Synthesis and characterization of composite magnetic zeolites using kaolin for softening water

Detalhes bibliográficos
Autor(a) principal: Raquel de Andrade Bessa
Data de Publicação: 2016
Tipo de documento: Dissertação
Idioma: por
Título da fonte: Biblioteca Digital de Teses e Dissertações da UFC
Texto Completo: http://www.teses.ufc.br/tde_busca/arquivo.php?codArquivo=17007
Resumo: The present work deals about the synthesis and characterization of magnetic zeolites obtained by hydrothermal route using kaolin from Brazilian Northeast as silicon and aluminum source. By means of the X-ray diffraction technique it was possible to identify zeolite LTA and zeolite P1 as major crystalline phases for each synthesis, with low intensity peaks referent to unreacted quartz present in the kaolin used, which is in accordance to the. FTIR spectra; the nanoparticles were identified as magnetite, with low intensity peaks referent to goethite. In scanning electron microscopy, however, it was not possible to morphologically identify these minor components, while the zeolites showed well defined morphologies, presenting unchanged morphology when in the composites form, but with nanoparticles dispersed over their surface, as expected. From transmission electron microscopy it was observed that the nanoparticles were of ca. 50 nm. Magnetic measurements indicated magnetite presence with superior diameter to critical diameter to superparamagnetic particles and remanent magnetization. Thermogravimetric analyses showed for the composites, lower mass loss than compared to the pure zeolites what may be associated to the improvement of its thermal stability. Granulometric distribution indicated nanoparticles agglomeration in variable sizes, while zeolites formed agglomerates of ca. 10 Âm. Water softening was accomplished by using both zeolites, with high efficiency on Ca2+ removal and similar behavior between the zeolite and its respective composite, being the best result observed for zeolite A, with efficiency of 97,95%, reaching equilibrium in the first contact minutes. The dependence on mass studies also showed that zeolite A and its composite presented the best efficiency, whereas zeolite P achieved the same removal levels using corresponding zeolite masses (45 mg). This way, the proposed method for zeolites synthesis proved to be efficient, so that the use of a magnet is capable to attract them, leading their excellent separation from the aqueous medium with its ionic exchange capacity unaffected.
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spelling info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisSynthesis and characterization of composite magnetic zeolites using kaolin for softening waterSÃntese e caracterizaÃÃo de compÃsitos de zeÃlitas magnÃticas utilizando caulim para abrandamento de Ãgua2016-02-19Adonay Rodrigues Loiola88127370304http://lattes.cnpq.br/9807982856173580CÃcero Pessoa de Moura82570507334http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4751378J5Cristiane Pinto Oliveira50612867315CV: http://lattes.cnpq.br/638358694296827804317906392http://lattes.cnpq.br/1585823257350406Raquel de Andrade BessaUniversidade Federal do CearÃPrograma de PÃs-GraduaÃÃo em QuÃmica UFCBRZeÃlita AZeÃlita PZeÃlitas magnÃticasNanopartÃculas magnÃticasAbrandamento de ÃguaZeolite AZeolite PMagnetic zeolitesMagnetite nanoparticlesWater softeningQUIMICAThe present work deals about the synthesis and characterization of magnetic zeolites obtained by hydrothermal route using kaolin from Brazilian Northeast as silicon and aluminum source. By means of the X-ray diffraction technique it was possible to identify zeolite LTA and zeolite P1 as major crystalline phases for each synthesis, with low intensity peaks referent to unreacted quartz present in the kaolin used, which is in accordance to the. FTIR spectra; the nanoparticles were identified as magnetite, with low intensity peaks referent to goethite. In scanning electron microscopy, however, it was not possible to morphologically identify these minor components, while the zeolites showed well defined morphologies, presenting unchanged morphology when in the composites form, but with nanoparticles dispersed over their surface, as expected. From transmission electron microscopy it was observed that the nanoparticles were of ca. 50 nm. Magnetic measurements indicated magnetite presence with superior diameter to critical diameter to superparamagnetic particles and remanent magnetization. Thermogravimetric analyses showed for the composites, lower mass loss than compared to the pure zeolites what may be associated to the improvement of its thermal stability. Granulometric distribution indicated nanoparticles agglomeration in variable sizes, while zeolites formed agglomerates of ca. 10 Âm. Water softening was accomplished by using both zeolites, with high efficiency on Ca2+ removal and similar behavior between the zeolite and its respective composite, being the best result observed for zeolite A, with efficiency of 97,95%, reaching equilibrium in the first contact minutes. The dependence on mass studies also showed that zeolite A and its composite presented the best efficiency, whereas zeolite P achieved the same removal levels using corresponding zeolite masses (45 mg). This way, the proposed method for zeolites synthesis proved to be efficient, so that the use of a magnet is capable to attract them, leading their excellent separation from the aqueous medium with its ionic exchange capacity unaffected.O presente trabalho trata da sÃntese e caracterizaÃÃo de zeÃlitas magnÃticas obtidas por impregnaÃÃo de nanopartÃculas de magnetita a zeÃlitas A e P, sintetizadas por mÃtodo hidrotÃrmico utilizando caulim branco do Nordeste brasileiro como fonte de silÃcio e alumÃnio. Por meio da tÃcnica de difraÃÃo de raios-X foi possÃvel identificar como fases cristalinas majoritÃrias a zeÃlita LTA e P1 para cada sÃntese, com picos de baixa intensidade referentes a quartzo, resistente ao processo tÃrmico de tratamento prÃvio do caulim, bem como nos espectros de infravermelho; as nanopartÃculas foram identificadas como magnetita, havendo ainda indÃcios da presenÃa de goethita em pequena quantidade. Nas anÃlises de microscopia eletrÃnica de varredura, entretanto, nÃo foi possÃvel identificar esses componentes minoritÃrios morfologicamente; enquanto que a morfologia das zeÃlitas mostrou-se bem definida, sem alteraÃÃes apÃs a formaÃÃo dos compÃsitos, apenas com nanopartÃculas espalhadas em sua superfÃcie, como desejado. A partir da microscopia eletrÃnica de transmissÃo, pÃde-se observar melhor a variaÃÃo de tamanho das nanopartÃculas, em mÃdia de 50 nm. Medidas magnÃticas das amostras com essa propriedade indicaram a presenÃa de magnetita com diÃmetro superior ao diÃmetro crÃtico para partÃculas superparamagnÃticas e magnetizaÃÃo remanente. As anÃlises termogravimÃtricas mostraram que a adiÃÃo das nanopartÃculas Ãs zeÃlitas diminuiu sua perda de massa diante do aumento de temperatura e as anÃlises de distribuiÃÃo granulomÃtrica indicaram a aglomeraÃÃo das nanopartÃculas em tamanhos variÃveis, enquanto que as zeÃlitas formaram aglomerados de aproximadamente 10 Âm. Os ensaios de abrandamento de Ãguas mostraram alta eficiÃncia das zeÃlitas em remover Ca2+, com comportamento similar entre a zeÃlita e o seu respectivo compÃsito, encontrando para a zeÃlita A o maior percentual de remoÃÃo, de 97,95 %, atingindo equilÃbrio nos primeiros minutos de aplicaÃÃo. Os estudos de massa tambÃm mostraram a eficiÃncia da zeÃlita A e de seu compÃsito, tendo a zeÃlita P se aproximado dos mesmos nÃveis de remoÃÃo em massas referentes a 45 mg de zeÃlita. Assim, o mÃtodo proposto para sÃntese das zeÃlitas magnÃticas mostrou-se eficiente, de modo que a utilizaÃÃo de um Ãmà à capaz de atraÃ-las facilitando a separaÃÃo do meio apÃs a aplicaÃÃo em meio aquoso e sua capacidade de troca iÃnica nÃo foi afetada.CoordenaÃÃo de AperfeiÃoamento de Pessoal de NÃvel Superiorhttp://www.teses.ufc.br/tde_busca/arquivo.php?codArquivo=17007application/pdfinfo:eu-repo/semantics/openAccessporreponame:Biblioteca Digital de Teses e Dissertações da UFCinstname:Universidade Federal do Cearáinstacron:UFC2019-01-21T11:30:25Zmail@mail.com -
dc.title.en.fl_str_mv Synthesis and characterization of composite magnetic zeolites using kaolin for softening water
dc.title.alternative.pt.fl_str_mv SÃntese e caracterizaÃÃo de compÃsitos de zeÃlitas magnÃticas utilizando caulim para abrandamento de Ãgua
title Synthesis and characterization of composite magnetic zeolites using kaolin for softening water
spellingShingle Synthesis and characterization of composite magnetic zeolites using kaolin for softening water
Raquel de Andrade Bessa
ZeÃlita A
ZeÃlita P
ZeÃlitas magnÃticas
NanopartÃculas magnÃticas
Abrandamento de Ãgua
Zeolite A
Zeolite P
Magnetic zeolites
Magnetite nanoparticles
Water softening
QUIMICA
title_short Synthesis and characterization of composite magnetic zeolites using kaolin for softening water
title_full Synthesis and characterization of composite magnetic zeolites using kaolin for softening water
title_fullStr Synthesis and characterization of composite magnetic zeolites using kaolin for softening water
title_full_unstemmed Synthesis and characterization of composite magnetic zeolites using kaolin for softening water
title_sort Synthesis and characterization of composite magnetic zeolites using kaolin for softening water
author Raquel de Andrade Bessa
author_facet Raquel de Andrade Bessa
author_role author
dc.contributor.advisor1.fl_str_mv Adonay Rodrigues Loiola
dc.contributor.advisor1ID.fl_str_mv 88127370304
dc.contributor.advisor1Lattes.fl_str_mv http://lattes.cnpq.br/9807982856173580
dc.contributor.referee1.fl_str_mv CÃcero Pessoa de Moura
dc.contributor.referee1ID.fl_str_mv 82570507334
dc.contributor.referee1Lattes.fl_str_mv http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4751378J5
dc.contributor.referee2.fl_str_mv Cristiane Pinto Oliveira
dc.contributor.referee2ID.fl_str_mv 50612867315
dc.contributor.referee2Lattes.fl_str_mv CV: http://lattes.cnpq.br/6383586942968278
dc.contributor.authorID.fl_str_mv 04317906392
dc.contributor.authorLattes.fl_str_mv http://lattes.cnpq.br/1585823257350406
dc.contributor.author.fl_str_mv Raquel de Andrade Bessa
contributor_str_mv Adonay Rodrigues Loiola
CÃcero Pessoa de Moura
Cristiane Pinto Oliveira
dc.subject.por.fl_str_mv ZeÃlita A
ZeÃlita P
ZeÃlitas magnÃticas
NanopartÃculas magnÃticas
Abrandamento de Ãgua
topic ZeÃlita A
ZeÃlita P
ZeÃlitas magnÃticas
NanopartÃculas magnÃticas
Abrandamento de Ãgua
Zeolite A
Zeolite P
Magnetic zeolites
Magnetite nanoparticles
Water softening
QUIMICA
dc.subject.eng.fl_str_mv Zeolite A
Zeolite P
Magnetic zeolites
Magnetite nanoparticles
Water softening
dc.subject.cnpq.fl_str_mv QUIMICA
dc.description.sponsorship.fl_txt_mv CoordenaÃÃo de AperfeiÃoamento de Pessoal de NÃvel Superior
dc.description.abstract.por.fl_txt_mv The present work deals about the synthesis and characterization of magnetic zeolites obtained by hydrothermal route using kaolin from Brazilian Northeast as silicon and aluminum source. By means of the X-ray diffraction technique it was possible to identify zeolite LTA and zeolite P1 as major crystalline phases for each synthesis, with low intensity peaks referent to unreacted quartz present in the kaolin used, which is in accordance to the. FTIR spectra; the nanoparticles were identified as magnetite, with low intensity peaks referent to goethite. In scanning electron microscopy, however, it was not possible to morphologically identify these minor components, while the zeolites showed well defined morphologies, presenting unchanged morphology when in the composites form, but with nanoparticles dispersed over their surface, as expected. From transmission electron microscopy it was observed that the nanoparticles were of ca. 50 nm. Magnetic measurements indicated magnetite presence with superior diameter to critical diameter to superparamagnetic particles and remanent magnetization. Thermogravimetric analyses showed for the composites, lower mass loss than compared to the pure zeolites what may be associated to the improvement of its thermal stability. Granulometric distribution indicated nanoparticles agglomeration in variable sizes, while zeolites formed agglomerates of ca. 10 Âm. Water softening was accomplished by using both zeolites, with high efficiency on Ca2+ removal and similar behavior between the zeolite and its respective composite, being the best result observed for zeolite A, with efficiency of 97,95%, reaching equilibrium in the first contact minutes. The dependence on mass studies also showed that zeolite A and its composite presented the best efficiency, whereas zeolite P achieved the same removal levels using corresponding zeolite masses (45 mg). This way, the proposed method for zeolites synthesis proved to be efficient, so that the use of a magnet is capable to attract them, leading their excellent separation from the aqueous medium with its ionic exchange capacity unaffected.
O presente trabalho trata da sÃntese e caracterizaÃÃo de zeÃlitas magnÃticas obtidas por impregnaÃÃo de nanopartÃculas de magnetita a zeÃlitas A e P, sintetizadas por mÃtodo hidrotÃrmico utilizando caulim branco do Nordeste brasileiro como fonte de silÃcio e alumÃnio. Por meio da tÃcnica de difraÃÃo de raios-X foi possÃvel identificar como fases cristalinas majoritÃrias a zeÃlita LTA e P1 para cada sÃntese, com picos de baixa intensidade referentes a quartzo, resistente ao processo tÃrmico de tratamento prÃvio do caulim, bem como nos espectros de infravermelho; as nanopartÃculas foram identificadas como magnetita, havendo ainda indÃcios da presenÃa de goethita em pequena quantidade. Nas anÃlises de microscopia eletrÃnica de varredura, entretanto, nÃo foi possÃvel identificar esses componentes minoritÃrios morfologicamente; enquanto que a morfologia das zeÃlitas mostrou-se bem definida, sem alteraÃÃes apÃs a formaÃÃo dos compÃsitos, apenas com nanopartÃculas espalhadas em sua superfÃcie, como desejado. A partir da microscopia eletrÃnica de transmissÃo, pÃde-se observar melhor a variaÃÃo de tamanho das nanopartÃculas, em mÃdia de 50 nm. Medidas magnÃticas das amostras com essa propriedade indicaram a presenÃa de magnetita com diÃmetro superior ao diÃmetro crÃtico para partÃculas superparamagnÃticas e magnetizaÃÃo remanente. As anÃlises termogravimÃtricas mostraram que a adiÃÃo das nanopartÃculas Ãs zeÃlitas diminuiu sua perda de massa diante do aumento de temperatura e as anÃlises de distribuiÃÃo granulomÃtrica indicaram a aglomeraÃÃo das nanopartÃculas em tamanhos variÃveis, enquanto que as zeÃlitas formaram aglomerados de aproximadamente 10 Âm. Os ensaios de abrandamento de Ãguas mostraram alta eficiÃncia das zeÃlitas em remover Ca2+, com comportamento similar entre a zeÃlita e o seu respectivo compÃsito, encontrando para a zeÃlita A o maior percentual de remoÃÃo, de 97,95 %, atingindo equilÃbrio nos primeiros minutos de aplicaÃÃo. Os estudos de massa tambÃm mostraram a eficiÃncia da zeÃlita A e de seu compÃsito, tendo a zeÃlita P se aproximado dos mesmos nÃveis de remoÃÃo em massas referentes a 45 mg de zeÃlita. Assim, o mÃtodo proposto para sÃntese das zeÃlitas magnÃticas mostrou-se eficiente, de modo que a utilizaÃÃo de um Ãmà à capaz de atraÃ-las facilitando a separaÃÃo do meio apÃs a aplicaÃÃo em meio aquoso e sua capacidade de troca iÃnica nÃo foi afetada.
description The present work deals about the synthesis and characterization of magnetic zeolites obtained by hydrothermal route using kaolin from Brazilian Northeast as silicon and aluminum source. By means of the X-ray diffraction technique it was possible to identify zeolite LTA and zeolite P1 as major crystalline phases for each synthesis, with low intensity peaks referent to unreacted quartz present in the kaolin used, which is in accordance to the. FTIR spectra; the nanoparticles were identified as magnetite, with low intensity peaks referent to goethite. In scanning electron microscopy, however, it was not possible to morphologically identify these minor components, while the zeolites showed well defined morphologies, presenting unchanged morphology when in the composites form, but with nanoparticles dispersed over their surface, as expected. From transmission electron microscopy it was observed that the nanoparticles were of ca. 50 nm. Magnetic measurements indicated magnetite presence with superior diameter to critical diameter to superparamagnetic particles and remanent magnetization. Thermogravimetric analyses showed for the composites, lower mass loss than compared to the pure zeolites what may be associated to the improvement of its thermal stability. Granulometric distribution indicated nanoparticles agglomeration in variable sizes, while zeolites formed agglomerates of ca. 10 Âm. Water softening was accomplished by using both zeolites, with high efficiency on Ca2+ removal and similar behavior between the zeolite and its respective composite, being the best result observed for zeolite A, with efficiency of 97,95%, reaching equilibrium in the first contact minutes. The dependence on mass studies also showed that zeolite A and its composite presented the best efficiency, whereas zeolite P achieved the same removal levels using corresponding zeolite masses (45 mg). This way, the proposed method for zeolites synthesis proved to be efficient, so that the use of a magnet is capable to attract them, leading their excellent separation from the aqueous medium with its ionic exchange capacity unaffected.
publishDate 2016
dc.date.issued.fl_str_mv 2016-02-19
dc.type.status.fl_str_mv info:eu-repo/semantics/publishedVersion
dc.type.driver.fl_str_mv info:eu-repo/semantics/masterThesis
status_str publishedVersion
format masterThesis
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dc.language.iso.fl_str_mv por
language por
dc.rights.driver.fl_str_mv info:eu-repo/semantics/openAccess
eu_rights_str_mv openAccess
dc.format.none.fl_str_mv application/pdf
dc.publisher.none.fl_str_mv Universidade Federal do CearÃ
dc.publisher.program.fl_str_mv Programa de PÃs-GraduaÃÃo em QuÃmica
dc.publisher.initials.fl_str_mv UFC
dc.publisher.country.fl_str_mv BR
publisher.none.fl_str_mv Universidade Federal do CearÃ
dc.source.none.fl_str_mv reponame:Biblioteca Digital de Teses e Dissertações da UFC
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reponame_str Biblioteca Digital de Teses e Dissertações da UFC
collection Biblioteca Digital de Teses e Dissertações da UFC
instname_str Universidade Federal do Ceará
instacron_str UFC
institution UFC
repository.name.fl_str_mv -
repository.mail.fl_str_mv mail@mail.com
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