Jari showed higher specific area.
Acesso aberto (Open Access)
Efeito do tempo de síntese de zeólita A a partir de caulim amazônico, conformação por extrusão e verificação desta na eficiência de adsorção de NH4 +
(Universidade Federal do Pará, 2015-04-24) SANTOS, Suzianny Cristina Arimatéa; NEVES, Roberto de Freitas; http://lattes.cnpq.br/9559386620588673
Kaolin is widely used in the field of materials (ceramics, pozzolans, fillers and manufacture of paints) as much as the waste and the product received. Currently the most exploited use has been in zeolite synthesis, as it presents the most noble applications. Zeolites are synthesized from silicon and aluminum sources, a fact that justifies the use of kaolin, because it is formed essentially by the clay mineral kaolinite (Al2Si2O5 (OH) 4). In this work we made a kaolin comparison of Grass River region with kaolin mineralogical / chemical and other Amazon kaolin reference to see if you can make it a reference material. The comparison was carried out by size analysis, X-ray diffraction, X-ray fluorescence, scanning electron microscopy, differential thermal analysis and infrared spectroscopy and crystallinity calculations. Moreover, the kaolin of the Rio Capim region was used as a source of silicon and aluminum to obtain the zeolite in order to determine the effect of time on the synthesis. Assays were performed in a time of 30 min, 1 h, 2 h and 24 h applied in these zeolites ammonia adsorption. From the synthesized zeolite was carried out the forming process by extrusion, evaluating various ligands (sodium silicate, bentonite, kaolin and CMC) and firing temperatures (500, 700 and 800 ° C). Later, these were extruded applied also in ammonium adsorption to check its efficiency. It was observed that it is possible to use kaolin Grass River as mineralogical reference material (high degree of structural order) and/or chemical, because it showed performance equal or close to the reference kaolin compared in this work. The zeolite A was synthesized from Amazon kaolin and this presented an excellent silicon and aluminum source. All synthesis times gave zeolite A zeolite in amounts of ~ 600 g. All zeolites showed a high degree of structural view to XRD and SEM. It was also found that synthetic zeolite A in 30 minutes time can be performed without loss in its application, since it presented below only 3% difference in adsorption efficiency compared to 24 h. The shaping by extrusion tests proved promising, 5 out of 10 trials were successful in obtaining granulated with physical strength. However, only the granules containing sodium silicate and CMC as a binder showed a high ammonia adsorption efficiency. With values of ~ 95,5% efficiency in 24 hours of contact.
Acesso aberto (Open Access)
Metacaulim: investigação da reatividade e da cinética de dissolução do alumínio em ácido sulfúrico
(Universidade Federal do Pará, 2012-12-11) LIMA, Paula Elissa Antonio de; NEVES, Roberto de Freitas; http://lattes.cnpq.br/9559386620588673
A research about reactivity and dissolution kinetics of metakaolin was carried out using kaolin for paper coating derived from the Rio Capim region (Pará State, Northern Brazil). The kaolin was calcined at 600, 700, 800, 900 and 1000ºC during 2 hours in order to obtain metakaolin, followed by leaching with sulfuric acid at constant temperatures within the range of 50-95ºC ± 3ºC. In the leachings, amounts of sulfuric acid corresponding to 10% above the stoichiometric values were used with respect to aluminum present in the material. Samples were collected in predetermined intervals every 15 minutes until a total time of 3 hours, which were subjected to aluminum analysis by the EDTA titrimetric method. The kaolin and products of calcinations and leachings were characterized by XRD, XRF, DTA-TG, SEM, BET analysis as well as granulometric and real density analysis. The results showed that the initial material was a mesoporous solid, in which the calcination process at 700ºC increased the number of mesopores in the material and sulfuric leaching process at 95ºC promoted the formation of a microporous solid with a high specific area (297.13 m²/g) and consisting essentially of amorphous silica. The calcination at temperatures above 800ºC indicated the beginning of the structure consolidation process. The reactivity of metakaolin was reduced with the increase of calcination temperatures in the range studied. The dissolution kinetics of aluminum in the metakaolin, obtained by calcination at 700ºC, followed the methods of homogeneous (Integral Method, Method of Half-Lives and Method of Initial Rates) and heterogeneous (Shrinking Core Model) reaction used. 96.85 kJ/mol of activation energy was found as well as leaching reaction of the first order with respect to aluminum from metakaolin and the first order with respect to acid concentration. Researches carried out previously, using one of the reagents with excess above 90%, are consistent with the data found in this study developed with only 10% excess.
Acesso aberto (Open Access)
Síntese de zeólitas A e 5A a partir de caulim: uma comparação dos métodos de síntese estático e dinâmico
(Universidade Federal do Pará, 2011-05-11) SANTOS, Suzianny Cristina Arimatéa; NEVES, Roberto de Freitas; http://lattes.cnpq.br/9559386620588673
Greater awareness of environmental issues and policies on conservation have been doing that arise with new proposals for waste recycling. One of those ways is to reuse the employment of the tailing of the beneficiation of kaolin in zeolite synthesis from kaolin tailing, because zeolites have a wide applicability. Zeolite 5A was synthesized by cation exchange using as starting material zeolite A and calcium solution. We have developed a process for synthesis of zeolite A and zeolite 5A, and the kinetic monitoring of obtaining these crystalline phases and scaling of zeolites A and 5A. The following methods were used: XRD, XRF, SEM, DTA-TG and sieve analysis. It was found that using the two methods of synthesis were obtained zeolites A and 5A, but with only variations in the intensities of their peaks, where the synthesized zeolites in dynamic method showed greater intensity and a greater possibility of scaling up production to 400g. The products were used in zeolite adsorption system, the adsorption tests of moisture in the air the same show promise, arriving adsorb up to 20% on the mass of zeolite. It was found that the new dynamic methodology developed for production of zeolite A in this work proved to be much higher than the previous static approach, because it allowed a greater increase in scale beyond the reduction of synthesis time.
Acesso aberto (Open Access)
Síntese e caracterização de analcina obtida a partir de rejeito caulim com aplicação em adsorção
(Universidade Federal do Pará, 2006-12-19) CORREA, Edinelson Saldanha; NEVES, Roberto de Freitas; http://lattes.cnpq.br/9559386620588673
In this work from kaolin processing industries from Ipixuna-PA were used in order to synthesi analcime derived zeolite as predominant crystalline phase though the hydrothermal process. The sample was converted into metakaolinite by calcinations at 700°C during 4 hours. From sample this metakaolinite a reacting mixture consisting of diatomite and sodium hydroxide was prepared. In order to determine of ideal conditions for analcime synthesis, a number of process variables were measured such as sodium availability, silicon ratio, nature of the silica source, pH of the reacting mixture, and auto clave residence time. Some important properties of the adsorbent where measured as well, such as thermal stability in the presence of acids hydrogen desorption kinetics, the trends of the adsorption isotherms as such as selectivity for copper, cadmium, zinc and nickel ions. Analcime synthesis from kaolin processing wastes was feasible. A displacement in the (h, k, l) planes was observed at 400 °C and was maintained up to 600°C, caused by the withdrawal of oxygen in positions 1/8 in analcime, shrinking the unit cell and in active channels and sites of zeolite, affecting its adsorption capacity.
Acesso aberto (Open Access)
Transformações térmicas e propriedades cerâmicas de resíduos de caulins das regiões do rio Capim e do rio Jari – Brasil
(Universidade Federal do Pará, 2006-03-23) MARTELI, Marlice Cruz; ANGÉLICA, Rômulo Simões; http://lattes.cnpq.br/7501959623721607; NEVES, Roberto de Freitas; http://lattes.cnpq.br/9559386620588673
Mullite, Al6Si2O13, is a relatively rare mineral in nature, formed under exceptional conditions of high temperature and pressure, which can be used to synthesize this mineral. Mullite presents excellent mechanical resistance at high and normal temperatures; low thermal expansion coefficient; good chemical and thermal stability. Such characteristics explain the importance of mullite in traditional and advanced ceramics. This research proposes the development of a process to synthesize mullite using the wastes from kaolin processing industries located in the rio Jari (Monte Dourado-PA) and rio Capim (Ipixuna-PA) districts. Preliminary studies are made on the synthesized materials for application as base materials for grog and silicon-aluminum refractory bricks. The steps are: (a) mineralogical and chemical characterization, verifying the differences between the materials; (b) processing through calcinations of the wastes at increasing levels of temperature with 100 oC increments, ranging from 600 to 1500 oC, during 3 hours at each level, so mineralogical changes can be observed and; (c) the study of temperature and impurities effects through X-ray powder diffraction, scanning electron microscopy, green bodies cleavage, thin layer and polished section; and of ceramics properties, through green bodies retraction (shrinking). The results of this work indicate that detrites from kaolin industries at rio Jari and rio Capim are constituted mainly by kaolinite. The PR samples showed a higher level of structural order than the CR samples. The increase in calcination temperature favored agglomeration in both samples. A higher content of Fe in the CR samples influenced mullite formation, activation energy, and linear shrinking in sintering. Also, through to the results of the refractarity essays, both industrial waste samples showed that they can be used as starting materials for refractories and grog.