Síntese de faujasita mesoporosa por síntese direta utilizando soft Template

Detalhes bibliográficos
Autor(a) principal: Almeida, Núbia Caroline de
Data de Publicação: 2017
Tipo de documento: Dissertação
Idioma: por
Título da fonte: Biblioteca Digital de Teses e Dissertações da UFRRJ
Texto Completo: https://rima.ufrrj.br/jspui/handle/20.500.14407/13466
Resumo: O mineral faujasita é isoestrutural das zeólitas sintéticas X e Y. Enquanto que a faujasita mineral possui composição de rede variável, a zeólita X apresenta razão de Si/Al entre 1,0 a 1,5 e a zeólita Y possui uma razão Si/Al superior a 1,5. A zeólita Y é o componente ativo do catalisador de craqueamento catalítico fluido (FCC), sendo desativada rapidamente pela formação de coque. Deste modo, gerar mesoporos possibilitaria maior rendimento no processo de FCC, pois melhoraria a transferência de massa. Amostras de faujasita mesoporosa foram preparadas por síntese direta utilizando surfactante CTABr como soft template em diferentes concentrações, tempos de cristalização e temperaturas. Para caracterização das amostras produzidas foram utilizadas as técnicas de difração de raios-X (DRX), adsorção/dessorção de N2, dessorção de NH3 à temperatura programada (TPD-NH3), ressonância nuclear magnética (RMN), microscopia eletrônica de varredura (MEV), espectroscopia de absorção no infra vermelho (FTIR), fluorescência de raios-X (FRX). Os resultados indicaram que houve aumento significativo no volume de mesoporos, 0,13 cm³/g, e formação de isotermas do tipo I e IV. As análises de DRX confirmaram a obtenção da estrutura faujasita com alto teor de cristalinidade. A razão de silício/alumínio obtida foi superior a 1,7, confirmando a presença de zeólita Y. Não foram observadas variações significativas na acidez total e houve a formação de apenas um pico de dessorção, caracterizado como acidez fraca. As análises de ressonância nuclear magnética mostraram um alto teor de alumínio octaédrico, associado ao alumínio extra rede. As imagens de microscopia eletrônica de varredura indicaram a formação de zeólita nanométrica. Os valores obtidos para tamanho de célula unitária estão condizentes com o presente na literatura; entre 24,18 e 25Å. As propriedades texturais melhoraram com a introdução do surfactante independente da temperatura de síntese. Os melhores resultados obtidos ocorreram para introdução de 0,5 mol de CTABr. Para amostras sintetizadas em temperaturas superiores, como 110°C, a introdução de surfactante propiciou a formação da estrutura faujasita em detrimento da estrutura hidroxisodalita. Para temperaturas mais elevadas, como 150°C, houve formação de fase contaminante; a zeólita GIS. Observou-se que o tamanho do cristal aumenta com o maior tempo de envelhecimento e é maior para amostras sintetizadas a 110°C. As amostras foram submetidas ainda a avaliação catalítica por meio da reação de craqueamento do n-heptano a 420°C, todavia não apresentaram resultados satisfatórios devido à grande quantidade de alumínio extra-rede.
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spelling Almeida, Núbia Caroline deFernandes, Lindoval Domiciano837.359.227-15http://lattes.cnpq.br/7921814684730923Passos, Fabio BarbozaMachado Junior, Hélio Fernandes110.028.327-30http://lattes.cnpq.br/47326618290091712023-12-22T02:47:04Z2023-12-22T02:47:04Z2017-05-08Almeida, Núbia Caroline de. Síntese de faujasita mesoporosa por síntese direta utilizando soft Template. 2017. 101 f. Dissertação (Programa de Pós-Graduação em Engenharia Química) - Universidade Federal Rural do Rio de Janeiro, [Seropédica - RJ] .https://rima.ufrrj.br/jspui/handle/20.500.14407/13466O mineral faujasita é isoestrutural das zeólitas sintéticas X e Y. Enquanto que a faujasita mineral possui composição de rede variável, a zeólita X apresenta razão de Si/Al entre 1,0 a 1,5 e a zeólita Y possui uma razão Si/Al superior a 1,5. A zeólita Y é o componente ativo do catalisador de craqueamento catalítico fluido (FCC), sendo desativada rapidamente pela formação de coque. Deste modo, gerar mesoporos possibilitaria maior rendimento no processo de FCC, pois melhoraria a transferência de massa. Amostras de faujasita mesoporosa foram preparadas por síntese direta utilizando surfactante CTABr como soft template em diferentes concentrações, tempos de cristalização e temperaturas. Para caracterização das amostras produzidas foram utilizadas as técnicas de difração de raios-X (DRX), adsorção/dessorção de N2, dessorção de NH3 à temperatura programada (TPD-NH3), ressonância nuclear magnética (RMN), microscopia eletrônica de varredura (MEV), espectroscopia de absorção no infra vermelho (FTIR), fluorescência de raios-X (FRX). Os resultados indicaram que houve aumento significativo no volume de mesoporos, 0,13 cm³/g, e formação de isotermas do tipo I e IV. As análises de DRX confirmaram a obtenção da estrutura faujasita com alto teor de cristalinidade. A razão de silício/alumínio obtida foi superior a 1,7, confirmando a presença de zeólita Y. Não foram observadas variações significativas na acidez total e houve a formação de apenas um pico de dessorção, caracterizado como acidez fraca. As análises de ressonância nuclear magnética mostraram um alto teor de alumínio octaédrico, associado ao alumínio extra rede. As imagens de microscopia eletrônica de varredura indicaram a formação de zeólita nanométrica. Os valores obtidos para tamanho de célula unitária estão condizentes com o presente na literatura; entre 24,18 e 25Å. As propriedades texturais melhoraram com a introdução do surfactante independente da temperatura de síntese. Os melhores resultados obtidos ocorreram para introdução de 0,5 mol de CTABr. Para amostras sintetizadas em temperaturas superiores, como 110°C, a introdução de surfactante propiciou a formação da estrutura faujasita em detrimento da estrutura hidroxisodalita. Para temperaturas mais elevadas, como 150°C, houve formação de fase contaminante; a zeólita GIS. Observou-se que o tamanho do cristal aumenta com o maior tempo de envelhecimento e é maior para amostras sintetizadas a 110°C. As amostras foram submetidas ainda a avaliação catalítica por meio da reação de craqueamento do n-heptano a 420°C, todavia não apresentaram resultados satisfatórios devido à grande quantidade de alumínio extra-rede.Coordenação de Aperfeiçoamento de Pessoal de Nível Superior, CAPES, Brasil.The faujasite mineral is isostructural of the synthetic zeolites X and Y. While the mineral faujasite has variable framework composition, the zeolite X has a Si/Al ratio of 1.0 to 1.5 and the zeolite Y has a Si / Al ratio greater than 1,5. Zeolite Y is the active component of the fluid catalytic cracking catalyst (FCC), being deactivated rapidly by the formation of coke. Thus, generating mesopores would allow greater yield in the FCC process, as it would improve mass transfer. Mesoporous faujasite samples were prepared by direct synthesis using CTABr surfactant as soft template at different concentrations, crystallization times and temperatures. For characterization of the produced samples were used the techniques of X-ray diffraction solid state (XRD), N2 adsorption / desorption, temperature programmed dessorption of NH3 (TPD-NH3), nuclear magnetic resonance (NMR), scanning electron microscopy (SEM), Infra Red Absorption Spectroscopy (FTIR), X-ray fluorescence (FRX). The results indicated there was a significant increase in the volume of mesopores, 0.13 cm³ / g, and formation of isotherms type I and IV. The XRD analyzes confirmed the obtaining of the faujasite structure with high crystallinity content. The Si/Al ratio obtained was higher than 1.7, confirming the presence of Y Zeolite. It was not observed a significant variation in the total acidity and only one desorption peak was formed, characterized as weak acidity. Nuclear magnetic resonance analyzes showed a high content of extra framework aluminum; octahedral. Scanning electron microscopy images indicated the formation of nanometric zeolite. The values obtained for unit cell size are consistent with the literature; between 24.18 and 25Å. The textural properties improved with the introduction of the surfactant independent of the synthesis temperature. The best results were obtained for the introduction of 0.5 mol of CTABr. For samples synthesized at higher temperatures, such as 110°C, the introduction of surfactant led to the formation of the Faujasite structure instead of the structure hydroxysodalite. For higher temperatures, such as 150°C, contaminant phase formation occurred; the GIS zeolite. It has been observed the crystal size increases with the longer aging time and is larger for samples synthesized at 110°C. 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ZUKAL, A.; PATZELOV, V.; LOHSE, U., Secondary Porous Structure Of Dealuminated Y Zeolites. Zeolites, v. 6, p. 133–https://tede.ufrrj.br/retrieve/64751/2017%20-%20N%c3%babia%20Caroline%20de%20Almeida.pdf.jpghttps://tede.ufrrj.br/jspui/handle/jspui/4568Submitted by Sandra Pereira (srpereira@ufrrj.br) on 2021-04-20T19:37:37Z No. of bitstreams: 1 2017 - Núbia Caroline de Almeida.pdf: 4735967 bytes, checksum: 6a00a466c1d280509e45a9fcc970f79f (MD5)Made available in DSpace on 2021-04-20T19:37:37Z (GMT). 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dc.title.por.fl_str_mv Síntese de faujasita mesoporosa por síntese direta utilizando soft Template
dc.title.alternative.eng.fl_str_mv Synthesis of mesoporous faujasite by direct synthesis using soft Template.
title Síntese de faujasita mesoporosa por síntese direta utilizando soft Template
spellingShingle Síntese de faujasita mesoporosa por síntese direta utilizando soft Template
Almeida, Núbia Caroline de
materiais mesoporosos
surfactante
faujasita
craqueamento catalítico
mesoporous materials
surfactant
faujasite
catalytic cracking
Engenharia Química
title_short Síntese de faujasita mesoporosa por síntese direta utilizando soft Template
title_full Síntese de faujasita mesoporosa por síntese direta utilizando soft Template
title_fullStr Síntese de faujasita mesoporosa por síntese direta utilizando soft Template
title_full_unstemmed Síntese de faujasita mesoporosa por síntese direta utilizando soft Template
title_sort Síntese de faujasita mesoporosa por síntese direta utilizando soft Template
author Almeida, Núbia Caroline de
author_facet Almeida, Núbia Caroline de
author_role author
dc.contributor.author.fl_str_mv Almeida, Núbia Caroline de
dc.contributor.advisor1.fl_str_mv Fernandes, Lindoval Domiciano
dc.contributor.advisor1ID.fl_str_mv 837.359.227-15
dc.contributor.advisor1Lattes.fl_str_mv http://lattes.cnpq.br/7921814684730923
dc.contributor.referee1.fl_str_mv Passos, Fabio Barboza
dc.contributor.referee2.fl_str_mv Machado Junior, Hélio Fernandes
dc.contributor.authorID.fl_str_mv 110.028.327-30
dc.contributor.authorLattes.fl_str_mv http://lattes.cnpq.br/4732661829009171
contributor_str_mv Fernandes, Lindoval Domiciano
Passos, Fabio Barboza
Machado Junior, Hélio Fernandes
dc.subject.por.fl_str_mv materiais mesoporosos
surfactante
faujasita
craqueamento catalítico
topic materiais mesoporosos
surfactante
faujasita
craqueamento catalítico
mesoporous materials
surfactant
faujasite
catalytic cracking
Engenharia Química
dc.subject.eng.fl_str_mv mesoporous materials
surfactant
faujasite
catalytic cracking
dc.subject.cnpq.fl_str_mv Engenharia Química
description O mineral faujasita é isoestrutural das zeólitas sintéticas X e Y. Enquanto que a faujasita mineral possui composição de rede variável, a zeólita X apresenta razão de Si/Al entre 1,0 a 1,5 e a zeólita Y possui uma razão Si/Al superior a 1,5. A zeólita Y é o componente ativo do catalisador de craqueamento catalítico fluido (FCC), sendo desativada rapidamente pela formação de coque. Deste modo, gerar mesoporos possibilitaria maior rendimento no processo de FCC, pois melhoraria a transferência de massa. Amostras de faujasita mesoporosa foram preparadas por síntese direta utilizando surfactante CTABr como soft template em diferentes concentrações, tempos de cristalização e temperaturas. Para caracterização das amostras produzidas foram utilizadas as técnicas de difração de raios-X (DRX), adsorção/dessorção de N2, dessorção de NH3 à temperatura programada (TPD-NH3), ressonância nuclear magnética (RMN), microscopia eletrônica de varredura (MEV), espectroscopia de absorção no infra vermelho (FTIR), fluorescência de raios-X (FRX). Os resultados indicaram que houve aumento significativo no volume de mesoporos, 0,13 cm³/g, e formação de isotermas do tipo I e IV. As análises de DRX confirmaram a obtenção da estrutura faujasita com alto teor de cristalinidade. A razão de silício/alumínio obtida foi superior a 1,7, confirmando a presença de zeólita Y. Não foram observadas variações significativas na acidez total e houve a formação de apenas um pico de dessorção, caracterizado como acidez fraca. As análises de ressonância nuclear magnética mostraram um alto teor de alumínio octaédrico, associado ao alumínio extra rede. As imagens de microscopia eletrônica de varredura indicaram a formação de zeólita nanométrica. Os valores obtidos para tamanho de célula unitária estão condizentes com o presente na literatura; entre 24,18 e 25Å. As propriedades texturais melhoraram com a introdução do surfactante independente da temperatura de síntese. Os melhores resultados obtidos ocorreram para introdução de 0,5 mol de CTABr. Para amostras sintetizadas em temperaturas superiores, como 110°C, a introdução de surfactante propiciou a formação da estrutura faujasita em detrimento da estrutura hidroxisodalita. Para temperaturas mais elevadas, como 150°C, houve formação de fase contaminante; a zeólita GIS. Observou-se que o tamanho do cristal aumenta com o maior tempo de envelhecimento e é maior para amostras sintetizadas a 110°C. As amostras foram submetidas ainda a avaliação catalítica por meio da reação de craqueamento do n-heptano a 420°C, todavia não apresentaram resultados satisfatórios devido à grande quantidade de alumínio extra-rede.
publishDate 2017
dc.date.issued.fl_str_mv 2017-05-08
dc.date.accessioned.fl_str_mv 2023-12-22T02:47:04Z
dc.date.available.fl_str_mv 2023-12-22T02:47:04Z
dc.type.status.fl_str_mv info:eu-repo/semantics/publishedVersion
dc.type.driver.fl_str_mv info:eu-repo/semantics/masterThesis
format masterThesis
status_str publishedVersion
dc.identifier.citation.fl_str_mv Almeida, Núbia Caroline de. Síntese de faujasita mesoporosa por síntese direta utilizando soft Template. 2017. 101 f. Dissertação (Programa de Pós-Graduação em Engenharia Química) - Universidade Federal Rural do Rio de Janeiro, [Seropédica - RJ] .
dc.identifier.uri.fl_str_mv https://rima.ufrrj.br/jspui/handle/20.500.14407/13466
identifier_str_mv Almeida, Núbia Caroline de. Síntese de faujasita mesoporosa por síntese direta utilizando soft Template. 2017. 101 f. Dissertação (Programa de Pós-Graduação em Engenharia Química) - Universidade Federal Rural do Rio de Janeiro, [Seropédica - RJ] .
url https://rima.ufrrj.br/jspui/handle/20.500.14407/13466
dc.language.iso.fl_str_mv por
language por
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