Navegando por Assunto "Sodalita"
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Dissertação Acesso aberto (Open Access) Cristaloquímica da sodalita Bayer derivada de bauxitas com alta sílica reativa de Paragominas-Pa(Universidade Federal do Pará, 2016-05-24) MELO, Caio César Amorim de; ANGÉLICA, Rômulo Simões; http://lattes.cnpq.br/7501959623721607In the Paragomina’s region, as well as the whole Brazilian north, gibbisitic bauxite deposits commonly shows high amount of kaolinite. The processing of this bauxites (called as High Silica Bauxites - BASR) became a challenge because in the conventional conditions of the Bayer process, the kaolinite is undesirably leached by NaOH solution, and then precipitated as sodalite. The formation of this phase brings a significant increase in process costs, both by increasing the processing time as the irreversible loss of NaOH robbed from the system to form sodalite, which is then discarded in the red mud. Given this metallurgical problem this study aimed to investigate the crystal chemistry of sodalite formed in conventional conditions of the Bayer process, so that, from these results, studies to reduce these losses of the process and facilitate the processing of BARS can be developed in the future. The materials investigated were kaolinitic gangues from 4 lithologies of an exploration well in Miltonia 3 mine (BN, BNC, BC and BCBA), as well as a kaolin from IMERYS S.A. The digestions were carried out in Teflon-lined, stainless steel autoclaves, using 1 g of solid material, 25 mL of NaOH solution and at a temperature of 150ºC in an oven. The NaOH concentration and the reaction time ranged from 2,5 to 5,0 M and 60 to 420 min, respectively. Then the solid material was characterized by XRD, DTA/TG, FTIR, SEM and ICP-OES. The results of the starting materials showed that the kaolin sample is essentially constituted by kaolinite, which has a high structural ordering degree. All the samples of kaolinitic gangue showed the same minerals: gibbsite, kaolinite, hematite, goethite and anatase. By the observation of the XRD patterns and DTA curves can be noted that the BN and BNC samples are more reactive than the others, possibly due a lower structural ordering degree and particle size. In the experiments with kaolin, it can be observed that are formed not one, but two sodalite phases, which coexist practically throughout the whole process and tending to an equilibrium phase. These two phases differs themselves by the amount and behavior of the NaOH and H2O molecules within the framework. The results of the refinments showed that these phases were: basic sodalita with cell parameter (ao) ~ 8,96 Å, which is predominant in the initial stages of the transformation, and hydrosodalite with ao ~ 8,85 Å dominant in the secondary stage (mainly in 180 min). The XRD results from kaolinitic gangues showed that in 60 min there was no full kaolinite/sodalite conversion, and the sodalite patterns in BN and BNC were more intense and well defined than BC and BCBA, confirming that these samples have more reactive kaolinites. The increase of the reaction time and NaOH concentration provided a slight increase of the structural sodalite order. It may be noted that in almost all experiments the only phase formed was basic sodalite. The exceptions were the lithologies: BCBA and BC, which hydrosodalite was formed in the highest time of reaction and NaOH concentration, thus showing that this phase is directly associated with a higher time, concentration and crystallinity of kaolinite available in the reaction medium. It can be observed that throughout the reaction, in shorter time and concentration it is not possible to achieve a balance, which leads to a constant interchange of predominant phase in the system. In the higher time and concentration experiments, a balance is virtually reached, in order that it cannot be observed separated diffraction peaks. However there is no significant increase of the structural ordering even for extreme times as 3 days of reaction. The ammonium chloride experiments showed that this reaction medium allows the formation of more crystalline phases than all others achieved in this research. However, it did not result in the diminished of the sodium consumption.Dissertação 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/9559386620588673In 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.Tese Acesso aberto (Open Access) Desenvolvimento do processo de síntese da zeólita A e da sodalita a partir de rejeitos de Caulim da Amazônia com aplicações em adsorção(Universidade Federal do Pará, 2011-08-31) MAIA, Ana Áurea Barreto; POLMANN, Herbert; ANGÉLICA, Rômulo Simões; http://lattes.cnpq.br/7501959623721607; 7501959623721607The minimization of industrial and domestic residues is one of the great challenges that human kind is facing. Several proposals are released for this intention, ranging from improving industrial processes in order to minimize waste generation, besides their use in the production of new materials. In this context, this work has the main purpose of using kaolin residues from industries located in the Pará State, northern Brazil, for the production of zeolites (e.g., zeolite A and sodalite). These companies exploit kaolin from the world famous Capim and Jari regions and produce high quality kaolin for the paper industry. Preliminary mineralogical and chemical characterization of the Capim (KC) and Jari (KJ) kaolin residues was carried out as the basis for further zeolite A and sodalite synthesis. The study of thermal activation of kaolinite at various temperatures was carried out using 27Al and 29Si magic angle spinning nuclear magnetic resonance (MAS NMR), in order to to produce highly reactive metakaolinite from KC and KJ residues. The zeolite NaA synthesis was performed for varying parameters such as time and Na/Al relation. Temperature was kept constant at 110 °C for the two starting materials (KC and KJ). The KA, MgA and CaA phases were prepared by ionic exchange from phase NaA. In the sodalite synthesis, kaolinite was used directly as starting material and two temperatures (150 and 200 °C) were utilized. The Na/anion and Na/Al relations were maintained constant and varied, respectively in the reaction mixture for KC and KJ. The removal performance of mixed metal ions (Co2+, Cr3+, Cu2+, Zn2+ e Ni2+) in aqueous solution was investigated by adsorption process on zeolite NaA prepared from KC an KJ as proposal to reduce environmental problem with industrial wastewater streams that contain heavy metals. The XRD results showed that the residues are mainly composed of kaolinite with extremely low impurity level. For comparing the residues from two regions, Capim and Jari verified that the KC displays a high degree of structural order. This difference displays significant influence in the ideal heating temperature to produce a material with high amount of 4-coordinated A1. As a result, the ideal temperature to produce highly reactive metakaolinite is: 600 °C for Jari kaolin residue and 700 °C for Capim kaolin residue. Zeolite A was produced with a large degree of structural order and was generally obtained as the only zeolitic product. The following synthesis conditions were used: Na/Al ratio of 1.64 and time 18 and 20 h for KC and KJ, respectively. The cationic exchange process between Na from zeolite A and K, Mg and Ca in solutions displays efficient result and with XRD data, was verified that the KA, MgA and CaA phases were obtained with success. The sodalite series was produced from KC and KJ and by FTIR was confirmed the chloride, sulphate and carbonate insertion in its structure. The KJ kaolinite displays high reactivated in the sodalite synthesis, it could be explicated by its low degree of structural order. The sorption capacity of heavy metals mixture (Co2+, Cr3+, Cu2+, Zn2+ e Ni2+) on zeolite NaA, produced from KC and KJ, display satisfactory values. The results revealed that the Langmuir model is more appropriate than Freundlich in the fit of the experimental data. Zeolite A, produced from residues (KC and KJ), could be excellent materials for the treatment of wastewater.Dissertação Acesso aberto (Open Access) Estudo da síntese de zeólitas tipo A, X e sodalita empregando reatores vítreos: análise dos métodos dinâmico e estático de síntese a partir de caulim residual da Região Amazônica(Universidade Federal do Pará, 2013-12-26) SENA, Rafael dos Santos Fernandes; MARTELLI, Marlice Cruz; http://lattes.cnpq.br/1213009262936026Kaolin processing companies generate kaolinitic residue that is stored in sedimentation ponds, occupying large physical areas. The utilization of these wastes is an important factor in the economic and the environmental terms. Here a study of the synthesis of A, X and sodalite zeolites using as raw material a kaolin waste from the Amazon Region is presented. The waste was pretreated for removal of the organic matter, comminuted and thermally activated at 750 °C for 2 hours. After selecting the optimum particle size for the synthesis by the pré-zeolitização step, two methods were tested to obtain the zeolites: dynamic and static. For the reaction mixture of the synthesis, were worked with the ratios SiO2/Al2O3 of 2/1 and 3/1 to obtain zeolites. Analyses of X-Ray Diffraction (XRD), X-Ray Fluorescence Spectroscopy (XRF) and Scanning Electron Microscopy (SEM) analyzes showed good phase formation for the NaA zeolite to the ratio 2/1, in the both sinthesys methods, dynamic and static, and without aging, and good phase formation for the NaX zeolite to the ratio 3/1, using static synthesis and with 12 hours aging. The sodalite phase was formed in the same stoichiometry of the NaX zeolite, but using static synthesis and without aging.Dissertação Acesso aberto (Open Access) Otimização da síntese de pigmentos zeolíticos ultramarinos derivados de rejeito de caulim usando um DOE 2ˆ3 completo.(Universidade Federal do Pará, 2024-07-03) JESUS, Geyna Evellyn Silva de; PAZ, Simone Patrícia Aranha da; http://lattes.cnpq.br/5376678084716817; https://orcid.org/0000-0002-5880-7638The state of Pará is recognized as an important center for kaolin production for paper coating, resulting in a significant amount of waste, mainly composed of kaolinite. Research groups at the Federal University of Pará have been exploring the use of this waste as an alternative source of silicon and aluminum in the synthesis of zeolites, particularly zeolite A, which has the potential for producing ultramarine pigments. These inorganic pigments are highly valued due to their deep blue color and good chemical and physical stability. LTA and sodalite zeolites are the main crystalline structures involved in this process, with the S3⁻ anionic radicals responsible for the blue color. The synthesis process involves calcination of the zeolite with sulfur and sodium carbonate, resulting in the diffusion of sodium polysulfides through the zeolite pores and the production of pigments with color variations depending on the synthesis conditions. The aim of the study was to understand how the crystalline structure of zeolites (LTA zeolite and sodalite) affects the pigment color and to propose an optimization for the more efficient synthesis of these pigments. To achieve these objectives, a sequential experimental design methodology (DOE) was applied. A Full Factorial Design followed by a Central Composite Design was used to identify the significant and influential factors in obtaining the ultramarine blue color. For optimization, the response surface methodology was employed in conjunction with the Excel Solver function. The response obtained was color, and the factors were temperature, time, and S/Na2CO4 ratio. The analyses that supported the crystallochemical discussion were: Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), X-ray fluorescence (XRF), differential scanning calorimetry (DSC), and thermogravimetry (TG), particle size distribution (PSD), zero point charge (ZPC), and UV-Vis diffuse reflectance spectroscopy, and Munsell Color System was used for color classification. The crystallochemical analyses of the pigments obtained from LTA zeolite revealed the insertion of S3⁻ chromophores into the zeolitic structure, which was corroborated by FTIR and DSC-TG analyses, highlighting characteristic peaks of these phases. UV-Vis spectroscopy revealed the presence of both S2⁻ (associated with green hue) and S3⁻ (associated with blue hue) chromophores, with the optimized product showing a higher concentration of S3⁻ chromophore, indicating the effectiveness of the planning. On the other hand, UV-Vis analysis of the pigment derived from sodalite did not show characteristic peaks of the chromophores of interest. Finally, this research assumes significant relevance in the global context of environmental impacts resulting from waste generation, offering a promising alternative for the management of kaolin waste and the production of synthetic ultramarine pigment. The synthesis of this pigment from LTA zeolite represents a more environmentally sustainable approach due to the almost negligible reduction in sulfur oxide emissions, positioning itself as a viable and environmentally conscious solution for obtaining this type of pigment.Tese Acesso aberto (Open Access) Produção de material zeolítico a partir de caulim da Amazônia em escala semi piloto: aplicação na adsorção de cobre(Universidade Federal do Pará, 2019-06-27) RODRIGUES, Emerson Cardoso; MACÊDO, Emanuel Negrão; http://lattes.cnpq.br/8718370108324505; SOUZA, José Antônio da Silva; http://lattes.cnpq.br/6157348947425968This work aims to synthesize a zeolite product composed of zeolite type "A" plus sodalite using as filler kaolin starting material. The synthesis of Zeolites was carried out in a short time and in a system with agitation, in a reactor of stainless steel with a volume of approximately 0.001 m3, that is, in semi-pilot scale. The system was heated by steam from a boiler. The X ray diffraction (XRD), X ray Fluorescence Spectrometry, Scanning Electron Microscopy (SEM), Granulometric Analysis and Differential and Gravimetric Thermal Analysis (DTA and TG) were identified and characterized. In the synthesis process the metakaolin was used as the source of silica and alumina, which was obtained at 600 ° C for 2 hours of calcination in a muffle furnace. A 5M sodium hydroxide solution was used as the sodium source. Several syntheses were carried out for a maximum duration of 180 minutes. Every 30 minutes aliquots of the product were taken for the study of reaction kinetics. The results of the zeolite syntheses were satisfactory and the product obtained was applied to the adsorption of Cu2+ ions, in which the influence of the variables: time, temperature, pH and adsorbent quantity were evaluated. The determination of the best adsorption model was performed by the Monte Carlo method via Markov Chain and through the Akaike Information Criterion the isotherms that were closest to the presented results were established. The results obtained were compared with other studies available in the literature and showed significant values, which characterize the process of zeolite production and adsorption as promising and efficient.Artigo de Periódico Acesso aberto (Open Access) Síntese hidrotermal de sodalita básica a partir de um rejeito de caulim termicamente ativado(2010) PAZ, Simone Patrícia Aranha da; ANGÉLICA, Rômulo Simões; NEVES, Roberto de FreitasBasic sodalite was successfully synthesized by hydrothermal method using kaolin waste as source of Aluminum and Silicon. This waste is mainly composed by kaolinite and is produced in large amount by kaolin processing industries for paper coating from the Amazon region. Initially, the waste has been calcined at 700 ºC for 2 h and then reacted with the following solutions: Na2CO3 and mixture of Na2CO3 + NaOH to 150 ºC with autogenous pressure for 24 h. The raw materials and transformed materials were characterized by XRD, FTIR and SEM. In both studied media, well-crystallized, basic sodalite was the only phase synthesized, while in the literature usually a mixture of zeolites is obtained.
