Textural properties study of Mg-Al layered double hydroxide with different molar ratios and upon hydrothermal treatments
Autor(a) principal: | |
---|---|
Data de Publicação: | 2014 |
Tipo de documento: | Tese |
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=13527 |
Resumo: | Layered Double Hydroxide (LDH) belongs to a class of ceramic materials that present structure formed by stacked layers of double metals hydroxides and an anion into the lamellar space. They present a large variety of applications possibilities, as industrial, environment, medicine, among others. Non-calcined Mg-Al layered double hydroxide (LDH) with molar ratio, x = Al / (Mg + Al), 0.20, 0.25 and 0.30 were synthesized using co-precipitation method, followed by hydrothermal treatment at a fixed temperature 80ÂC and different aging from 2 to 35 days. The material obtained was characterized by XRD, IR, TG, SEM and EDS. The samples crystallinity was evaluated and particle size was calculated using Scherrer equation. Sorption of anionic acid blue 25 and reactive blue 4 dyes from aqueous solution was investigated for some of the 0.25 molar ratio samples. The purpose of this research was to study the effect of hydrothermal treatment aging conditions on textural properties of synthetic hydrotalcite with different molar ratios and propose a mathematical function to predict crystallite size and crystallinity. This function takes just two of many parameters in consideration: hydrothermal treatment aging time and molar ratio. The obtained as-synthesized samples with a molar ratio 0.20 and 0.25 showed good crystallinity for all the samples. On the other hand the third samples with molar ratio 0.30 showed poor crystallinity, a pronounced shift in the correspondent basal planes peaks 003 and 006, and a broadening in all peaks. The shift in the basal planes was shown to be statistically significant to the others. A non-expected result was found in disagreement with literature: a new crystalline phase was observed in two 0.20 molar ratio samples. MEV and EDS results indicate the existence of a probable amorphous phase in the 0.30 molar ratio samples. The amorphous phase would explain the reduction in crystallinity of this series samples. Just the function to predict the crystallinity was obtained and showed in a 3D and hypsometric graphics. This function may be used to predict a characteristic of a synthesized LDH for an industrial application, like adsorption. |
id |
UFC_6b762e1db315fd02a9cc31ce4d05e981 |
---|---|
oai_identifier_str |
oai:www.teses.ufc.br:7724 |
network_acronym_str |
UFC |
network_name_str |
Biblioteca Digital de Teses e Dissertações da UFC |
spelling |
info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisTextural properties study of Mg-Al layered double hydroxide with different molar ratios and upon hydrothermal treatmentsTextural properties study of Mg-Al layered double hydroxide with different molar ratios and upon hydrothermal treatments2014-02-28Ricardo EmÃlio Ferreira Quevedo Nogueira20333560353http://lattes.cnpq.br/6064127323404237SebastiÃo MardÃnio Pereira de Lucena25878760363Jose Marcos Sasaki41317874900Walney Silva Araujo21325102562http://lattes.cnpq.br/5265070571589358Francisca Maria Martins Pereira40808041304http://lattes.cnpq.br/4567080204141998Emmanuelle de Oliveira Sancho76878775353http://lattes.cnpq.br/684981901850915251271664372http://lattes.cnpq.br/0610200537263713Paulo DemÃtrios da Silva LimaUniversidade Federal do CearÃPrograma de PÃs-GraduaÃÃo em Engenharia e CiÃncia de MateriaisUFCBRHDL Hidrotalcita CristalinidadeLDH Hydrotalcite Crystallinity AdsorptionENGENHARIA DE MATERIAIS E METALURGICALayered Double Hydroxide (LDH) belongs to a class of ceramic materials that present structure formed by stacked layers of double metals hydroxides and an anion into the lamellar space. They present a large variety of applications possibilities, as industrial, environment, medicine, among others. Non-calcined Mg-Al layered double hydroxide (LDH) with molar ratio, x = Al / (Mg + Al), 0.20, 0.25 and 0.30 were synthesized using co-precipitation method, followed by hydrothermal treatment at a fixed temperature 80ÂC and different aging from 2 to 35 days. The material obtained was characterized by XRD, IR, TG, SEM and EDS. The samples crystallinity was evaluated and particle size was calculated using Scherrer equation. Sorption of anionic acid blue 25 and reactive blue 4 dyes from aqueous solution was investigated for some of the 0.25 molar ratio samples. The purpose of this research was to study the effect of hydrothermal treatment aging conditions on textural properties of synthetic hydrotalcite with different molar ratios and propose a mathematical function to predict crystallite size and crystallinity. This function takes just two of many parameters in consideration: hydrothermal treatment aging time and molar ratio. The obtained as-synthesized samples with a molar ratio 0.20 and 0.25 showed good crystallinity for all the samples. On the other hand the third samples with molar ratio 0.30 showed poor crystallinity, a pronounced shift in the correspondent basal planes peaks 003 and 006, and a broadening in all peaks. The shift in the basal planes was shown to be statistically significant to the others. A non-expected result was found in disagreement with literature: a new crystalline phase was observed in two 0.20 molar ratio samples. MEV and EDS results indicate the existence of a probable amorphous phase in the 0.30 molar ratio samples. The amorphous phase would explain the reduction in crystallinity of this series samples. Just the function to predict the crystallinity was obtained and showed in a 3D and hypsometric graphics. This function may be used to predict a characteristic of a synthesized LDH for an industrial application, like adsorption.HidrÃxidos Duplos Lamelares (HDL) pertencem a uma classe de materiais cerÃmicos formados por camadas empilhadas de hidrÃxidos metÃlicos com um Ãnion entre os espaÃos lamelares. Apresentam uma grande variedade de possÃveis aplicaÃÃes, na Ãrea industrial, ambiental, medicinal, entre outras. HidrÃxidos Duplos Lamelares (HDL) nÃo calcinados de MagnÃsio e AlumÃnio com razÃo molar x = Al / (Mg + Al), 0,20, 0,25 e 0,30 foram sintetizados utilizando o mÃtodo de co-precipitaÃÃo, seguido por tratamento hidrotÃrmico em temperatura fixa de 80  C e diferente tempos de maturaÃÃo de 2 a 35 dias. O material obtido foi caracterizado por DRX, IV, TG, MEV e EDS. A cristalinidade das amostras foi avaliada e tamanho de partÃcula foi calculado usando a equaÃÃo Scherrer. Foram investigadas adsorÃÃo de corantes Ãcido azul 25 e azul reativo 4 para algumas amostras de razÃo molar 0,25. O objetivo deste trabalho foi estudar o efeito do tratamento hidrotÃrmico e condiÃÃes de tempo de maturaÃÃo nas propriedades texturais de hidrotalcita sintetizada com diferentes razÃes molares e propor uma funÃÃo matemÃtica para prever o tamanho de cristalito e cristalinidade. Esta funÃÃo leva apenas dois de muitos parÃmetros em consideraÃÃo: tempo de tratamento hidrotÃrmico e razÃo molar. As amostras obtidas com uma razÃo molar 0,20 e 0,25 apresentaram boa cristalinidade para todas as amostras. Por outro lado, as amostras com razÃo molar 0,30 apresentaram baixa cristalinidade, um pronunciado deslocamento nos picos basais 003 e 006, e um alargamento em todos os picos. O deslocamento desses picos para essa Ãltima amostra foi mostrado ser estatisticamente significativo em relaÃÃo Ãs outras duas. Um resultado nÃo esperado foi encontrado em desacordo com a literatura: uma nova fase cristalina foi observada em duas amostras de razÃo molar 0,20. Os resultados do MEV e EDS indicam que hà uma provÃvel fase amorfa nas amostras de razÃo molar 0,30. A fase amorfa explicaria a reduÃÃo da cristalinidade das amostras dessa sÃrie. Apenas a funÃÃo para prever a cristalinidade foi obtida e mostrada em grÃficos 3D e hipsomÃtricos. Esta funÃÃo pode ser usada para prever caracterÃsticas de um HDL sintetizado para uma aplicaÃÃo industrial, tal como a adsorÃÃo.http://www.teses.ufc.br/tde_busca/arquivo.php?codArquivo=13527application/pdfinfo:eu-repo/semantics/openAccessporreponame:Biblioteca Digital de Teses e Dissertações da UFCinstname:Universidade Federal do Cearáinstacron:UFC2019-01-21T11:26:45Zmail@mail.com - |
dc.title.en.fl_str_mv |
Textural properties study of Mg-Al layered double hydroxide with different molar ratios and upon hydrothermal treatments |
dc.title.alternative.pt.fl_str_mv |
Textural properties study of Mg-Al layered double hydroxide with different molar ratios and upon hydrothermal treatments |
title |
Textural properties study of Mg-Al layered double hydroxide with different molar ratios and upon hydrothermal treatments |
spellingShingle |
Textural properties study of Mg-Al layered double hydroxide with different molar ratios and upon hydrothermal treatments Paulo DemÃtrios da Silva Lima HDL Hidrotalcita Cristalinidade LDH Hydrotalcite Crystallinity Adsorption ENGENHARIA DE MATERIAIS E METALURGICA |
title_short |
Textural properties study of Mg-Al layered double hydroxide with different molar ratios and upon hydrothermal treatments |
title_full |
Textural properties study of Mg-Al layered double hydroxide with different molar ratios and upon hydrothermal treatments |
title_fullStr |
Textural properties study of Mg-Al layered double hydroxide with different molar ratios and upon hydrothermal treatments |
title_full_unstemmed |
Textural properties study of Mg-Al layered double hydroxide with different molar ratios and upon hydrothermal treatments |
title_sort |
Textural properties study of Mg-Al layered double hydroxide with different molar ratios and upon hydrothermal treatments |
author |
Paulo DemÃtrios da Silva Lima |
author_facet |
Paulo DemÃtrios da Silva Lima |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Ricardo EmÃlio Ferreira Quevedo Nogueira |
dc.contributor.advisor1ID.fl_str_mv |
20333560353 |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/6064127323404237 |
dc.contributor.advisor-co1.fl_str_mv |
SebastiÃo MardÃnio Pereira de Lucena |
dc.contributor.advisor-co1ID.fl_str_mv |
25878760363 |
dc.contributor.referee1.fl_str_mv |
Jose Marcos Sasaki |
dc.contributor.referee1ID.fl_str_mv |
41317874900 |
dc.contributor.referee2.fl_str_mv |
Walney Silva Araujo |
dc.contributor.referee2ID.fl_str_mv |
21325102562 |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/5265070571589358 |
dc.contributor.referee3.fl_str_mv |
Francisca Maria Martins Pereira |
dc.contributor.referee3ID.fl_str_mv |
40808041304 |
dc.contributor.referee3Lattes.fl_str_mv |
http://lattes.cnpq.br/4567080204141998 |
dc.contributor.referee4.fl_str_mv |
Emmanuelle de Oliveira Sancho |
dc.contributor.referee4ID.fl_str_mv |
76878775353 |
dc.contributor.referee4Lattes.fl_str_mv |
http://lattes.cnpq.br/6849819018509152 |
dc.contributor.authorID.fl_str_mv |
51271664372 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/0610200537263713 |
dc.contributor.author.fl_str_mv |
Paulo DemÃtrios da Silva Lima |
contributor_str_mv |
Ricardo EmÃlio Ferreira Quevedo Nogueira SebastiÃo MardÃnio Pereira de Lucena Jose Marcos Sasaki Walney Silva Araujo Francisca Maria Martins Pereira Emmanuelle de Oliveira Sancho |
dc.subject.por.fl_str_mv |
HDL Hidrotalcita Cristalinidade |
topic |
HDL Hidrotalcita Cristalinidade LDH Hydrotalcite Crystallinity Adsorption ENGENHARIA DE MATERIAIS E METALURGICA |
dc.subject.eng.fl_str_mv |
LDH Hydrotalcite Crystallinity Adsorption |
dc.subject.cnpq.fl_str_mv |
ENGENHARIA DE MATERIAIS E METALURGICA |
dc.description.abstract.por.fl_txt_mv |
Layered Double Hydroxide (LDH) belongs to a class of ceramic materials that present structure formed by stacked layers of double metals hydroxides and an anion into the lamellar space. They present a large variety of applications possibilities, as industrial, environment, medicine, among others. Non-calcined Mg-Al layered double hydroxide (LDH) with molar ratio, x = Al / (Mg + Al), 0.20, 0.25 and 0.30 were synthesized using co-precipitation method, followed by hydrothermal treatment at a fixed temperature 80ÂC and different aging from 2 to 35 days. The material obtained was characterized by XRD, IR, TG, SEM and EDS. The samples crystallinity was evaluated and particle size was calculated using Scherrer equation. Sorption of anionic acid blue 25 and reactive blue 4 dyes from aqueous solution was investigated for some of the 0.25 molar ratio samples. The purpose of this research was to study the effect of hydrothermal treatment aging conditions on textural properties of synthetic hydrotalcite with different molar ratios and propose a mathematical function to predict crystallite size and crystallinity. This function takes just two of many parameters in consideration: hydrothermal treatment aging time and molar ratio. The obtained as-synthesized samples with a molar ratio 0.20 and 0.25 showed good crystallinity for all the samples. On the other hand the third samples with molar ratio 0.30 showed poor crystallinity, a pronounced shift in the correspondent basal planes peaks 003 and 006, and a broadening in all peaks. The shift in the basal planes was shown to be statistically significant to the others. A non-expected result was found in disagreement with literature: a new crystalline phase was observed in two 0.20 molar ratio samples. MEV and EDS results indicate the existence of a probable amorphous phase in the 0.30 molar ratio samples. The amorphous phase would explain the reduction in crystallinity of this series samples. Just the function to predict the crystallinity was obtained and showed in a 3D and hypsometric graphics. This function may be used to predict a characteristic of a synthesized LDH for an industrial application, like adsorption. HidrÃxidos Duplos Lamelares (HDL) pertencem a uma classe de materiais cerÃmicos formados por camadas empilhadas de hidrÃxidos metÃlicos com um Ãnion entre os espaÃos lamelares. Apresentam uma grande variedade de possÃveis aplicaÃÃes, na Ãrea industrial, ambiental, medicinal, entre outras. HidrÃxidos Duplos Lamelares (HDL) nÃo calcinados de MagnÃsio e AlumÃnio com razÃo molar x = Al / (Mg + Al), 0,20, 0,25 e 0,30 foram sintetizados utilizando o mÃtodo de co-precipitaÃÃo, seguido por tratamento hidrotÃrmico em temperatura fixa de 80  C e diferente tempos de maturaÃÃo de 2 a 35 dias. O material obtido foi caracterizado por DRX, IV, TG, MEV e EDS. A cristalinidade das amostras foi avaliada e tamanho de partÃcula foi calculado usando a equaÃÃo Scherrer. Foram investigadas adsorÃÃo de corantes Ãcido azul 25 e azul reativo 4 para algumas amostras de razÃo molar 0,25. O objetivo deste trabalho foi estudar o efeito do tratamento hidrotÃrmico e condiÃÃes de tempo de maturaÃÃo nas propriedades texturais de hidrotalcita sintetizada com diferentes razÃes molares e propor uma funÃÃo matemÃtica para prever o tamanho de cristalito e cristalinidade. Esta funÃÃo leva apenas dois de muitos parÃmetros em consideraÃÃo: tempo de tratamento hidrotÃrmico e razÃo molar. As amostras obtidas com uma razÃo molar 0,20 e 0,25 apresentaram boa cristalinidade para todas as amostras. Por outro lado, as amostras com razÃo molar 0,30 apresentaram baixa cristalinidade, um pronunciado deslocamento nos picos basais 003 e 006, e um alargamento em todos os picos. O deslocamento desses picos para essa Ãltima amostra foi mostrado ser estatisticamente significativo em relaÃÃo Ãs outras duas. Um resultado nÃo esperado foi encontrado em desacordo com a literatura: uma nova fase cristalina foi observada em duas amostras de razÃo molar 0,20. Os resultados do MEV e EDS indicam que hà uma provÃvel fase amorfa nas amostras de razÃo molar 0,30. A fase amorfa explicaria a reduÃÃo da cristalinidade das amostras dessa sÃrie. Apenas a funÃÃo para prever a cristalinidade foi obtida e mostrada em grÃficos 3D e hipsomÃtricos. Esta funÃÃo pode ser usada para prever caracterÃsticas de um HDL sintetizado para uma aplicaÃÃo industrial, tal como a adsorÃÃo. |
description |
Layered Double Hydroxide (LDH) belongs to a class of ceramic materials that present structure formed by stacked layers of double metals hydroxides and an anion into the lamellar space. They present a large variety of applications possibilities, as industrial, environment, medicine, among others. Non-calcined Mg-Al layered double hydroxide (LDH) with molar ratio, x = Al / (Mg + Al), 0.20, 0.25 and 0.30 were synthesized using co-precipitation method, followed by hydrothermal treatment at a fixed temperature 80ÂC and different aging from 2 to 35 days. The material obtained was characterized by XRD, IR, TG, SEM and EDS. The samples crystallinity was evaluated and particle size was calculated using Scherrer equation. Sorption of anionic acid blue 25 and reactive blue 4 dyes from aqueous solution was investigated for some of the 0.25 molar ratio samples. The purpose of this research was to study the effect of hydrothermal treatment aging conditions on textural properties of synthetic hydrotalcite with different molar ratios and propose a mathematical function to predict crystallite size and crystallinity. This function takes just two of many parameters in consideration: hydrothermal treatment aging time and molar ratio. The obtained as-synthesized samples with a molar ratio 0.20 and 0.25 showed good crystallinity for all the samples. On the other hand the third samples with molar ratio 0.30 showed poor crystallinity, a pronounced shift in the correspondent basal planes peaks 003 and 006, and a broadening in all peaks. The shift in the basal planes was shown to be statistically significant to the others. A non-expected result was found in disagreement with literature: a new crystalline phase was observed in two 0.20 molar ratio samples. MEV and EDS results indicate the existence of a probable amorphous phase in the 0.30 molar ratio samples. The amorphous phase would explain the reduction in crystallinity of this series samples. Just the function to predict the crystallinity was obtained and showed in a 3D and hypsometric graphics. This function may be used to predict a characteristic of a synthesized LDH for an industrial application, like adsorption. |
publishDate |
2014 |
dc.date.issued.fl_str_mv |
2014-02-28 |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/doctoralThesis |
status_str |
publishedVersion |
format |
doctoralThesis |
dc.identifier.uri.fl_str_mv |
http://www.teses.ufc.br/tde_busca/arquivo.php?codArquivo=13527 |
url |
http://www.teses.ufc.br/tde_busca/arquivo.php?codArquivo=13527 |
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 Cearà |
dc.publisher.program.fl_str_mv |
Programa de PÃs-GraduaÃÃo em Engenharia e CiÃncia de Materiais |
dc.publisher.initials.fl_str_mv |
UFC |
dc.publisher.country.fl_str_mv |
BR |
publisher.none.fl_str_mv |
Universidade Federal do Cearà |
dc.source.none.fl_str_mv |
reponame:Biblioteca Digital de Teses e Dissertações da UFC instname:Universidade Federal do Ceará instacron:UFC |
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 |
_version_ |
1643295199764414464 |