During a winter season, when snow covers the watershed, the frequency of rain-on-snow (ROS) events is still raising. ROS can cause severe natural hazards like floods or wet avalanches. Prediction of ROS effects is linked to better understanding of snowpack runoff dynamics and its composition. Deploying rainfall simulation together with hydrological tracers was tested as a convenient tool for this purpose. Overall 18 sprinkling experiments were conducted on snow featuring different initial conditions in mountainous regions over middle and western Europe. Dye tracer brilliant blue (FCF) was used for flow regime determination, because it enables to visualise preferential paths and layers interface. Snowpack runoff composition was assessed by hydrograph separation method, which provided appropriate results with acceptable uncertainty. It was not possible to use concurrently these two techniques because of technical reasons, however it would extend our gained knowledge. Snowmelt water amount in the snowpack runoff was estimated by energy balance (EB) equation, which is very efficient but quality inputs demanding. This was also the reason, why EB was deployed within only single experiment. Timing of snowpack runoff onset decrease mainly with the rain intensity. Initial snowpack properties like bulk density or wetness are less important for time of runoff generation compared to the rain intensity. On the other het when same rain intensity was applied, non-ripe snowpack featuring less bulk density created runoff faster than the ripe snowpack featuring higher bulk density. Snowpack runoff magnitude mainly depends on the snowpack initial saturation. Ripe snowpack with higher saturation enabled to generate higher cumulative runoff where contributed by max 50 %. In contrary, rainwater travelled through the non-ripe snowpack relatively fast and contributed runoff by approx. 80 %. Runoff prediction was tested by deploying Richards equation included in SNOWPACK model. The model was modified using a dual-domain approach to better simulate snowpack runoff under preferential flow conditions. Presented approach demonstrated an improvement in all simulated aspects compared to the more traditional method when only matrix flow is considered.

This diploma thesis critically handles memorial book of John George of Schwamberg, leading noble of Bohemian kingdom, politician, contemporary and inheritor of lasts Rosenbergs. Partly dedicated to memorial books as a phenomenon of early modern age and live of John George from Schwamberg. Objective of this diploma thesis is approximate personal life of Schwamberg, partly his itinerary and circle of "masters and friends" through notes recorded in memorial book. Emphasis is put on individual listings and ilustrations and the differences are taken into account from other memorial books from the same period, possibly on matters that can be found in memorial books routinely too. Diploma thesis deals with emergence of memorial book of John George from Schwamberg, its destiny after death of John George and its next owners too.

No description available.

Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2016-03-09T23:03:54Z No. of bitstreams: 1 YuriMiguelVariani_DISSERT.pdf: 3175747 bytes, checksum: 334b76f54aeba438cc28f8534c116513 (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2016-03-11T19:15:29Z (GMT) No. of bitstreams: 1 YuriMiguelVariani_DISSERT.pdf: 3175747 bytes, checksum: 334b76f54aeba438cc28f8534c116513 (MD5) / Made available in DSpace on 2016-03-11T19:15:29Z (GMT). No. of bitstreams: 1 YuriMiguelVariani_DISSERT.pdf: 3175747 bytes, checksum: 334b76f54aeba438cc28f8534c116513 (MD5) Previous issue date: 2015-06-10 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior - CAPES / Os estudos realizados neste trabalho t?m como objetivo contribuir ao entendimento dos fatores direcionadores quer est?o envolvidos em uma cristaliza??o de uma estrutura ze?litica. Para alcan?ar tal objetivo, foram sintetizados tr?s novos c?tions org?nicos a base de um anel imidaz?lio: 1,2,3-trietilimidaz?lio (123TEI), 2-etil-1,3- dimetilimidaz?lio (2E13DMI) e 1,2,3-trietil-4-metilimidaz?lio (123TE4MI). Foi avaliando seu car?ter como direcionadores de estrutura (do ingl?s, Structure-Directing Agents - SDAs) na s?ntese de ze?litas puramente sil?cicas em meio fluor?drico. Por sua vez, foi estudado a concentra??o do gel de s?ntese em distintas rela??es H2O/SiO2, resultando na cristaliza??o de duas fases zeol?ticas, MFI e STF. Os c?tions org?nicos foram an?lisados mediante resson?ncia magn?tica nuclear (RMN de 13C), comprovando sua obten??o. Todos os materiais s?lidos obtidos foram caracterizados por difra??o de raios-X, an?lise termogravim?trica (TG/DTA), an?lise qu?mico elementar CNH, microscopia eletr?nica de varredura (MEV) e adsor??o-dessor??o de N2 dos materiais zeol?ticos obtidos, ze?litas MFI com o c?tion 123TEI e a ze?lita STF com o emprego dos tr?s c?tions, sendo tamb?m realizado um estudo te?rico computacional de din?mica molecular, avaliando e comparando as energias de intera??o entre o c?tion 123TEI mediante dados experimentais e 2E13DMI teoricamente com a estrutura zeol?tica MFI.

Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2018-03-12T13:04:19Z No. of bitstreams: 1 RafaelChavesLima_DISSERT.pdf: 15500276 bytes, checksum: 4f1a759afd6ed9c7eeb174d02f229d3e (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2018-03-13T20:23:09Z (GMT) No. of bitstreams: 1 RafaelChavesLima_DISSERT.pdf: 15500276 bytes, checksum: 4f1a759afd6ed9c7eeb174d02f229d3e (MD5) / Made available in DSpace on 2018-03-13T20:23:09Z (GMT). No. of bitstreams: 1 RafaelChavesLima_DISSERT.pdf: 15500276 bytes, checksum: 4f1a759afd6ed9c7eeb174d02f229d3e (MD5) Previous issue date: 2018-01-30 / O Conselho Nacional de Desenvolvimento Cient?fico e Tecnol?gico - CNPq / A assimila??o do modo como uma ze?lita ? formada partindo de um sistema amorfo e o controle sobre tamanho e morfologia dos produtos de s?ntese s?o aspectos fundamentais para a ?engenharia zeol?tica?. Um sistema para a s?ntese da ze?lita mordenita foi estudado, o qual possibilitou a obten??o de fase MOR sem indica??o da presen?a de qualquer outra fase. Foram realizadas varia??es nos par?metros: condi??o de tratamento t?rmico, temperatura, tempo, dilui??o do gel, teor e grau de pureza da ?gua, teor de s?dio, envelhecimento e tipo de s?lica, visando o estabelecimento da rela??o entre o tamanho e a morfologia dos produtos de s?ntese com as modifica??es efetuadas. A temperatura de cristaliza??o mostrou ser um fator primordial com rela??o ao tamanho de part?culas e cristalitos. A dilui??o do gel de s?ntese (50% m/m) proporcionou uma redu??o na agrega??o dos cristalitos e a varia??o do teor de ?gua na s?ntese implicou em mudan?as nas taxas de zeolitiza??o. O teor de s?dio modificou o crescimento dos cristais e o aumento de intercrescimentos e agrega??es de part?culas. Mudan?as na fonte de s?lica incrementaram a taxa de crescimento dos cristais e contribuiram para altera??es no tamanho dos mesmos. Cristais maiores foram obtidos a partir de sistemas com maior concentra??o de c?tions s?dio enquanto agregados de nanocristalitos. Agregados de pequenos cristalitos de mordenita pura de at? cerca de 50 nm foram obtidos com s?nteses realizadas a 150 ?C e com a dilui??o do gel j? preparado. Menores teores de s?dio e ?gua e o uso de fontes de s?lica de maior ?rea espec?fica (relativa a este tipo de material) tamb?m tendem ? resultar em menores cristalitos. Condi??es opostas viabilizaram o maior crescimento, gerando cristais de at? 1 ?m em m?dia. Os resultados mostraram que ? poss?vel exercer algum controle sobre o tamanho de part?cula e de cristalitos da ze?lita mordenita atrav?s do ajuste de par?metros inerentes ao sistema convencional de s?ntese. / The assimilation of the way a zeolite is formed from an amorphous system and the control over size and morphology of the synthesis products are fundamental aspects for "zeolitic engineering". A system for the synthesis of the mordenite zeolite was studied, which made it possible to obtain MOR phase without indicating the presence of any other phase. Variations were made in the parameters: thermal treatment condition, temperature, time, gel dilution, water content and degree of purity, sodium content, aging and type of silica, aiming to establish the relationship between product size and morphology with the modifications made. The crystallization temperature showed to be a prime factor with respect to particle size and crystallites. Dilution of the synthesis gel (50% w / w) provided a reduction in the crystallite aggregation and the variation of the water content in the synthesis implied changes in zeolitization rates. The sodium content modified the growth of the crystals and the increase of intergrowths and aggregations of particles. Changes in the silica source increased the growth rate of the crystals and contributed to changes in their size. Larger crystals were obtained from systems with higher concentrations of sodium cations as nanocrystallite aggregates. Aggregates of small pure mordenite crystallites of up to about 50 nm were obtained with syntheses performed at 150 ? C and with the dilution of the already prepared gel. Lower sodium and water content and the use of silica sources with a greater specific area (relative to this type of material) also tend to result in smaller crystallites. Opposite conditions enabled the highest growth, generating crystals up to 1 ?m on average. The results showed that it is possible to exert some control over the particle size and crystallites of the mordenite zeolite by adjusting parameters inherent to the conventional synthesis system.

Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2017-01-10T12:38:21Z No. of bitstreams: 1 BrunaMariaEmerencianoDasChagas_TESE.pdf: 6590840 bytes, checksum: f29703c72f7b97886bfe14570fa8d656 (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2017-01-11T13:13:01Z (GMT) No. of bitstreams: 1 BrunaMariaEmerencianoDasChagas_TESE.pdf: 6590840 bytes, checksum: f29703c72f7b97886bfe14570fa8d656 (MD5) / Made available in DSpace on 2017-01-11T13:13:01Z (GMT). No. of bitstreams: 1 BrunaMariaEmerencianoDasChagas_TESE.pdf: 6590840 bytes, checksum: f29703c72f7b97886bfe14570fa8d656 (MD5) Previous issue date: 2016-06-09 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior (CAPES) / Recentemente as microalgas e cianobact?rias vem sendo muito estudadas como fonte de biocombust?veis devido a sua elevada produtividade, elevado teor de ?leo e capacidade de crescer em uma grande variedade de climas e terras sem competir com a produ??o de alimentos. A pir?lise ? um m?todo de convers?o termoqu?mica eficaz capaz de converter biomassa em bio-?leo, carv?o e gases combust?veis. O bio-?leo ? uma mistura l?quida de compostos org?nicos potencial para substituir o ?leo diesel. Tem sido demosntrado que bio-?leos de microalgas e cianobact?rias s?o mais est?veis, apresentam teor de oxig?nio mais baixo e poder calor?fico mais alto que bio-?leos de biomassa lignocelul?sica, embora contenha um alto teor de nitrog?nio devido a presen?a de prote?nas na mat?ria-prima. A Spirulina ? uma cianobact?ria que vem sendo muito estudada nos processos de degrada??o t?rmica por apresentar alto teor de prote?nas (74%) e baixo teor de lip?dios (< 1%) podendo ser totalmente convertida em biocombust?vel. Nesta tese, foi investigado o potencial de produ??o de combust?veis e qu?micos a partir da pir?lise r?pida de Spirulina. Os experimentos de pir?lise r?pida convencional em Py-GC/MS foram conduzidos para investigar a influ?ncia dos par?metros de pir?lise, tais como temperatura, taxa de aquecimento e tempo de resid?ncia nos rendimentos dos produtos. O rendimento dos produtos da pir?lise foi maximizado a 450 ?C e 30 s, independente da taxa de aquecimento. Essas condi??es foram escolhidas para o estudo da pir?lise catal?tica com 9 ze?litas diferentes para avaliar a produ??o de hidrocarbonetos espec?ficos, compostos oxigenados e nitrogenados em func?o da raz?o biomassa/catalisador. O rendimento de hidrocarbonetos arom?ticos aumentou ? medida que a propor??o de catalisador/biomassa aumentou de 1:1 para 10:1. A ze?lita H-ZSM5 (23) apresentou o rendimento m?ximo de hidrocarbonetos e a maior redu??o de f?nois quando comparada as outras ze?litas, por?m os compostos nitrogenados totais n?o foram significativamente reduzidos por nenhum catalisador testado. Posteriormente testes de pir?lise r?pida de Spirulina foram conduzidos em um reator de leito fluidizado da USDA-ARS sob diferentes atmosferas de rea??o. Foram testadas a pir?lise convencional com atmosfera inerte (N2) e um processo de pir?lise com atmosfera reativa compostas por gases reciclados da pi?lise, denominado ?Tail Gas Reactive Pyrolysis? (TGRP). O bio-?leo, carv?o e gases produzidos pelo processo TGRP tiveram suas caracter?sticas melhoradas em rela??o aos produtos obtidos na pir?lise convencional, houve um aumento na concentra??o dos hidrocarbonetos arom?ticos e predominaram compostos nitrogenados com um ?nico ?tomo de nitrog?nio (piridinas, pirroles, indoles, nitrilas e amidas). Devido a esta composi??o, esse bio-?leo apresentou um n?vel suficientemente elevado de estabilidade t?rmica para ser destilado. Al?m disso, o bio-?leo produzido pelo processo TGRP foi mais est?vel, menos ?cido e apresentou um poder calor?fico mais alto que bio-?leos de biomassa lignocelul?sica. / Recently microalgae and cyanobacteria have been widely studied as a source of biofuels due to its high yield, high oil content and ability to grow on a wide variety of climates and land without competing with food production. Pyrolysis is an effective thermochemical conversion method capable of converting biomass to fuels, including bio-oil, bio-char and gas. Bio-oil is a liquid mixture of organic compounds that can be a source of valuable chemicals and potential to replace diesel oil depending on its quality. It has been shown that bio-oil from microalgae and other proteinaceous biomass are more stable, have a low oxygen content and higher calorific value than those produced from lignocellulosic feedstock, though contains high nitrogen content due to the presence of protein in its constitution. Spirulina is a cyanobacteria that has been studied in the thermal degradation processes due to its high protein and low lipids content. In this thesis, we investigated the potential for production of fuels and chemicals from the fast pyrolysis of Spirulina. Conventional fast pyrolysis experiments in Py-GC/MS were performed to investigate the influence of pyrolysis parameters such as temperature, heating rate and residence time in distribution of products. The pyrolysis yield was maximized at 450 ?C and 30 s, regardless of heating rate. H-ZSM5 (23) showed the maximum hydrocarbon yield and the largest phenols reduction when compared to the other zeolites, but the total nitrogenated compounds were not significantly reduced by any catalyst tested although some specific nitrogenous have been reduced or eliminated. H-? (38) was also able to increase aromatics production, although its effect was less significant when compared to H-ZSM5 (23) and (50). Subsequently tests of Spirulina fast pyrolysis were conducted in USDA?s bubbling fluidized bed pyrolysis reactor under different reaction atmospheres. Conventional (N2 atmosphere) and reactive (Tail Gas Reactive Pyrolysis - TGRP) pyrolysis were tested. Biooil, bio-char and gas obtained from TGRP process had their fuel characteristics improved when compared to the products from conventional pyrolysis. TGRP Spirulina pyrolysis oil showed an increased concentration of aromatics hydrocarbon and the presence of nitrogenous compounds with single nitrogen atom (pyridines, pyrroles, indoles, nitriles and amides), low oxygen content and low acidity being thermally stable therefore a good feedstock for distillation process. Distillation successfully allowed concentrating various chemicals into distillate fractions which, in turn, could be individually isolated for processing to fuels or chemical co-products.

Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2017-01-27T12:21:52Z No. of bitstreams: 1 MarcilioDosSantosTavares_TESE.pdf: 4345486 bytes, checksum: 8f84f78e0923aad2b8781e75eb8573ea (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2017-01-30T12:18:04Z (GMT) No. of bitstreams: 1 MarcilioDosSantosTavares_TESE.pdf: 4345486 bytes, checksum: 8f84f78e0923aad2b8781e75eb8573ea (MD5) / Made available in DSpace on 2017-01-30T12:18:04Z (GMT). No. of bitstreams: 1 MarcilioDosSantosTavares_TESE.pdf: 4345486 bytes, checksum: 8f84f78e0923aad2b8781e75eb8573ea (MD5) Previous issue date: 2016-07-29 / O conhecimento da composi??o do petr?leo e seus produtos ? uma necessidade imprescind?vel numa refinaria para o ajuste das condi??es do processo. Desta forma a otimiza??o do refino de petr?leo ? fundamental para a predi??o da distribui??o dos produtos e sua qualidade. Realizar o estudo cin?tico da degrada??o t?rmica e catal?tica na presen?a da ze?lita H ?Beta e avaliar os produtos obtidos por PY - CG/ MS de petr?leo leve foi o objetivo principal deste trabalho. Contudo, foram feitas correla??es de dados obtidos atrav?s da destila??o Simulada por Cromatografia a G?s (SIMDIST), da an?lise termogravim?trica (TG/DTG) e da pir?lise acoplada a um espectr?metro de massas (GC/MS), para auxiliar nas an?lises dos dados obtidos. Atrav?s da t?cnica de Fluoresc?ncia de Raios X por Energia Dispersiva (EDX), seguindo o m?todo ASTM D4294 foi poss?vel determinar o teor de enxofre contido na amostra. A termogravimetria (TG/DTG) apresentou tr?s etapas de perdas de massa, onde a primeira etapa est? relacionada ? remo??o de hidrocarbonetos e compostos org?nicos leves. Na segunda etapa ocorre a decomposi??o de arom?ticos de alta massa molecular. E na terceira etapa, ocorreu a degrada??o de coque. Atrav?s da t?cnica de PY ? GC/MS foram detectados os produtos de degrada??o da amostra de petr?leo nas temperaturas de 250?C, 350?C e 450?C, com e sem a presen?a da ze?lita H-Beta. A degrada??o t?rmica e catal?tica da amostra de petr?leo leve foi realizada da temperatura ambiente at? 900?C, nas raz?es de aquecimento de 5, 10 e 20oC min-1. As curvas geradas pela TG/DTG apresentaram uma degrada??o mais acelerada na amostra de petr?leo sem catalisador H-Beta. Esses resultados foram ratificados pela energia de ativa??o, calculada atrav?s do m?todo cin?tico ? Livre (Vyazovkin modelfree Kinetic), em que a presen?a do catalisador reduziu a energia, em especial na faixa de craqueamento, mostrando a efici?ncia do processo, principalmente para a obten??o de materiais leves da composi??o da amostra de petr?leo leve, como diesel e gasolina. / Knowledge of the oil composition and its products is an absolute necessity in a refinery for adjusting the process conditions. Thus the optimization of petroleum refining is essential for predicting the distribution of products and their quality. Perform the kinetic study of the thermal and catalytic degradation in the presence of zeolite H -Beta and evaluate the products obtained by PY-GC/MS of light oil was the main objective of this work. However, data correlations were made obtained by Simulated Distillation by Gas Chromatography (SIMDIST), the thermal gravimetric analysis (TG / DTG) and pyrolysis coupled to a mass spectrometer (GC/MS), to assist in the analysis of data. Through Fluorescence technique of X-ray energy dispersive (EDX) following the ASTM D4294 method it was possible to determine the sulfur content in the sample. Thermogravimetry (TG/DTG) showed three-step weight loss, where the first stage relates to the removal of light hydrocarbons and organic compounds. The second step is decomposition of aromatic high molecular weight. And the third stage was the degradation of coke. Through the technique PY-GC/MS were detected degradation products of the oil sample at temperatures of 250?C, 350?C and 450?C, with and without the presence of zeolite H-Beta. The thermal and catalytic degradation of light oil sample was carried out from room temperature to 900C, the heating rates of 5, 10 and 20 ? C min-1. The curves generated by TG/DTG showed a faster degradation in the sample oil without H-Beta catalyst. These results were confirmed by activation energy calculated using the kinetic method - Free (Vyazovkin modelfree Kinetic) in the presence of the catalyst decreased energy, in particular in cracking band, showing the process efficiency, particularly for obtaining lightweight materials of light oil sample composition, such as diesel and gasoline.

Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2017-02-17T18:43:03Z No. of bitstreams: 1 LindianeBieseki_TESE.pdf: 5268310 bytes, checksum: 259162ecc5d58cc1ee42eb6746ffdb22 (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2017-02-17T20:42:31Z (GMT) No. of bitstreams: 1 LindianeBieseki_TESE.pdf: 5268310 bytes, checksum: 259162ecc5d58cc1ee42eb6746ffdb22 (MD5) / Made available in DSpace on 2017-02-17T20:42:31Z (GMT). No. of bitstreams: 1 LindianeBieseki_TESE.pdf: 5268310 bytes, checksum: 259162ecc5d58cc1ee42eb6746ffdb22 (MD5) Previous issue date: 2016-06-17 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior (CAPES) / As ze?litas s?o uma classe de peneiras moleculares de estrutura cristalina e podem apresentar diferentes composi??es pela substitui??o de Si por outro elemento. No caso dos silicogermanatos, ?tomos de Si s?o substitu?dos por Ge na rede estrutural e s?o classificados como zeotipos. Neste estudo s?o apresentados resultados referentes a s?ntese de silicogermanatos zeol?ticos utilizando tr?s diferentes estrat?gias. Uma destas, ? a utiliza??o de compostos org?nicos que possam atuar como direcionadores de estrutura. No presente estudo foram utilizados 3 compostos diferentes com rela??o C/N+ de 6, 15 e 13, sendo dois compostos de uso in?dito em s?ntese de ze?litas. Os compostos foram avaliados em rela??o a resist?ncia a troca i?nica e em s?ntese de ze?litas utilizando diferentes composi??es, que incluem principalmente o uso de Sil?cio e Germ?nio e alguns testes com Boro. Algumas s?nteses foram realizadas em meio b?sico e outras em meio fluor?drico. Para caracteriza??o dos compostos org?nicos foram usadas as t?cnicas de Resson?ncia Magn?tica Nuclear (RMN), Espectroscopia na regi?o do Infravermelho (IV) e An?lise Qu?mica por CHN. Tamb?m foram realizados experimentos combinado o uso de um direcionador org?nico e um inorg?nico, neste caso LiOH. Os produtos de s?ntese de ze?litas foram caracterizados por Difra??o de raios-X (DRX), An?lise Termogravim?trica (TG), An?lise Qu?mica por CHN, an?lise qu?mica por Espectrometria de Emiss?o At?mica por Plasma Acoplado Indutivamente (ICP-AES), Espectroscopia na regi?o do Infravermelho (IV), Microscopia Eletr?nica de Varredura (MEV) e An?lise Qu?mica por Espectroscopia por Dispers?o de Energia (EDS). Com o uso do composto Iodeto de N,N,N-trimetil-2-adamantam?nio ? (3SDA(I)1), j? utilizado em s?ntese de ze?litas, foi sintetizado um silicogermanato com estrutura do tipo STT. / Zeolites are one class of molecular sieves with cristalline structure and may have different compositions for the replacement of Si by another element. In the case of silicogermanates, Si atoms were replaced by Ge in the structural network and are denominated zeotypes. In this study, results were obtained of the silicogermanate zeolites synthesis using different strategies. One of these is the use of organic compounds that can act as structure direct agent. In the present study, it was used three different compounds with C/N+ = 6, 15 and 13; being two of these novel compounds for use in zeolite synthesis. The compounds were evaluated for resistance to ion exchange and in zeolites synthesis using different compositions that primarily include the use of silicon and germanium and boron in some tests. Some syntheses were carried out in basic medium and others in the hydrofluoric medium. For characterization of organic compounds were used the Nuclear Magnetic Resonance techniques (NMR), Infrared spectroscopy (IR) and chemical analysis for CHN. Some procedures were also performed with the combined use of an organic and an inorganic driver, in this case LiOH. The zeolites synthesis products were characterized by Diffraction X-ray (XRD), Thermogravimetry analysis (TGA), chemical analysis by CHN, chemical analysis by Inductively plasma atomic emission spectroscopy (ICP-AES), Infrared Spectroscopy (IR) and Scanning electron microscope (SEM) and Energy Dispersive Spectroscopy (EDS). With the use of the N,N,N-Trimethyl-2-adamantammonium iodide - (3SDA(I)1), known in zeolite synthesis, it was possible to synthesize a silicogermanate with STT type structure.

Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2017-02-20T21:21:26Z No. of bitstreams: 1 ManuelaSilvaMartinsDeOliveira_DISSERT.pdf: 4629063 bytes, checksum: 9e9e1aef7dcd4aa2529d87a665e32ac6 (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2017-02-23T20:56:18Z (GMT) No. of bitstreams: 1 ManuelaSilvaMartinsDeOliveira_DISSERT.pdf: 4629063 bytes, checksum: 9e9e1aef7dcd4aa2529d87a665e32ac6 (MD5) / Made available in DSpace on 2017-02-23T20:56:18Z (GMT). No. of bitstreams: 1 ManuelaSilvaMartinsDeOliveira_DISSERT.pdf: 4629063 bytes, checksum: 9e9e1aef7dcd4aa2529d87a665e32ac6 (MD5) Previous issue date: 2016-08-05 / Conselho Nacional de Desenvolvimento Cient?fico e Tecnol?gico (CNPq) / O l?tio ? um dos elementos que apresentam um elevado interesse comercial, justamente devido as suas caracter?sticas que possibilitam a utiliza??o em baterias de ?on l?tio, medicamentos, ligas, dentre outras aplica??es. Sua diversificada aplicabilidade aliada ?s dificuldades de obten??o faz com que esse material tenha um alto valor comercial. Um dos principais minerais de onde pode-se extrair l?tio ? o Espodum?nio. Industrialmente, o principal processo de obten??o do l?tio do espodum?nio ? a extra??o via ?cido sulf?rico. Tal processo gera como subproduto uma grande quantidade de res?duo s?lico-aluminoso que n?o possui destino final, sendo em sua maioria armazenados em aterros ou deixados ao ar livre. Foram estudados neste trabalho, diferentes procedimentos de s?ntese buscando diferentes estruturas zeol?ticas como uma maneira de agregar valor a este res?duo industrial. Seguiu-se como base a receita tradicional de cada estrutura fornecida pela ?International Zeolite Association? (IZA) modificando-a com a adi??o do res?duo s?lico-aluminoso. Os materiais sintetizados foram caracterizados atrav?s de difra??o de raios-X e microscopia eletr?nica de varredura (MEV). Foi poss?vel sintetizar ze?litas MER, EDI e MOR com alta cristalinidade e fase ?nica, sendo a primeira vez em que estas estruturas s?o obtidas atrav?s do res?duo s?lico-aluminoso proveniente da extra??o do l?tio do mineral espodum?nio. Outros materiais, tais como ze?lita LTA, foram obtidos, mas com pouca cristalinidade ou com mais de uma fase presente. Estudos complementares de otimiza??o desta s?ntese se fazem necess?rios. / Lithium is one of the elements that have a high commercial interest, precisely because of its features that allow use in lithium ion batteries, medicines, alloys, among other applications. Its diverse applicability allied to obtain difficulties makes this material has a high commercial value. One of the major minerals which can extract lithium is spodumene. Industrially, the main process of obtaining the spodumene lithium is extracted via sulfuric acid. This process generates as a byproduct a lot of silico-aluminous waste that has no final destination, being mostly stored in landfills or left outdoors. They were studied in this work, different synthetic procedures seeking different zeolite structures as a way to add value to this industrial waste. This was followed based on the traditional recipe of each structure provided by the "International Zeolite Association" (IZA) modifying it with the addition of silica-alumina residue. The synthesized materials were characterized by X-ray diffraction and scanning electron microscopy (SEM). It was possible to synthesize zeolites MER, EDI and MOR with high crystallinity and single phase, the first being that these structures are obtained by silico-aluminous waste from the extraction of the mineral spodumene lithium. Other materials, such as LTA zeolite, were obtained, but with low crystallinity or with more than one phase present. Further optimization studies are needed.

Submitted by Celso Magalhaes (celsomagalhaes@ufrrj.br) on 2017-06-09T13:11:00Z No. of bitstreams: 1 2016 - Glenda Cristina da Silva Lopes.pdf: 3117864 bytes, checksum: 398fb3e84e1b16247f7cc7afb1069541 (MD5) / Made available in DSpace on 2017-06-09T13:11:00Z (GMT). No. of bitstreams: 1 2016 - Glenda Cristina da Silva Lopes.pdf: 3117864 bytes, checksum: 398fb3e84e1b16247f7cc7afb1069541 (MD5) Previous issue date: 2016-08-26 / Funda??o de Apoio a Pesquisa Cient?fica e Tecnol?gica da UFRRJ-FAPUR / In the present dissertation it was conduced the study of the mesoporous mordenite production by the direct synthesis using hydrothermal media or dry gel convertion. Activated charcoal, starch, carboxymethylcellulose and carbon black were used as mesoporosity templating. To evaluate the effect of these templates, samples were prepared with molar composition of 20 SiO2: 1 Al2O3: 6 Na2O: 600 H2O, by hydrothermal synthesis and 20 SiO2: 1 Al2O3: 4 Na2O, by dry synthesis, following procedures described in the literature and adding different amounts of templates to the synthesis gel. As reagents for the synthesis gel assay, were utilized sodium hydroxide, sodium aluminate, silica (Aerosil 200) and deionized water. The synthesis temperature was 175 ? C, while the synthesis time was 5 days and 3 days for the hydrothermal and dry method, respectively. For characterization of the samples was used X-ray diffraction (XRD), analysis by nitrogen adsorption/desorption measurements and determination of the acidity by temperature programmed desorption of ammonia (NH3-TPD). An evaluation of the samples was carried out using the n-heptane cracking reaction at 380 ? C. By X-ray diffraction, it was observed that the majority of the experiments formated of mordenite phase. The textural properties, particularly the volume of mesopores, improved in most samples synthesized in the presence of the template, however, the values obtained were lower than those defined in the literature for mesoporous materials. The samples showed only a peak of ammonia adsorption in NH3-TPD profiles, related to weak acid sites. Most samples synthesized in the presence of drivers showed an increase in the conversion of n-heptane, while the samples obtained by dry gel convertion showed higher conversion than the hydrothermally synthesized. / No presente trabalho foi realizado o estudo da produ??o de mordenita mesoporosa a partir da s?ntese direta, em meio hidrot?rmico e seco, na presen?a do carv?o ativado, amido, carboximetilcelulose e negro de fumo como direcionadores de mesoporosidade. Para avaliar o efeito desses direcionadores, foram preparadas amostras com composi??o molar de 20 SiO2: 1 Al2O3: 6 Na2O: 600 H2O, pela s?ntese hidrot?rmica e 20 SiO2: 1 Al2O3: 4 Na2O, pela s?ntese seca, seguindo os procedimentos descritos na literatura e adicionando quantidades diferentes dos direcionadores ao gel de s?ntese. Como reagentes para o gel de s?ntese, foram utilizados hidr?xido de s?dio, aluminato de s?dio, s?lica (aerosil 200) e ?gua deionizada. A temperatura de s?ntese foi de 175 ?C, enquanto o tempo de s?ntese foi de 5 dias e 3 dias, para o m?todo hidrot?rmico e seco, respectivamente. Para caracteriza??o das amostras usou-se difra??o de raios X (DRX), an?lise textural por medidas de adsor??o/dessor??o de nitrog?nio e determina??o da acidez por dessor??o de am?nia ? temperatura programada (TPD-NH3). Realizou-se a avalia??o catal?tica das amostras atrav?s da rea??o de craqueamento de n-heptano a 380 ?C. Pelos difratogramas de raios X, foi observado que na maioria dos experimentos ocorreu a forma??o da mordenita. As propriedades texturais, especialmente o volume de mesoporos, melhoraram na maioria das amostras sintetizadas na presen?a do direcionador, por?m, os valores obtidos foram inferiores aos definidos pela literatura para materiais mesoporosos. As amostras apresentaram apenas um pico de adsor??o de am?nia nos perfis de TPD-NH3, referentes aos s?tios ?cidos fracos. A maioria das amostras sintetizadas na presen?a dos direcionadores apresentou aumento na convers?o do n-heptano, sendo que as amostras obtidas por s?ntese em meio seco apresentaram maior convers?o do que as sintetizadas em meio hidrot?rmico.