Síntese de hidróxido duplo lamelar Mg-Al via rota mecanoquímica
Autor(a) principal: | |
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Data de Publicação: | 2022 |
Tipo de documento: | Dissertação |
Idioma: | por |
Título da fonte: | Repositório Institucional da UFS |
Texto Completo: | http://ri.ufs.br/jspui/handle/riufs/16685 |
Resumo: | The synthesis of layered double hydroxides Mg-Al (LDH Mg-Al) via mechanochemical routes is reported. Manual grinding and horizontal ball milling were using as precursors aluminum hydroxide and magnesium oxide. The parameters of grinding time and addition of water were analyzed. The obtained products were characterized by x-ray diffraction (XRD), fourier transform infared (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (MET), termogravimetry (TG/DTG), electron diffraction (SAED) and in addition, three samples were selected to be submitted to tests of adsorption of humic acid by UV-Visible spectroscopy. A green synthesis was promoted due to the non-use of water in large quantities. Manual grinding samples obtained at 10 minutes of grinding with 2.0 mL of water added positive results simlarly to samples synthesized with the aid of an aging stage. The formation of HDL phases were also observed in samples obtained in 80 hours and 100 hours of grinding with horizontal ball milling, while the presence of crystalline phases of MgO precursor was reduced by around 40 hours of grinding. Samples obtained at 10 minutes of manual dry grinding showed intermediate phases, indicating the importance of adding water in the synthesis process. The formation of the LDH product obtained manually with the addition of water even if in small quantities discards the use of traditional methods involving solutions, such as coprecipitation for example. FTIR bands, MET and SEM microscopies, electron diffraction and TG/DTG curves complemented the discussion about x-ray diffraction, with emphasis on the FTIR that presented information to some free (OH) groups – no participation in hydrogen bonds – characteristics of Al(OH)3 and the amorphization behavior of this reagent used as a precursor. Adsorption testes revealed that one of the products obtained by manual milling showed excellent humic acid adsorption property when compared to other samples, one obtained by co-precipitation and the other commercial. |
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Bento, Gabriel SoaresGimenez, Iara de Fátima2022-10-24T17:27:52Z2022-10-24T17:27:52Z2022-08-26BENTO, Gabriel Soares. Síntese de hidróxido duplo lamelar Mg-Al via rota mecanoquímica. 2022. 91 f. Dissertação (Mestrado em Ciência e Engenharia de Materiais) – Universidade Federal de Sergipe, São Cristóvão, 2022.http://ri.ufs.br/jspui/handle/riufs/16685The synthesis of layered double hydroxides Mg-Al (LDH Mg-Al) via mechanochemical routes is reported. Manual grinding and horizontal ball milling were using as precursors aluminum hydroxide and magnesium oxide. The parameters of grinding time and addition of water were analyzed. The obtained products were characterized by x-ray diffraction (XRD), fourier transform infared (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (MET), termogravimetry (TG/DTG), electron diffraction (SAED) and in addition, three samples were selected to be submitted to tests of adsorption of humic acid by UV-Visible spectroscopy. A green synthesis was promoted due to the non-use of water in large quantities. Manual grinding samples obtained at 10 minutes of grinding with 2.0 mL of water added positive results simlarly to samples synthesized with the aid of an aging stage. The formation of HDL phases were also observed in samples obtained in 80 hours and 100 hours of grinding with horizontal ball milling, while the presence of crystalline phases of MgO precursor was reduced by around 40 hours of grinding. Samples obtained at 10 minutes of manual dry grinding showed intermediate phases, indicating the importance of adding water in the synthesis process. The formation of the LDH product obtained manually with the addition of water even if in small quantities discards the use of traditional methods involving solutions, such as coprecipitation for example. FTIR bands, MET and SEM microscopies, electron diffraction and TG/DTG curves complemented the discussion about x-ray diffraction, with emphasis on the FTIR that presented information to some free (OH) groups – no participation in hydrogen bonds – characteristics of Al(OH)3 and the amorphization behavior of this reagent used as a precursor. Adsorption testes revealed that one of the products obtained by manual milling showed excellent humic acid adsorption property when compared to other samples, one obtained by co-precipitation and the other commercial.Relata-se a síntese de hidróxidos duplos lamelares Mg-Al por rotas mecanoquímicas. A moagem manual e a moagem com auxílio de moinho de bolas horizontal foram empregadas usando como precursores hidróxido de alumínio e óxido de magnésio. Os parâmetros de tempo de moagem e adição de água foram analisados. Os produtos obtidos foram caracterizados por difratometria de raios-X, FTIR, microscopia eletrônica de varredura (MEV), microscopia eletrônica de transmissão (MET), termogravimetria (TG/DTG), difração de elétrons (SAED) e além disso foram selecionadas três amostras para serem submetidas a testes preliminares de adsorção de ácido húmico. Promoveuse uma síntese verde devido a não utilização de água em grandes quantidades. Amostras de moagem manual obtidas a 10 minutos com 2,0 mL de água adicionada desempenharam resultados positivos similarmente a amostras que foram sintetizadas com menor adição de água e com auxílio de etapa de envelhecimento. A formação das fases HDL foi observada também para em amostras obtidas a 80 e 100 horas de moagem com moinho de bolas horizontal, ao passo que a presença de precursor MgO foi reduzida por volta de 40 horas de moagem. Amostras obtidas a 10 minutos de moagem manual a seco, apresentaram fases intermediárias, indicando a importância da adição de água no processo de síntese. A formação do produto HDL obtido por moagem manual, mesmo que em pequenas quantidades, descarta a utilização de métodos tradicionais de síntese que envolvem soluções, como co-precipitação por exemplo. As bandas de FTIR, as microscopias MET e MEV, a difração de elétrons e as curvas TG/DTG complementaram a discussão acerca da difratometria de raios-X, com destaque para o FTIR que apresentou muitas informações sobre grupos (OH) livres - sem participação em ligações de hidrogênio - típicos de Al(OH)3 e o comportamento de amorfização deste reagente utilizado como precursor. Testes de adsorção revelaram que um dos produtos obtidos por moagem manual apresentou ótima propriedade de adsorção de ácido húmico quando comparado a outras amostras, uma obtida por co-precipitação e outra comercial.São CristóvãoporCiência dos materiaisNanopartículasAlumínioMagnésioÁcido húmicoHidróxido duplo lamelarMecanoquímicaMoagemMoinhoLayered double hydroxidesMechanochemicalHumic acidGriddingMillingENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICASíntese de hidróxido duplo lamelar Mg-Al via rota mecanoquímicainfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisPós-Graduação em Ciência e Engenharia de MateriaisUniversidade Federal de Sergipereponame:Repositório Institucional da UFSinstname:Universidade Federal de Sergipe (UFS)instacron:UFSinfo:eu-repo/semantics/openAccessLICENSElicense.txtlicense.txttext/plain; charset=utf-81475https://ri.ufs.br/jspui/bitstream/riufs/16685/1/license.txt098cbbf65c2c15e1fb2e49c5d306a44cMD51ORIGINALGABRIEL_SOARES_BENTO.pdfGABRIEL_SOARES_BENTO.pdfapplication/pdf1895117https://ri.ufs.br/jspui/bitstream/riufs/16685/2/GABRIEL_SOARES_BENTO.pdf6ccad5590c56bca4c5cdfcff3cdd654fMD52TEXTGABRIEL_SOARES_BENTO.pdf.txtGABRIEL_SOARES_BENTO.pdf.txtExtracted texttext/plain148637https://ri.ufs.br/jspui/bitstream/riufs/16685/3/GABRIEL_SOARES_BENTO.pdf.txta174c4f4378424934017da2dc275fd60MD53THUMBNAILGABRIEL_SOARES_BENTO.pdf.jpgGABRIEL_SOARES_BENTO.pdf.jpgGenerated Thumbnailimage/jpeg1282https://ri.ufs.br/jspui/bitstream/riufs/16685/4/GABRIEL_SOARES_BENTO.pdf.jpg50bd32c39e34cc049bb5bcf631ecabf7MD54riufs/166852022-10-24 14:27:52.415oai:ufs.br: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Repositório InstitucionalPUBhttps://ri.ufs.br/oai/requestrepositorio@academico.ufs.bropendoar:2022-10-24T17:27:52Repositório Institucional da UFS - Universidade Federal de Sergipe (UFS)false |
dc.title.pt_BR.fl_str_mv |
Síntese de hidróxido duplo lamelar Mg-Al via rota mecanoquímica |
title |
Síntese de hidróxido duplo lamelar Mg-Al via rota mecanoquímica |
spellingShingle |
Síntese de hidróxido duplo lamelar Mg-Al via rota mecanoquímica Bento, Gabriel Soares Ciência dos materiais Nanopartículas Alumínio Magnésio Ácido húmico Hidróxido duplo lamelar Mecanoquímica Moagem Moinho Layered double hydroxides Mechanochemical Humic acid Gridding Milling ENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICA |
title_short |
Síntese de hidróxido duplo lamelar Mg-Al via rota mecanoquímica |
title_full |
Síntese de hidróxido duplo lamelar Mg-Al via rota mecanoquímica |
title_fullStr |
Síntese de hidróxido duplo lamelar Mg-Al via rota mecanoquímica |
title_full_unstemmed |
Síntese de hidróxido duplo lamelar Mg-Al via rota mecanoquímica |
title_sort |
Síntese de hidróxido duplo lamelar Mg-Al via rota mecanoquímica |
author |
Bento, Gabriel Soares |
author_facet |
Bento, Gabriel Soares |
author_role |
author |
dc.contributor.author.fl_str_mv |
Bento, Gabriel Soares |
dc.contributor.advisor1.fl_str_mv |
Gimenez, Iara de Fátima |
contributor_str_mv |
Gimenez, Iara de Fátima |
dc.subject.por.fl_str_mv |
Ciência dos materiais Nanopartículas Alumínio Magnésio Ácido húmico Hidróxido duplo lamelar Mecanoquímica Moagem Moinho |
topic |
Ciência dos materiais Nanopartículas Alumínio Magnésio Ácido húmico Hidróxido duplo lamelar Mecanoquímica Moagem Moinho Layered double hydroxides Mechanochemical Humic acid Gridding Milling ENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICA |
dc.subject.eng.fl_str_mv |
Layered double hydroxides Mechanochemical Humic acid Gridding Milling |
dc.subject.cnpq.fl_str_mv |
ENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICA |
description |
The synthesis of layered double hydroxides Mg-Al (LDH Mg-Al) via mechanochemical routes is reported. Manual grinding and horizontal ball milling were using as precursors aluminum hydroxide and magnesium oxide. The parameters of grinding time and addition of water were analyzed. The obtained products were characterized by x-ray diffraction (XRD), fourier transform infared (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (MET), termogravimetry (TG/DTG), electron diffraction (SAED) and in addition, three samples were selected to be submitted to tests of adsorption of humic acid by UV-Visible spectroscopy. A green synthesis was promoted due to the non-use of water in large quantities. Manual grinding samples obtained at 10 minutes of grinding with 2.0 mL of water added positive results simlarly to samples synthesized with the aid of an aging stage. The formation of HDL phases were also observed in samples obtained in 80 hours and 100 hours of grinding with horizontal ball milling, while the presence of crystalline phases of MgO precursor was reduced by around 40 hours of grinding. Samples obtained at 10 minutes of manual dry grinding showed intermediate phases, indicating the importance of adding water in the synthesis process. The formation of the LDH product obtained manually with the addition of water even if in small quantities discards the use of traditional methods involving solutions, such as coprecipitation for example. FTIR bands, MET and SEM microscopies, electron diffraction and TG/DTG curves complemented the discussion about x-ray diffraction, with emphasis on the FTIR that presented information to some free (OH) groups – no participation in hydrogen bonds – characteristics of Al(OH)3 and the amorphization behavior of this reagent used as a precursor. Adsorption testes revealed that one of the products obtained by manual milling showed excellent humic acid adsorption property when compared to other samples, one obtained by co-precipitation and the other commercial. |
publishDate |
2022 |
dc.date.accessioned.fl_str_mv |
2022-10-24T17:27:52Z |
dc.date.available.fl_str_mv |
2022-10-24T17:27:52Z |
dc.date.issued.fl_str_mv |
2022-08-26 |
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 |
BENTO, Gabriel Soares. Síntese de hidróxido duplo lamelar Mg-Al via rota mecanoquímica. 2022. 91 f. Dissertação (Mestrado em Ciência e Engenharia de Materiais) – Universidade Federal de Sergipe, São Cristóvão, 2022. |
dc.identifier.uri.fl_str_mv |
http://ri.ufs.br/jspui/handle/riufs/16685 |
identifier_str_mv |
BENTO, Gabriel Soares. Síntese de hidróxido duplo lamelar Mg-Al via rota mecanoquímica. 2022. 91 f. Dissertação (Mestrado em Ciência e Engenharia de Materiais) – Universidade Federal de Sergipe, São Cristóvão, 2022. |
url |
http://ri.ufs.br/jspui/handle/riufs/16685 |
dc.language.iso.fl_str_mv |
por |
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por |
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info:eu-repo/semantics/openAccess |
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openAccess |
dc.publisher.program.fl_str_mv |
Pós-Graduação em Ciência e Engenharia de Materiais |
dc.publisher.initials.fl_str_mv |
Universidade Federal de Sergipe |
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