Navegando por Assunto "Zeolitos"

Agora exibindo 1 - 9 de 9

Acesso aberto (Open Access)
Arenito zeolítico com propriedades pozolânicas adicionadas ao cimento Portland
(Universidade Federal do Pará, 2011-08-29) PICANÇO, Marcelo de Souza; BARATA, Márcio Santos; http://lattes.cnpq.br/7450171369766897; ANGÉLICA, Rômulo Simões; http://lattes.cnpq.br/7501959623721607
The proper use of pozzolans enables the production of special cements with lower manufacturing cost and higher durability in comparison with cements without mineral additions. It also enables significant gains in productivity and extending equipments life in the fabric, limestone reserves, and also helping in the reduction of CO2 release into the atmosphere. Zeolites have been used as pozzolanic material in mixtures with Fuller’s Earth and water in buildings from the ancient Roman Empire. Nowadays, there are many discussions involving pozzolanic reactivity of natural zeolites in the incorporation of Portland cement. In the Northeastern region of Brazil, sedimentary zeolites related to sandstones of the Parnaiba Basin wer discovered by the Geological Survey of Brazil in the 2000s. These sandstones are mainly composed by quartz, natural zeolites (estilbity) and clay (smectite). Preliminary studies have pointed that this sandstone may be used as pozzolanic material in Portland cements. The material must be previously sieved to remove quartz and thermally activated, since stilbite is a zeolite with low pozzolanic activity. The main objective of this work is to advance the understanding of the factors that govern the quality and performance of Portland cement modified with this zeolitic sandstone. For this work the structure was divided into three main stages, related to three specific objectives, so that the results are presented in the form of three scientific papers, described as follow: - Evaluation of the natural pozzolanic activity of the zeolitic sandstone to be used as mineral addition in the Portland cement. - The determination of which particle size provides the highest zeolite and smectite concentration, besides the calcination temperature that leads to a higer pozzolanic activity. - The establishing of the best amount of thermally activated zeolitic sandstone to be incorporated as a mineral addition in the Portland cement. During all phases, different instrumental techniques were used for the chemical and mineralogical characterization of the starting materials and products (sandstone + lime mortar, mortar with Portland cement + sandstone + Portland cement pastes sandstone), including: spectroscopy x-ray fluorescence, x-ray diffraction, thermal analysis and scanning electron microscopy. Heat-flow calorimetru assays were carried out to evaluate the physical properties, besides mechanical testing of compressive strength of cement mortars Porltand. In the first stage of the experimental program, the zeolitic sandstone was sieved into different granulometric fractions in order to remove the inert phases (quartz and other minerals), and concentrate the zeolite for further pozzolanic assays. In the second stage, after the first characterization of the samples, we used the zeolitic sandstone that passed in the # 200 and # 325 sieves and calcined at temperatures of 150º C, 300° C and 500° C. Finally, in the third stage, # 200 fraction was calcined at 500 ° C and mixed in different proportions (10, 20 and 30%) in the mortar. The results of the first stage, which culminated in the first article showed that the zeolitic sandstone accelerated the hydration of Portland cement due to the extreme fineness of the material. The sandstone showed pozzolanic activity, and estilbite is the main responsible for this behavior. However, the reactivity was slightly lower than the minimum required to be employed as pozzolan on an industrial scale. Additional studies are needed to ascertain if the thermal treatment between 400° C and 300o C could increase the pozzolanic activity of the sandstone due to the destruction of the crystalline structure of both estilbite and smectite. For the second stage, the results showed that the # 200 fraction was the most suitable because of the higher estilbite concentration (15%) in comparison to the # 325 ssample (2%). The calcination temperature of 500º C has provided the highest pozzolanic activity due to more effective destruction of the crystalline structure of both estilbite and smectite. More moderate temperatures of 150° C and 300° C were not enough. Mortars with the 200 # sample calcined at 500 ° C reached values smaller as those required for a material to be considered as a pozzolane, in this case, 6 MPa for mortar of lime and 75% for the pozzolanic activity index (IAP). The results showed from the third stage showed that the AZ2-3 mixture (10% of zeolitic sandstone incorporated in Portland cement type CPI-S), showed the best result of compressive strength and mineralogical properties of the samples suitable for the production a commercial cement type CPII-Z. In general, one concludes that the zeolitic sandstone from northeastern Brazil has the potential feasibility of producing a CPII-Z cement, whose pozolan contents ranges from 6 to 14% in the Portland cement, according to the ABNT - NBR 11578. Although the strength of the mortar with 10% of AZ2- 3 has reached resistance values close to the reference mortar with 100% of CPI-S, further studies should be carried out in order to find better proportion of sandstone and to meet the requirements for future commercialization.
Acesso aberto (Open Access)
Atividade pozolânica de arenito zeolítico da região Nordeste do Brasil
(2012-06) PICANÇO, Marcelo de Souza; ANGÉLICA, Rômulo Simões; BARATA, Márcio Santos
In northeastern Brazil, sedimentary zeolites occur associated with sandstones of the Corda Formation (Parnaiba Paleozoic Basin), discovered in the 2000s. These sandstones are composed of quartz, natural zeolites (estilbite) and clay minerals (smectite). Preliminary studies have shown that this sandstone can be used as a pozzolanic material in Portland-cement-based systems after the material has been sieved to remove the quartz and after thermal activation because the estilbite has low pozzolanic activity. The main objective of this study was to determine the best particle size distribution that yields the highest smectite and zeolite concentration, besides the best temperature for higher pozzolanic activity. The experimental program employed the zeolitic sandstone passing through a #200 and #325 mesh sieve and calcination at the following temperatures: 150°C, 300°C and 500°C. Chemical analysis of the sieved samples was carried out by X-ray fluorescence spectroscopy and X-ray diffractometry, while mineralogical characterization was done by X-ray and thermogravimetric analysis and thermogravimetry..To assess reactivity, calorimetry driving and mechanical tests for pozzolanic activity in hydrated lime and cement Porltand were performed. The results showed that the sample sieved through at #200 mesh was the most suitable because it had a higher concentration of estilbite and a higher percentage of material seived compared to the sample sieved at #325 mesh, 15% and 2% respectively. The 500°C calcination temperature was accompanied by increased pozzolanic activity due to changes in estilbite and smectite cristalinity; the more moderate temperatures of 150°C and 300°C were not sufficient to achieve similar results. The mortars with sandstone sieved at #200 mesh and calcinated at 500°C reached the minimum limits required for a material to be considered as pozzolanic, i.e, 6 MPa for hydrated lime mortars and 75% for the pozzolanic index activity (PAI).
Acesso aberto (Open Access)
Avaliação preliminar do emprego de arenito zeolítico da região nordeste do Brasil como material pozolânico para cimento Portland
(2011-12) PICANÇO, Marcelo de Souza; ANGÉLICA, Rômulo Simões; BARATA, Márcio Santos
Natural zeolites usually exhibit pozzolanic activity without any additional treatment, e.g. thermal activation. They have been used for building since the ancient Roman Empire times in the production of hydraulic cements and concretes. Nowadays, there are many discussions involving the natural zeolites pozzolanic reactivity in the incorporation of the Portland cement composition. The appropriate use of pozzolans enables the production of special cements with lower manufacturing cost and with a greater durability in comparison with the corresponding cements without addition. In Brazil, zeolite consumption comes either from the importation of foreign countries or synthetic products. No zeolite mine is available in the country and only few geological occurrences were already described in the literature without any commercial interest. In northeast Brazil, the Geological Survey (CPRM) discovered zeolite-bearing sandstones related to Cretaceous sedimentary rocks of the Parnaíba Paleozoic Basin. The main purpose of this paper is to evaluate the possible use of such sandstones as pozzolan for using in Portland cements (CPI-S). A bulk sample of the zeolitic sandstone (AZ) was collected in the field. In the laboratory, preparation included drying, milling and sieving at the following grain-size fractions, in order to remove quartz and concentrate the zeolite: 100# (AZ-1), 200# (AZ-2) and 325# (AZ-3). After mineralogical evaluation, the AZ-2 fraction was selected for further analysis and assays. The experimental study was mainly based on mineralogical characterization, including: X-ray diffraction (XRD), chemical analysis and heat flow calorimetry, besides pozzolanic activity assay and compressive strength. The results show that the mineralogical composition of the zeolitic sandstone is mainly quartz, zeolite (stilbite) and smectite. Stilbite is the main pozzolanic phase, and the smectite can also play an important role. The hydration of the Portland cement was accelerated due to the very fine grained nature of the material. Meanwhile, the reactivity obtained was slightly below the standard requirements to be used in industrial scale. Additional studies should be carried out in order to evaluate if a further thermal treatment (between 300 °C and 500 °C) may increase the pozzolanic activity due to the stilbite destruction around this temperature. The same happens with kaolinite that needs thermal treatment above 550 ºC to convert to the amorphous phase metakaolin in order to be used as one of the most commons pozzolans in the cement industry. The main purpose was to contribute for the production of an alternative kind of cement which produces less pollution to the environment (CO2 decrease in the atmosphere) with cost saving. In addition, it is expected to contribute for the exploitation of the sedimentary zeolites occurrences which have been relatively well studied from a geological point, but are still not mined.
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)
Estabilidade térmica da zeólita A sintetizada a partir de um rejeito de caulim da Amazônia
(2008-09) MAIA, Ana Áurea Barreto; ANGÉLICA, Rômulo Simões; NEVES, Roberto de Freitas
Zeolite A was calcined at 200, 400, 600, 800 and 1000 °C for 2h to evaluate its thermal stability. The zeolite A was synthesized using kaolin waste from kaolin processing industries for paper coating located in the Amazon region. Both zeolite A and further calcined products were characterized by X-ray diffraction analysis and scanning electron microscopy. The zeolite A structure remained stable up to 600 °C, where only small variations in peak intensities were observed. At 800 °C the diffraction pattern still exhibited zeolite A but with the absence of some peaks. At 1000 °C nepheline, mullite and probably sodalite were formed. The zeolite A was also heated at 900 and 950 °C to check the two exothermic peaks observed in the DTA curve. The X-ray diffraction analysis indicated the presence of nepheline, sodalite and mullite.
Acesso aberto (Open Access)
Potencialidade adsorvente da zeólita A derivada de rejeito de caulim na remoção de corantes
(Universidade Federal do Pará, 2017-10-18) ARAÚJO, Leiliane Cristina Cardoso; CORRÊA, José Augusto Martins; http://lattes.cnpq.br/6527800269860568
In the States of Pará and Amapá are the largest Brazilian reserves of kaolin. The process of beneficiation of this material generates a significant volume of waste, this is kaolin that is out of the specifications for paper coverage and ends up becoming an environmental liability, since large areas are required to be deposited. This reject consists mainly of the kaolinite clay that presents Si and Al in a ratio of 1: 1, ideal to be used as raw material in the synthesis of zeolites. Zeolite A is a microporous synthetic aluminosilicate, easily synthesized from kaolin waste, making it a low cost and effective material to remove contaminants present in the effluents, such as dyes, besides having a high degree of selectivity and other characteristics that make it an excellent adsorbent. Among the most used processes in the dye removal is the adsorption, because it has several advantages such as: low cost, high removal rates and the possibility of adsorbent recovery. The work methodology was carried out in four stages: 1) Zeolite A synthesis: the Tube Press kaolin was used as starting material from the company located in the Capim-PA River, which was subsequently calcined at 700 ° C for 2h, solution of NaOH (5 mols L-1) and distilled water. They were kept in a reactor for 2 h at 95 ° C under stirring. After the synthesis the material was washed to pH = 7 and dried. Both the starting material and the products were identified and characterized by DRX, MEV, DTA-TGA and granulometric analysis. 2) The adsorption study was performed with AM and VC dye solution at concentrations of 2-26mg L-1. The equilibrium, adsorption kinetics and thermodynamics were obtained. The tests were done in a batch system and the solutions after adsorption were analyzed in UV-Visible spectrophotometer, using λ = 585nm for AM and λ = 665nm for VC. 3) Zeolite A regeneration was performed with 50 ml of the dye solution in the concentration 10 mg L -1 and 150 mg zeolite A. After 24 h the suspension was centrifuged, the supernatant analyzed and the solid dried and then calcined at 650 °C for 2 h to a five-fold cycle. 4) Desorption study: 50 ml of AM and VC dye solution at 10 mg L-1 and 150 mg zeolite A, after adsorption of 24 h the solid was separated by centrifugation and the water and methanol solvents were subsequently added in five proportions to give the initial volume of 50 ml and kept under stirring for 24 hours and after analysis of the supernatant in UV-Visible spectrophotometer. In the results of the adsorption equilibrium, the percentage of adsorption decreases with increasing concentration, as more dye molecules are incorporated into the adsorbent, reducing the area and the available active sites. The maximum adsorption capacity at equilibrium for MA was 5.1 mg g-1 and for the CV of 14.09 mg g-1, in this way the equilibrium adsorption capacity was higher for the CV as compared to the MA. The mathematical model that best fit the experimental data of AM equilibrium was the Sips isotherm that combines characteristics of the Langmuir and Freudlich isotherms, whereas for the VC dye the best model is that of Freudlich suggesting that adsorption occurs in multilayers. The adsorption kinetics of AM and VC were adjusted to the pseudo second order model. The thermodynamics of adsorption of AM at temperatures of 30 °C to 70 °C is a spontaneous process, favored at higher temperatures. The thermal regeneration of zeolite A after 5 cycles of regeneration had a loss in the efficiency of the AM adsorption in 7% and 3% for the CV, indicating the possibility of reuse of the adsorbent. Desorption with the 50% mixture of each solvent showed the best results.
Acesso aberto (Open Access)
Síntese de zeólita do tipo faujasita a partir de um rejeito de caulim
(2012-12) HILDEBRANDO, Edemarino Araujo; ANGÉLICA, Rômulo Simões; NEVES, Roberto de Freitas; DIAZ, Francisco Rolando Valenzuela
Zeolitic materials were synthesized using as main source of silicon and aluminum an industrial waste generated during the processing of kaolin for paper coating, the starting material and formed phases as reaction products were characterized by XRD, SEM and DRIFT. The synthesis process occurred in hydrothermal conditions and the effects, time-temperature, as well as the relations Si/Al and Na/Al were considered. The results show that in the methodology developed from kaolin waste, initially calcined at 700 ºC for 2 h, subjected then reaction in alkaline medium at 90 ºC for 48 h in presence of additional silica was obtained faujasite-type zeolite with good crystallinity as phase predominant in the synthesis product.
Acesso aberto (Open Access)
Síntese, caracterização físico-química e aplicação de alumínossilicatos como adsorventes
(Universidade Federal do Pará, 2003-05) CASTRO, Elton Anderson Santos de; LEMOS, Vanda Porpino; http://lattes.cnpq.br/1829861620854008
In this work three differente aluminosilicates were used for evaluation of the index of recovery of the coloring monovalent metilene blue. The no-porous clay mineral, Kaolinite, from Capim river area in Pará, Brazil, was treated with hydrochloric acid 5N in order to increase the specific area. The microporous molecular sieve, zeolite NaP, was synthesized through the hidrotermal method, with the kaolinite of Capim river area being used as source of Si and Al. The hidrotermal method was also used for the synthesis of the mesoporous molecular sieve Al-MCM-48, wich received thermal treatment (calcination) at 540ºC under flow of N2 and air for 7h to removal of the agent director (surfactant). The porous and no-porous materials were characterized by X-ray diffraction, infrared spectrophotometry, thermodifferential and termogravimetric analyses and adsorption and desorption methods with N2. Chemical analysis for the clay mineral has been performed and scanning electronic microscopy was used for the microporous aluminosilicate. These materials were tested as adsorbents in the recovery of the metilene blue at concentration of 6ppm, in different times (20, 40, 60 and 120min) with the contact method being used. The concentration, separation method of phases and the more appropriate wave length were studied. The determination of the recovery index for the organic coloring, using the three materials, was performed through visible spectrophotometry. XRD and chemical analysis results revealed the high purity of the clay mineral kaolinite. The specific surface area increased by 31,23% after acid activation. The specific area obtained for Al-MCM-48, was of 1219m2g-1, which is a characteristic value for this kind of materials. The results of XRD indicate that the zeolita NaP was formed, but traces of the feldspatoid hidroxysodalite are also present, what could be confirmed by the SEM images. The values of the recovery index for the metilene blue demonstrated that the kaolinite under acid activation was the most effective (100% of recovery), followed by the zeolite NaP (97,89% of recovery) and Al-MCM-48 (97,35% of recovery). The results indicate the viability of use of these materials as agents for pre-concentration in cromatographic analyses.
Acesso aberto (Open Access)
Utilização de rejeito de caulim da Amazônia na síntese da zeólita A
(2007-09) MAIA, Ana Áurea Barreto; CORREA, Edinelson Saldanha; ANGÉLICA, Rômulo Simões; SOUZA, Célio Augusto Gomes de; NEVES, Roberto de Freitas
Zeolite A and Hydroxysodalite were synthesized after kaolin wastes from kaolin processing industries for paper coating, located in the Amazon region. The waste is mainly composed by kaolinite, which has the same SiO2/Al2O3 ratio requested for those two zeolites. Thereby, synthesis process may occur in two steps: 1) the kaolin was submitted to thermal treatment, through calcination process at 700 °C for 2 h, in order to obtain the metakaolinite phase. The metakaolinite obtained reacted with NaOH solution, in hydrothermal conditions, using autoclaves, at the following temperatures: 80, 110 and 150 °C for 24 h. The starting materials were identified and characterized by means of X-Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM) analysis and synthesis products were characterized by means of XRD, SEM, Thermal Methods (DTA-DTG) and Fourier Transformed Infrared Spectroscopy (FTIR). A mixture of Zeolite A and Hydroxysodalite was obtained through this process at 150°C. In the temperature of 110 ºC there was only the Zeolite A formation. Nevertheless, in the lowest synthesis temperature (80°C) there was no crystalline material formation for the established conditions.