Obtenção de nanossílica funcionalizada visando o uso como aditivo em misturas cimentícias

Detalhes bibliográficos
Autor(a) principal: Sousa, Ionara Pereira da Silva
Data de Publicação: 2017
Tipo de documento: Dissertação
Idioma: por
Título da fonte: Repositório Institucional da UFG
Texto Completo: http://repositorio.bc.ufg.br/tede/handle/tede/7806
Resumo: The basic science on cements and concretes has incorporated research related to the understanding of the effects of the addition of nanosilica, and more recently functionalized nanosilicas, on the properties of cement pastes, mortars and concretes. In this context, the aim of this work was to prepare amino-functionalized nanosilicas from a commercial nanosilica (NS), provided as an aqueous colloidal suspension, by employing 3-aminopropiltrietoxissilano (APTS) as reactant, and to evaluate the characteristics of the samples. The functionalization reactions were performed in a biphasic system composed of dichloromethane and water, and employing different APTS/NS molar ratios. The materials were obtained as aqueous suspensions and their characteristics were evaluated at pH 4, 7 e 10. The functionalization of NS was evidenced by the presence of infrared bands associated to the aminopropyl group. Bands associated to silanol (-SiOH) and alcoxide (Si-OCH2CH3) groups were observed indicating that the hydrolysis and condensation reactions were not complete. The 29Si NMR signals of Si-C bonds confirmed the functionalization. The thermogravimetric curves indicated an increase of the amount of aminopropyl groups incorporated on NS as the APTS/NS ratio increased. Transmission electron microscopy images showed an increase in the mean particle sizes after functionalization. The aqueous suspended nanoparticles showed a positive zeta potential at pH 4 (+23 to +27 mV) and at pH 7 (+14 to +29 mV), indicating the presence of protonated amine groups. The zeta potential at pH 10 was weakly negative (-0.10 to -7,6 mV) for the samples prepared from the lower APTS/NS molar ratios (7.1 and 14.2 x 10-2), and still positive (+11 and +15 mV) for those prepared from the higher molar ratios (28.5 and 42.7 x 10-2), suggesting the existence of a higher amount of superficial amino groups within the latter. The mean hydrodynamic radius of the functionalized particles were greater (22 a 281 nm) than that of the NS (12 nm) at all pH values, with superior values for suspended particles at pH 10, particularly for samples prepared from the lower APTS/NS ratios. The amount of aggregates of bigger size (~100 to 2000 nm) was greater for samples prepared from the lower APTS/NS ratios. These variable characteristics are interesting for comparative studies involving the effects of the addition of these suspensions in cement pastes over the microstructure and properties of the resulting materials.
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spelling Sartoratto, Patrícia Pommé Confessorihttp://lattes.cnpq.br/9777959525393785Rêgo, João Henrique da SilvaMartins, Paulo Robertohttp://lattes.cnpq.br/7282834278937260Sousa, Ionara Pereira da Silva2017-09-27T11:09:36Z2017-09-15SOUSA, I. P. S. Obtenção de nanossílica funcionalizada visando o uso como aditivo em misturas cimentícias. 2017. 72 f. Dissertação (Mestrado em Química) - Universidade Federal de Goiás, Goiânia, 2017.http://repositorio.bc.ufg.br/tede/handle/tede/7806ark:/38995/0013000008nbsThe basic science on cements and concretes has incorporated research related to the understanding of the effects of the addition of nanosilica, and more recently functionalized nanosilicas, on the properties of cement pastes, mortars and concretes. In this context, the aim of this work was to prepare amino-functionalized nanosilicas from a commercial nanosilica (NS), provided as an aqueous colloidal suspension, by employing 3-aminopropiltrietoxissilano (APTS) as reactant, and to evaluate the characteristics of the samples. The functionalization reactions were performed in a biphasic system composed of dichloromethane and water, and employing different APTS/NS molar ratios. The materials were obtained as aqueous suspensions and their characteristics were evaluated at pH 4, 7 e 10. The functionalization of NS was evidenced by the presence of infrared bands associated to the aminopropyl group. Bands associated to silanol (-SiOH) and alcoxide (Si-OCH2CH3) groups were observed indicating that the hydrolysis and condensation reactions were not complete. The 29Si NMR signals of Si-C bonds confirmed the functionalization. The thermogravimetric curves indicated an increase of the amount of aminopropyl groups incorporated on NS as the APTS/NS ratio increased. Transmission electron microscopy images showed an increase in the mean particle sizes after functionalization. The aqueous suspended nanoparticles showed a positive zeta potential at pH 4 (+23 to +27 mV) and at pH 7 (+14 to +29 mV), indicating the presence of protonated amine groups. The zeta potential at pH 10 was weakly negative (-0.10 to -7,6 mV) for the samples prepared from the lower APTS/NS molar ratios (7.1 and 14.2 x 10-2), and still positive (+11 and +15 mV) for those prepared from the higher molar ratios (28.5 and 42.7 x 10-2), suggesting the existence of a higher amount of superficial amino groups within the latter. The mean hydrodynamic radius of the functionalized particles were greater (22 a 281 nm) than that of the NS (12 nm) at all pH values, with superior values for suspended particles at pH 10, particularly for samples prepared from the lower APTS/NS ratios. The amount of aggregates of bigger size (~100 to 2000 nm) was greater for samples prepared from the lower APTS/NS ratios. These variable characteristics are interesting for comparative studies involving the effects of the addition of these suspensions in cement pastes over the microstructure and properties of the resulting materials.A ciência básica na área de cimentos e concretos tem incorporado pesquisas relacionadas ao entendimento dos efeitos da adição de nanossílica e, mais recentemente, de nanossílica funcionalizada nas propriedades de pastas de cimento, argamassas e concretos. Neste contexto, o objetivo deste trabalho foi preparar nanossílicas funcionalizadas com grupos amina a partir de uma nanossílica comercial (NS), fornecida como uma suspensão coloidal aquosa, empregando-se o reagente 3-aminopropiltrietoxissilano (APTS) e avaliar as características das amostras obtidas. As reações de funcionalização foram realizadas em um sistema reacional bifásico constituído de diclorometano e água, empregando-se diferentes razões molares APTS/NS. Os materiais foram obtidos como suspensões aquosas, cujas características foram avaliadas em pH 4, 7 e 10. A funcionalização da NS foi evidenciada pela presença das bandas relativas ao grupo aminopropil nos espectros de infravermelho, onde também foram observadas bandas dos grupos silanol (-SiOH) e alcóxido (Si-OCH2CH3), indicando que as reações de hidrólise e condensação não foram completas. Os sinais nos espectros de RMN de 29Si característicos de ligações Si-C confirmaram a funcionalização. As curvas termogravimétricas indicaram que houve aumento no teor de grupos aminopropil incorporados à NS com o aumento da razão APTS/NS empregada. As imagens de microscopia eletrônica de transmissão mostraram um aumento do tamanho médio das partículas após a funcionalização. As nanopartículas funcionalizadas em suspensão aquosa apresentaram potencial zeta positivo em pH 4 (+23 a +27 mV) e em pH 7 (+14 a +29 mV), indicando a presença de grupos amina protonados. Já em pH 10, o potencial zeta foi fracamente negativo (-0,10 a -7,6 mV) para amostras preparadas com menor razão APTS/NS (7,1 e 14,2 x 10-2), e positivos (+11 e +15 mV) para aquelas preparadas com razão molar maior (28,5 e 42,7 x 10-2), sugerindo um maior teor de grupos amina superficiais nestas últimas. Os raios hidrodinâmicos médios das partículas funcionalizadas foram maiores (22 a 281 nm) do que o da NS (12 nm) para todos os valores de pH, com valores maiores para partículas suspensas em pH 10. O teor de agregados de maior tamanho (~100 a 2000 nm) foi maior para as amostras preparadas com menor razão APTS/NS. Essas características variadas são interessantes para estudos comparativos dos efeitos de adição dessas suspensões em pastas de cimento, sobre a microestrutura e propriedades dos materiais resultantes.Submitted by Luciana Ferreira (lucgeral@gmail.com) on 2017-09-27T11:09:10Z No. of bitstreams: 2 Dissertação - Ionara Pereira da Silva Sousa - 2017.pdf: 5120392 bytes, checksum: 786f15ae0e6cf83fa9560a114e84f6a2 (MD5) license_rdf: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5)Approved for entry into archive by Luciana Ferreira (lucgeral@gmail.com) on 2017-09-27T11:09:36Z (GMT) No. of bitstreams: 2 Dissertação - Ionara Pereira da Silva Sousa - 2017.pdf: 5120392 bytes, checksum: 786f15ae0e6cf83fa9560a114e84f6a2 (MD5) license_rdf: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5)Made available in DSpace on 2017-09-27T11:09:36Z (GMT). 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dc.title.eng.fl_str_mv Obtenção de nanossílica funcionalizada visando o uso como aditivo em misturas cimentícias
title Obtenção de nanossílica funcionalizada visando o uso como aditivo em misturas cimentícias
spellingShingle Obtenção de nanossílica funcionalizada visando o uso como aditivo em misturas cimentícias
Sousa, Ionara Pereira da Silva
Nanossílica
3-aminopropiltrietoxissilano nanosilica
Funcionalização
Functionalization
3-aminopropyltriethoxysilane
Nanosilica
CIENCIAS EXATAS E DA TERRA::QUIMICA
title_short Obtenção de nanossílica funcionalizada visando o uso como aditivo em misturas cimentícias
title_full Obtenção de nanossílica funcionalizada visando o uso como aditivo em misturas cimentícias
title_fullStr Obtenção de nanossílica funcionalizada visando o uso como aditivo em misturas cimentícias
title_full_unstemmed Obtenção de nanossílica funcionalizada visando o uso como aditivo em misturas cimentícias
title_sort Obtenção de nanossílica funcionalizada visando o uso como aditivo em misturas cimentícias
author Sousa, Ionara Pereira da Silva
author_facet Sousa, Ionara Pereira da Silva
author_role author
dc.contributor.advisor1.fl_str_mv Sartoratto, Patrícia Pommé Confessori
dc.contributor.advisor1Lattes.fl_str_mv http://lattes.cnpq.br/9777959525393785
dc.contributor.referee1.fl_str_mv Rêgo, João Henrique da Silva
dc.contributor.referee2.fl_str_mv Martins, Paulo Roberto
dc.contributor.authorLattes.fl_str_mv http://lattes.cnpq.br/7282834278937260
dc.contributor.author.fl_str_mv Sousa, Ionara Pereira da Silva
contributor_str_mv Sartoratto, Patrícia Pommé Confessori
Rêgo, João Henrique da Silva
Martins, Paulo Roberto
dc.subject.por.fl_str_mv Nanossílica
3-aminopropiltrietoxissilano nanosilica
Funcionalização
topic Nanossílica
3-aminopropiltrietoxissilano nanosilica
Funcionalização
Functionalization
3-aminopropyltriethoxysilane
Nanosilica
CIENCIAS EXATAS E DA TERRA::QUIMICA
dc.subject.eng.fl_str_mv Functionalization
3-aminopropyltriethoxysilane
Nanosilica
dc.subject.cnpq.fl_str_mv CIENCIAS EXATAS E DA TERRA::QUIMICA
description The basic science on cements and concretes has incorporated research related to the understanding of the effects of the addition of nanosilica, and more recently functionalized nanosilicas, on the properties of cement pastes, mortars and concretes. In this context, the aim of this work was to prepare amino-functionalized nanosilicas from a commercial nanosilica (NS), provided as an aqueous colloidal suspension, by employing 3-aminopropiltrietoxissilano (APTS) as reactant, and to evaluate the characteristics of the samples. The functionalization reactions were performed in a biphasic system composed of dichloromethane and water, and employing different APTS/NS molar ratios. The materials were obtained as aqueous suspensions and their characteristics were evaluated at pH 4, 7 e 10. The functionalization of NS was evidenced by the presence of infrared bands associated to the aminopropyl group. Bands associated to silanol (-SiOH) and alcoxide (Si-OCH2CH3) groups were observed indicating that the hydrolysis and condensation reactions were not complete. The 29Si NMR signals of Si-C bonds confirmed the functionalization. The thermogravimetric curves indicated an increase of the amount of aminopropyl groups incorporated on NS as the APTS/NS ratio increased. Transmission electron microscopy images showed an increase in the mean particle sizes after functionalization. The aqueous suspended nanoparticles showed a positive zeta potential at pH 4 (+23 to +27 mV) and at pH 7 (+14 to +29 mV), indicating the presence of protonated amine groups. The zeta potential at pH 10 was weakly negative (-0.10 to -7,6 mV) for the samples prepared from the lower APTS/NS molar ratios (7.1 and 14.2 x 10-2), and still positive (+11 and +15 mV) for those prepared from the higher molar ratios (28.5 and 42.7 x 10-2), suggesting the existence of a higher amount of superficial amino groups within the latter. The mean hydrodynamic radius of the functionalized particles were greater (22 a 281 nm) than that of the NS (12 nm) at all pH values, with superior values for suspended particles at pH 10, particularly for samples prepared from the lower APTS/NS ratios. The amount of aggregates of bigger size (~100 to 2000 nm) was greater for samples prepared from the lower APTS/NS ratios. These variable characteristics are interesting for comparative studies involving the effects of the addition of these suspensions in cement pastes over the microstructure and properties of the resulting materials.
publishDate 2017
dc.date.accessioned.fl_str_mv 2017-09-27T11:09:36Z
dc.date.issued.fl_str_mv 2017-09-15
dc.type.status.fl_str_mv info:eu-repo/semantics/publishedVersion
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dc.identifier.citation.fl_str_mv SOUSA, I. P. S. Obtenção de nanossílica funcionalizada visando o uso como aditivo em misturas cimentícias. 2017. 72 f. Dissertação (Mestrado em Química) - Universidade Federal de Goiás, Goiânia, 2017.
dc.identifier.uri.fl_str_mv http://repositorio.bc.ufg.br/tede/handle/tede/7806
dc.identifier.dark.fl_str_mv ark:/38995/0013000008nbs
identifier_str_mv SOUSA, I. P. S. Obtenção de nanossílica funcionalizada visando o uso como aditivo em misturas cimentícias. 2017. 72 f. Dissertação (Mestrado em Química) - Universidade Federal de Goiás, Goiânia, 2017.
ark:/38995/0013000008nbs
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language por
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600
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publisher.none.fl_str_mv Universidade Federal de Goiás
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MD5
repository.name.fl_str_mv Repositório Institucional da UFG - Universidade Federal de Goiás (UFG)
repository.mail.fl_str_mv tasesdissertacoes.bc@ufg.br
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