Síntese e caracterização de materiais nanoporosos para pirólise catalítica de óleos pesados

The present work reports the study of nanoporous structures, aiming at their use in research directed to the current demand of the petroleum industry to value heavy oil. Initially, two ways were chosen for the synthesis of porous structures from the molecular sieves of type Si-MCM-41. In the first way, the structure MCM-41 is precursory for heteroatom substitutes of silicon, generating catalyst of the type Al-MCM-41 from two different methods of incorporation of the metal. This variation of the incorporation method of Aluminum in the structure of Si-MCM-41 was carried out through the conventional procedure, where the aluminum source was incorporated to the gel of synthesis, and the procedure post-synthesis, where the Aluminum source was incorporated in catalyst after the synthesis of Si-MCM-41. In the second way, the MCM-41 acts as a support for growth of nanocrystals of zeolite embedded in their mesoporous, resulting in hybrid MCM-41/ZSM-5 catalyst. A comparative analysis was carried through characterizations by XRD, FTIR, measures of acidity through n-butylamine adsorption for TGA, SEM-XRF and N2 adsorption. Also crystalline aluminosilicate with zeolitic structure MFI of type ZSM-5 was synthesized without using organic templates. Methodologies to the preparation of these materials are related by literature using conventionally reactants that supply oxides of necessary silicon and aluminum, as well as a template agent, and in some cases co-template. The search for new routes of preparation for the ZSM-5 aimed at, above all, the optimization of the same as for the time and the temperature of synthesis, and mainly the elimination of the use of organic templates, that are material of high cost and generally very toxic. The current study is based on the use of the H2O and Na+ cations playing the role of structural template and charge compensation in the structure. Characterizations by XRD, FTIR, SEM-XRF and N2 adsorption were also conducted for this material in order to compare the samples of ZSM-5 synthesized in the absence of template and those used industrially and synthesized using structuring

Utilização de rejeitos de Caulins na Síntese de Zeólita A

Three studies were performed using tailings kaolin for the synthesis of zeolite A. The first synthesis of zeolite A was performed using a kaolin waste generated from the beneficiation of kaolin for paper production process was studied. The kaolin waste was thermally activated at a temperature range of 550-800°C. For comparison was performed a synthesis pattern of Zeolite A(procedure IZA). The prepared materials were characterized by 27Al MAS NMR, X-ray diffraction and scanning electron microscopy with microprobe rays. The pre-tramento proved to be the most appropriate and suitable temperatures are between 600 and 700°C. Observed the formation of zeolite A in all materials, reaching 52% crystallinity, and the presence of phase sodalite and amorphous material. The second study was the use of a highly reactive metakaolin originating from the Jari region in the synthesis of zeolite A by a new method of hydrothermal synthesis. The zeolite is obtained pure and highly crystalline employing the Jari kaolin calcined at 600 ° C for 2h when the transformation to metakaolin occurs. Get to zeolite phase A at 4pm. The best crystallization time was of 24 h afforded a crystallinity of 67.9%. The third study was the evaluation of the NaOH / metakaolin and crystallization time on the synthesis of zeolite NaA from a sample of kaolin waste, named Kaolin Coverage. The experiments were performed using statistical design (axial points) and rejoinder the center point. The samples were characterized by X-ray diffraction (XRD), scanning microscopic analysis and chemical analysis using an EPMA microprobe. The results showed that a relationship exists between the amount of NaOH added and the crystallization time. The experiment performed using the lowest ratio NaOH / metakaolin (0.5) and shorter (4 h) produced an amorphous material. The increase ratio of NaOH / metakaolin and crystallization time leads to formation of a more crystalline NaA phase, but the presence of phase with sodalite as impurities

Síntese e caracterização de argilas pilarizadas com pilares mistos Al/Co

Two pillaring methods were tested to synthesize pillared clays containing mixed Al/Co pillars. Using the first method, based on the traditional procedure, were obtained materials containing different Co concentrations: 10, 25, 50, 75 and 100 % of Co in the pillaring solution. Just the experiments with low concentrations (10 and 25 % of Co) has formed pillared clays, whereas the sample with 25 % of cobalt showed best results compared with the one obtained just using Al as pillaring agent (basal spacing higher than 18 Å and surface area bigger than 300 m²/g). The 27Al NMR results pointed out the formation of mixed Al/Co pillars due to decreased between the intensities of AlVI/AlIV signals, indicating that the AlIV content decreased while Co content increased, suggesting the isomorphic substitution of Al atoms for Co in the Keggin ion structure (pillaring agent). For the samples containing 75 and 100 % of cobalt, it was verified the formation of others materials, which could be identified as hydrotalcite like compounds. The second pillarization method was named mixed layers, because the objective was to intercalate clay layers with hydrotalcite layers. Thus, after calcination, the hydrotalcite layers would dehydroxylate, resulting just in the metals oxides, intercalated between the clay sheets, thus generating, a pillared clay. For this purpose, were tested 4 synthesis procedures: physical mixture, mixture in water, ionic exchange under reflux and in situ synthesis. Of these, the method which showed the best results was the in situ synthesis, in which basal spacings of 14 Å (after calcination) were obtained, indicating that the samples are intercalated with metal oxides (Mg and Al). This procedure was reproduced with a Co-Al LDH (layered double hydroxide) and similar results were obtained, testifying the method reproducibility

Síntese de catalisadores nanoporosos na ausência total e parcial de direcionadores orgânicos para pirólise catalítica de óleos pesados e intermediários

The processing of heavy oil produced in Brazil is an emergency action and a strategic plan to obtain self-sufficiency and economic surpluses. Seen in these terms, it is indispensable to invest in research to obtain new catalysts for obtaining light fraction of hydrocarbons from heavy fractions of petroleum. This dissertation for the degree of Doctor of Philosophy reports the materials preparation that combine the high catalytic activity of zeolites with the greater accessibility of the mesoporosity, more particularly the HZSM-5/MCM-41 hybrid, done by synthesis processes with less environmental impact than conventional ones. Innovative methodologies were developed for the synthesis of micro-mesoporous hybrid material by dual templating mechanism and from crystalline zeolitic aluminosilicate in the absence of organic template. The synthesis of hybrid with pore bimodal distribution took place from one-single organic directing agent aimed to eliminate the use of organic templates, acids of any kind or organic solvents like templating agent of crystalline zeolitic aluminosilicate together with temperature-programmed microwave-assisted, making the experimental procedures of preparation most practical and easy, with good reproducibility and low cost. The study about crystalline zeolitic aluminosilicate in the absence of organic template, especially MFI type, is based on use of H2O and Na+ cation playing a structural directing role in place of an organic template. Advanced characterization techniques such as X-Ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), Scanning Electron Microscopy (SEM), Highresolution Transmission Electron Microscopy (HRTEM), Adsorption of N2 and CO2, kinetic studies by Thermogravimetric Analysis (TGA) and Pyrolysis coupled to Gas Chromatography/Mass Spectrometry (Pyrolysis-GC/MS) were employed in order to evaluate the synthesized materials. Achieve the proposed objectives, has made available a set of new methodologies for the synthesis of zeolite and hybrid micro-mesoporous material, these suitable for catalytic pyrolysis of heavy oils aimed at producing light fraction

Estudo integrado do potencial fitorremediador da Eichhornia crassipes em ambientes naturais e sua utilização para obtenção de extratos proteicos

This study aimed to analyze the phytoremediation potential of Eichhornia crassipes in natural environments, optimize the extraction process of crude protein from plant tissue and, obtain and characterize this process in order to determine its viability of use instead of the protein sources of animal and/or human feed. For this, it has been determined in Apodi/Mossoró river water the concentration of ammonium ions, nitrite, nitrate, calcium, magnesium, potassium, iron, copper, manganese, zinc, nickel, cobalt, sodium, aluminum, cádmium, lead, and total chromium; It was determined in plant tissue of aquatic macrophytes of Eichhornia crassipes species present in Apodi/Mossoró River the moisture content, ash, calcium, magnesium, potassium, iron, copper, manganese, zinc, nickel, cobalt, sodium, aluminum, cadmium, lead, total chromium, total nitrogen and crude protein. It was also determined the translocation factor and bioaccumulation of all the quantified elements; It was developed and optimized the extraction procedure of crude protein based on the isoelectric method and a factorial design 24 with repetition; It was extracted and characterized the extract obtained by determining the moisture content, ash, magnesium, potassium, iron, copper, manganese, zinc, nickel, cobalt, sodium, cadmium, total nitrogen and crude protein. And finally, it was also characterized the protein extract using Thermogravimetric Analysis (TG), Derived Thermogravimetric (DTG), Differential Scanning Calorimetry (DSC), Infrared Spectroscopy (FT-IR) and jelly-like electrophoresis of polyacrylamide (SDS -PAGE) to assess the their molecular weights/mass. Thus, from the results obtained for the translocation and bioaccumulation factors was found that the same can be used as phytoremediation agent in natural environments of all quantified elements. It was also found that the developed method of extraction and protein precipitation was satisfactory for the purpose of the work, which gave the best conditions of extraction and precipitation of proteins as: pH extraction equal to 13.0, extraction temperature equals 60 ° C, reaction time equals to 30 minutes, and pH precipitation equals to 4.0. As for the extract obtained, the total nitrogen and crude protein were quantified higher than those found in the plant, increasing the crude protein content approximately 116.88% in relation to the quantified contente in the vegetal tissue of macrophyte. The levels of nickel and cadmium were the unique that were found below the detection limit of used the equipment. The electrophoretic analysis allowed us to observe that the protein extract obtained is composed of low polypeptide chains by the molecular and phytochelatins, with 6 and 15 kDa bands. Analysis of TG, DTG, DSC and FT-IR showed similarities in protein content of the obtained extracts based on different collection points and 9 parts of the plant under study, as well as commercial soy protein and casein. Finally, based on all these findings, it was concluded that the obtained extract in this work can be used instead of the protein sources of animal feed should, before that, test its digestibility. As human supplementation, it is necessary to conduct more tests associated with the optimization process in the sense of removing undesirable components and constant monitoring of the water body and the raw material used

Aplicabilidade da voltametria de pulso diferencial na quantificação de ácido fólico e ácido oxálico: um método comparativo

The development of more selective and sensitive analytical methods is of great importance in different areas of knowledge, covering, for example, food, biotechnological, environmental and pharmaceutical sectors. The study aimed to employ the technique electroanalytical differential pulse voltammetry (DPV) as an innovative and promising alternative for identification and quantification of organic compounds. The organic compounds were investigated in this study oxalic acid (OA) and folic acid (FA). The electrochemical oxidation of oxalic acid has been extensively studied as a model reaction in the boundary between the organic and inorganic electrochemistry. Since the AF, an essential vitamin for cell multiplication in all tissues, which is essential for DNA synthesis. The AF has been investigated using analytical techniques, liquid chromatography and molecular absorption spectrophotometry. The results obtained during the experimental procedure indicated that the process of electrochemical oxidation of oxalic acid is strongly dependent on the nature of the anode material and the oxidation mechanism, which affects their detection. Efficient removal was observed in Ti/PbO2 anodes, graphite, BDD and Pt 90, 85, 80 and 78% respectively. It was also shown that the DPV employing glassy carbon electrode offers a fast, simple, reliable and economical way to determine the AO during the process of electrochemical oxidation. Furthermore, electroanalytical methods are more expensive than commonly used chromatographic analysis and other instrumental methods involving toxic reagents and higher cost. Compared with the classical method of titration and DPV could be a good fit, confidence intervals and detection limits confirming the applicability of electroanalytical technique for monitoring the degradation of oxalic acid. For the study of AF was investigated the electrocatalytic activity of the carbon paste electrode for identification and quantification in pharmaceutical formulations by applying the DPV. The results obtained during the experimental procedure showed an irreversible oxidation peak at 9.1 V characteristic of FA. The carbon paste sensor showed low detection limit of 5.683×10−8 mol L-1 reducing matrix effects. The spectrophotometric analysis showed lower concentrations of HF compared with those obtained by HPLC and DPV. The levels of AF were obtained according to the methodology proposed by the Brazilian Pharmacopoeia. The electroanalytical method (DPV) proposed is cheaper than GC analysis commonly used by the pharmaceutical industry. The results demonstrated the potential of these electroanalytical techniques for future applications in environmental, chemical and biological sensors

Qualidade de vida de pacientes com deformidade dentofacial

In the last decade, an increasing number of studies focusing on the impact of oral deformities on quality of life have been published. However, the evaluation of patients at different phases of the treatment has not been performed. Therefore, the purpose of this study was to determine the impact that dentofacial deformities have on patients` quality of life, as well as the influence exerted by social, economic, demographic and orthodontic factors, type and severity of malocclusion. A bicentric study - of the cross-sectional type of repeated panels - involving two cities - Natal and Rio de Janeiro - was carried out. A total of 227 patients participated in the study: 71 patients in the initial phase of the treatment (before any orthosurgical procedure), 115 patients in the pre-surgical (with braces) phase and 41 patients in the postoperative phase. The quality of life was measured using the Orthognatic Quality of Life Questionnnaire - OQLQ, translated and validated into Portuguese. The normative and aesthetic need for treatment was assessed with the Index of Orthodontic Treatment Need (IOTN) and the Dental Aesthetic Index (DAI); the social, economic and demographic factors, the type of service and malocclusion were also assessed. The data were analyzed through χ2/ Fisher`s exact test to seek the association between the nominal categorical variables in the three phases of treatment, Mann Whitney and Kruskal-Wallis test for gauging the existence of significant differences between two and three groups regarding each domain of OQLQ, respectively. For all tests, it was adopted a significance level of 5%. There was a statistically significant difference (p <0.001) in the general scores of OQLQ and in the domains of social aspects, facial aesthetics and oral function, when the "postoperative group" was compared to the "initial" and "orthodontic preparation" groups. Women, single, aged between 31 and 59 and living in Natal had the greatest impact on quality of life among patients in the "orthodontic preparation" group. Only the variable "income" (2 to 3 minimum wages), for the "initial" group, and gender (female) for the "postoperative" group, showed significant association with quality of life. The normative variable IOTN (DHC and AC) showed significant association with the OQLQ for the "initial" group, and the IOTN-AC-auto in the group of orthodontic preparation, being less important to women. We conclude that the ortho-surgical therapy has positive effects on quality of life after orthognathic surgery

Satisfaçã dos Usuários e a qualidade da atenção primária à saúde no Rio Grande do Norte

O presente estudo tem por objetivo avaliar a satisfação dos usuários em relação à qualidade da Atenção Primária à Saúde no Rio Grande do Norte. Trata-se de Pesquisa Avaliativa observacional transversal, com abordagem quantitativa, a qual faz parte da Avaliação Externa do Programa de Melhoria do Acesso e da Qualidade da Atenção Básica (PMAQ), da Universidade Federal do Rio Grande do Norte. Foram utilizados dados secundários de todas as entrevistas com usuários das equipes que participaram da Avaliação Externa do PMAQ no Estado do RN. A pesquisa foi realizada em 167 municípios do Estado do Rio Grande do Norte, na qual a população foi composta por 1.650 usuários. A amostra se deu por conveniência a partir dos seguintes critérios: usuários que estavam presentes na Unidade Básica de Saúde (UBS) para realizar qualquer tipo de procedimento e que consentisse em participar da avaliação. Foram excluídos os que tinham ido pela primeira vez na unidade e aqueles que não frequentaram há mais de 12 meses. A coleta dos dados foi realizada no período de setembro a novembro de 2013. Para tanto, foi elaborado um protocolo de pesquisa contendo as seguintes dimensões: organizacional, interpessoal e estrutural. Em relação à dimensão organizacional os resultados mostram que a marcação de consultas tem se configurado em empecilho ao acesso do usuário ao serviço de saúde, uma vez que se faz necessário para o atendimento, enfrentar filas, antes da abertura da unidade para pegar fichas. No tocante ao funcionamento da unidade, se destaca o fato dos usuários referirem que o horário de funcionamento da unidade atende à suas necessidades, apesar de funcionar 5 (cinco) dias por semana, a maioria das unidades permanece fechada no horário de almoço. Outro dado importante refere-se à coordenação do cuidado, cujos resultados apresentam diferenças maiores entre os usuários da região metropolitana e do interior do Estado em relação à Capital. Essa diferença se expressa principalmente em relação de marcação de consulta com outros profissionais especialistas. A dimensão interpessoal, no que diz respeito à categorias interação usuário-serviço-equipe e vínculo, demonstraram alguns avanços, contudo os melhores resultados foram observados em relação a satisfação com o cuidado, onde mais de 50% dos usuários se mostraram satisfeitos com o cuidado recebido nas unidades. Em contrapartida, o estudo mostrou que, na opinião de 56% dos usuários da capital, a falta de materiais e equipamentos influencia negativamente no cuidado. Por fim, o estudo contribuiu para reforçar a ideia de que a avaliação da satisfação dos usuários dos serviços de saúde pode ser uma ferramenta importante para subsidiar o processo de decisão compartilhada, de forma a se repensar as práticas profissionais, reorganizar o processo de trabalho desenvolvido, realocar recursos, readequar ações e redefinir objetivos que estejam coerentes com o projeto de saúde estabelecido

Avaliação da satisfação das usuárias sobre a atenção à saúde da mulher no Rio Grande do Norte

This work discusses the evaluation of the satisfaction of the users on the women health care focusing on the quality of the primary care in the State of Rio Grande do Norte-BR. The main objective of this research is evaluate the satisfaction of the users about the actions applied to women health in the primary health care in Rio Grande do Norte, observing the information available through the Programa de Melhoria do Acesso e da Qualidade da Atenção Básica (PMAQ-AB). The specific objectives are: the evaluation of aspects related to women health; the evaluation of the specific actions related to welcoming the pregnant and; the evaluation of the information related to the postpartum. This dissertation is characterized as an evaluative research made through a multicentric transversal study, using a quantitative approach, which is part of the External Evaluation of the PMAQ-AB in the State of Rio Grande do Norte, made by the Federal University of Rio Grande do Norte. Some secondary data of the interviews with the users who were in the Basic Health Units were used during the External Evaluation of the PMAQ-AB in Rio Grande do Norte. The sample was collected following these criteria: the users that were in the Basic Health Units to attend to any procedure; they must had used the services for at least one year; and they must had agreed to participate the research. The ones that were attending to the services for the first time and the ones that did not use the services for at least 12 months were excluded from the sample. To the data collection it was used a chart of variables/indicators with the following information to the analysis: Women Health Care, Specific Care of the Pregnant and Information about he postpartum. The descriptive analysis of the data were made through absolute and relative frequencies of the variables using the software Statistic Package for Social Sciences (SPSS) for Windows, version 22.0.0. The results show a positive picture of the satisfaction of the users about the actions of the primary healthcare in women health in the State of the Rio Grande do Norte. Another important analysis is the integration of the primary health care with other points of the Healthcare System aiming to reorient the Model of Healthcare as a starter of the access and quality of the services given to the users. Therefore, the evaluation of the satisfaction of the users in health care is essential among all the agents involved in the process of consolidation of the Unified Health System SUS. Also having the need of rethinking the professional practice, reorganizing the processes of work of the multiprofessional teams in health care, enabling financial resources, inputs and materials, planning and systematizing new actions of healthcare aiming to ensure a perfect health care to the people

Violência Sexual Infanto-Juvenil em Natal: uma avaliação do Programa Sentinela

Analyze the problem of sexual violence suffered by children and adolescents in the city of Natal / Rio Grande do Norte (RN), attended by the Programa Sentinela, a service aimed at combating sexual violence children and teenagers who serves on the council of Natal. Thus aims to review the implementation of the Programa Sentinela in Natal / RN, in the period 2001 to 2006, verifying that the program has contributed to the access of children and adolescents who are victims of abuse and sexual exploitation to fundamental rights under the Statute Children and adolescents (ECA) and the Local Plan and the National gainst Infanto-Youth Sexual Violence. It has a theoretical and methodological approach quantitative and qualitative, covering the issue of sexual violence against children and adolescents, as one of the expressions of economic relationships, gender, race and culture that make up the material and symbolic structure of society. It methodological procedure: review of literature on the subject and conducting interviews with professionals and families of children and adolescent victims of sexual violence. Investigate as the unit of analysis the Sentinel Program. The analysis on the governmental actions of this period on this social problem points to the continuity and little change in the care of victims of sexual violence: despite maintain features and palliative assistencialistas, favoring the "Network of Sexual Tourism", go through some innovations in terms of securing rights from the ECA, which is the need for transparency and democratization in the management of government policies. In research undertaken, Brazil will only be combating this type of crime when each of the social actors are actually doing their share, down taboos, facing corruption and strengthening a system of guarantee of rights, which target children and adolescents are unprotected, and often ignored by Brazilian society

Ganho genético com base no tamanho efetivo populacional de progênies de seringueira

O objetivo deste trabalho foi estimar os ganhos genéticos de um teste de progênies de seringueira para a produção de borracha seca e, com base no maior tamanho efetivo populacional e maior ganho genético, obter os melhores indivíduos. Foram utilizadas 30 progênies de meios-irmãos, provenientes de sementes de polinização mista - alogamia e autogamia - de testes clonais no Estado de São Paulo. Utilizou-se o delineamento experimental de blocos ao acaso, com 30 tratamentos (progênies), 3 repetições e parcelas lineares de 10 plantas, em um espaçamento de 3x3 m, o que totalizou 900 plantas úteis. Aos três anos, o perímetro, a 50 cm do solo (PA50), e a produção de borracha seca (PBS) foram avaliadas por meio do teste precoce de produção Hamaker Morris-Mann (HMM). As variáveis foram analisadas pelo método de modelo linear misto, via procedimento REML/BLUP, em progênies com sistema reprodutivo misto e taxa de autofecundação de 22%. A identificação dos 20 melhores indivíduos quanto à PBS e ao PA50 proporcionou ganho genético de 67,96 e 16,48%, respectivamente, e um coeficiente de endogamia de aproximadamente 2,82%. O teste de progênies proporciona produção de sementes com melhor valor genético, grande variabilidade e baixa endogamia

Uso de antibióticos para o controle de bactérias endógenas visando à micropropagação da figueira

A descontaminação dos explantes é um dos princípios básicos para o sucesso da cultura de tecidos. Um dos problemas diagnosticados na propagação in vitro da figueira, através de gemas apicais, é a contaminação endógena dos explantes por bactérias. Este trabalho teve como objetivo avaliar a eficiência de alguns antibióticos em meio de cultura para o controle de bactérias endógenas em gemas apicais de figueira. Foram avaliados os seguintes tratamentos: T1(sem adição de antibiótico); T2 (30 mg L-1 de cloranfenicol); T3 (250 mg L-1 de ampicilina sódica); T4 (500 mg L-1 de ácido nalidícico); T5 (150 mg L-1 de cefalotina sódica); T6 (500 mg L-1 de tetraciclina), e T7 (400 mg L-1 de norfloxacina). Após coletados em campo, os segmentos de ramos contendo as gemas foram colocados em recipiente com água corrente. Posteriormente, as gemas apicais foram imersas em álcool etílico a 70% e hipoclorito de sódio a 2,5%. Todo procedimento de desinfestação externa dos explantes foi realizado em câmara de fluxo laminar. Os explantes foram inoculados em tubos de ensaio contendo 15 mL de meio básico MS suplementado, após a autoclavagem, com as doses de antibióticos de acordo com os tratamentos estabelecidos. Após a inoculação, os explantes foram mantidos em sala de crescimento por quatro dias no escuro e, em seguida, sob fotoperíodo de 16 horas de luz branca fria e irradiância de 25 µmol m s-1, na temperatura de 22 ± 3ºC. A assepsia realizada externamente nos explantes foi suficiente para o controle de contaminação fúngica, e a adição de antibióticos ao meio, após autoclavagem, foi eficiente para o controle de bactérias endógenas, cujo antibiótico ampicilina sódica proporcionou mais de 90% de explantes sobreviventes.