Preparação e caracterização de nanocompósitos poliméricos baseados em poliuretano termorrígido e nanotubos de carbono de paredes múltiplas

Detalhes bibliográficos
Ano de defesa: 2015
Autor(a) principal: Mayara Cele Gonçalves Santos
Orientador(a): Não Informado pela instituição
Banca de defesa: Não Informado pela instituição
Tipo de documento: Dissertação
Tipo de acesso: Acesso aberto
Idioma: por
Instituição de defesa: Universidade Federal de Minas Gerais
Programa de Pós-Graduação: Não Informado pela instituição
Departamento: Não Informado pela instituição
País: Não Informado pela instituição
Palavras-chave em Português:
Link de acesso: https://hdl.handle.net/1843/SFSA-A44QJA
Resumo: The main goal of this work is to verify the improvement of thermal and mechanical properties on an elastomeric thermoset polyurethane matrix through the preparation of polymeric nanocomposites with multi-walled carbon nanotubes (unmodified and chemically modified). For that, stable suspensions of nanotubes were prepared (with different concentrations) in poly (tetramethylene ether glycol) with the employment of a roll mill with micrometric separation. It were used carbon nanotubes synthesized at UFMG (Laboratory of Nanomaterials/ Physics Department) that have been modified by acid treatment and by the insertion of isocyanate groups. Images obtained by scanning and transmission electronic microscopies showed that the developed procedures did not cause significant change in the aspect ratio of the nanotubes. Thermogravimetric data indicated that the amount of oxygenated and isocyanate groups placed on the surface of the nanotubes were of the order 7% and 36%, respectively. In a subsequent step, the nanotube/polyol suspensions were reacted with 2,4-toluene diisocyanate and 1,4-butanediol for the production of polyurethane prepolymers. The processing conditions and the quantity of reagents had been developed for keep the free NCO contents in the prepolymers in the range from 7.2 to 7.8. The nanocomposites were prepared by the prepolymer reaction (via free NCO groups) with the 4,4-methylene-bis-ortho-chloroaniline cure agent. Images at different scales obtained by optical, and scanning and transmission electronic microscopies demonstrated that, despite of the existence of millimeter aggregated of nanotubes, the nanofiller was dispersed at the micro and nanometric scales. In all composites there are small regions with aggregated nanotubes, besides of small bundles and isolated nanotubes throughout the matrix. The nanotubes were covered by the matrix, suggesting good adhesion filler/PUE, especially in the composites prepared with acid and isocyanate modified nanotubes. The nanotubes are "sewing" the PUE matrix. This is an important feature for their effect as mechanical reinforcement. Thermogravimetry results showed that MWCNTs dont have (in any concentration or type of nanotube) major influence on the thermal stability and degradation mechanism of the polymeric matrix. The tensile, tear and hardness tests showed that the produced nanocomposites presented significant improvements in all analyzed properties. The best results were verified for the composite prepared with 0.26 wt% of isocyanate-modified nanotubes. In this composite it was verified an increase of 17% in elasticity modulus, and 23% in tear resistance with maintenance of the tensile strength alongation at break, tenacity and hardness. The procedures of modification of nanotubes surface, dispersion in polyol and preparation of the prepolymer developed in this study allowed the production of nanocomposites without major impact on the value chain of the polymer and that can be used in applications requiring large mechanical loads.
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spelling 2019-08-12T23:44:47Z2025-09-08T23:48:42Z2019-08-12T23:44:47Z2015-07-30https://hdl.handle.net/1843/SFSA-A44QJAThe main goal of this work is to verify the improvement of thermal and mechanical properties on an elastomeric thermoset polyurethane matrix through the preparation of polymeric nanocomposites with multi-walled carbon nanotubes (unmodified and chemically modified). For that, stable suspensions of nanotubes were prepared (with different concentrations) in poly (tetramethylene ether glycol) with the employment of a roll mill with micrometric separation. It were used carbon nanotubes synthesized at UFMG (Laboratory of Nanomaterials/ Physics Department) that have been modified by acid treatment and by the insertion of isocyanate groups. Images obtained by scanning and transmission electronic microscopies showed that the developed procedures did not cause significant change in the aspect ratio of the nanotubes. Thermogravimetric data indicated that the amount of oxygenated and isocyanate groups placed on the surface of the nanotubes were of the order 7% and 36%, respectively. In a subsequent step, the nanotube/polyol suspensions were reacted with 2,4-toluene diisocyanate and 1,4-butanediol for the production of polyurethane prepolymers. The processing conditions and the quantity of reagents had been developed for keep the free NCO contents in the prepolymers in the range from 7.2 to 7.8. The nanocomposites were prepared by the prepolymer reaction (via free NCO groups) with the 4,4-methylene-bis-ortho-chloroaniline cure agent. Images at different scales obtained by optical, and scanning and transmission electronic microscopies demonstrated that, despite of the existence of millimeter aggregated of nanotubes, the nanofiller was dispersed at the micro and nanometric scales. In all composites there are small regions with aggregated nanotubes, besides of small bundles and isolated nanotubes throughout the matrix. The nanotubes were covered by the matrix, suggesting good adhesion filler/PUE, especially in the composites prepared with acid and isocyanate modified nanotubes. The nanotubes are "sewing" the PUE matrix. This is an important feature for their effect as mechanical reinforcement. Thermogravimetry results showed that MWCNTs dont have (in any concentration or type of nanotube) major influence on the thermal stability and degradation mechanism of the polymeric matrix. The tensile, tear and hardness tests showed that the produced nanocomposites presented significant improvements in all analyzed properties. The best results were verified for the composite prepared with 0.26 wt% of isocyanate-modified nanotubes. In this composite it was verified an increase of 17% in elasticity modulus, and 23% in tear resistance with maintenance of the tensile strength alongation at break, tenacity and hardness. The procedures of modification of nanotubes surface, dispersion in polyol and preparation of the prepolymer developed in this study allowed the production of nanocomposites without major impact on the value chain of the polymer and that can be used in applications requiring large mechanical loads.Universidade Federal de Minas GeraisPoliuretano termorrígido elastoméricoNanocompósitosDispersão de nanotubos de carbono modificadosPropriedades mecânicasNanotubos de carbonoPoliuretanas Propriedades mecânicasFísico-químicaCompósitos poliméricosNanotubos de carbonoPropriedades mecanicasNanotecnologiaPreparação e caracterização de nanocompósitos poliméricos baseados em poliuretano termorrígido e nanotubos de carbono de paredes múltiplasinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisMayara Cele Gonçalves Santosinfo:eu-repo/semantics/openAccessporreponame:Repositório Institucional da UFMGinstname:Universidade Federal de Minas Gerais (UFMG)instacron:UFMGRodrigo Lassarote LavalClaudinei Rezende CaladoLuiz Carlos Alves de OliveiraO trabalho de mestrado desenvolvido teve como objetivo principal a melhoria das propriedades térmicas e mecânicas de uma matriz poliuretano termorrígido elastomérico por meio da preparação de nanocompósitos poliméricos com nanotubos de carbono de paredes múltiplas (não modificados e modificados quimicamente). Para isso, foram preparadas suspensões estáveis dos nanotubos (com diferentes concentrações) em poli(tetrametileno éter glicol) com o emprego de moinho de rolos com separação micrométrica. Utilizou-se nanotubos de carbono sintetizados na UFMG (Laboratório de Nanomateriais do Departamento de Física) que foram modificados por tratamento ácido e pela inserção de grupos isocianato. Imagens obtidas por microscopias eletrônicas de varredura e transmissão mostraram que os procedimentos desenvolvidos não causaram alteração significativa na razão de aspecto dos nanotubos. Dados de termogravimetria indicaram que os teores de grupos oxigenados e de grupos isocianato inseridos na superfície dos nanotubos foram da ordem de 7% e 36%, respectivamente. Numa etapa posterior, as suspensões nanotubo/poliol foram reagidas com 2,4-tolueno diisocianato e 1.4-butanodiol para a produção de pré-polímeros de poliuretano. As condições de processamento e quantidade dos reagentes foram desenvolvidas para que o teor de NCO livre desses pré-polímeros ficasse na faixa de 7,2 a 7,8. Os nanocompósitos foram preparados pela reação do pré-polímero (via grupos NCO livres) com o agente de cura 4,4-metileno-bis-orto-cloro-anilina. Imagens em diferentes escalas obtidas por microscopias ótica, eletrônicas de varredura e transmissão demostraram que embora existam agregados milimétricos de nanotubos, houve dispersão da nanocarga nas escalas micro e nanométricas. Em todos os compósitos existem pequenas regiões com agregados de nanotubos, além de em pequenos feixes e nanotubos isolados ao longo da matriz. Os nanotubos foram recobertos pela matriz, o que sugere boa adesão carga/PUE, principalmente nos compósitos com nanotubos modificados por tratamento ácido e com isocianato. Os nanotubos estão ¿costurando¿ a matriz de PUE, uma característica importante para seu efeito como reforço mecânico. Resultados de termogravimetria mostraram que os MWCNTs não exercem (para nenhuma concentração ou tipo de nanotubo) grande influência na estabilidade térmica e no mecanismo de degradação da matriz polimérica. Os ensaios mecânicos de tração, rasgo e dureza mostraram que os nanocompósitos produzidos apresentaram melhoras significativas em todas as propriedades analisadas. Os melhores resultados foram encontrados para o compósito preparado com 0,26% (em massa) de nanotubos modificados com isocianato, no qual pode-se verificar aumentos de até 17% no módulo de elasticidade, 23% na resistência ao rasgo com manutenção da resistência à tração, alongamento na ruptura, tenacidade e dureza. Os procedimentos de modificação da superfície dos nanotubos, dispersão em poliol e preparação de pré-polímero desenvolvidos neste trabalho permitem a produção de nanocompósitos sem grandes impactos na cadeia de valores do polímero e que podem ser utilizados em aplicações que requeiram grande solicitação mecânica.UFMGORIGINALdisserta__o___mayara_cele_gon_alves_santos.pdfapplication/pdf3960844https://repositorio.ufmg.br//bitstreams/9e7595d8-1796-4b04-9d40-fbc0afc08dd2/download580928edb90b6160519b7f4b06eb73acMD51trueAnonymousREADTEXTdisserta__o___mayara_cele_gon_alves_santos.pdf.txttext/plain207833https://repositorio.ufmg.br//bitstreams/20629bd9-71ed-45ea-8a11-268fa71c3f2b/download06ac4d9170da9a48eb476f26fb1765acMD52falseAnonymousREAD1843/SFSA-A44QJA2025-09-08 20:48:42.894open.accessoai:repositorio.ufmg.br:1843/SFSA-A44QJAhttps://repositorio.ufmg.br/Repositório InstitucionalPUBhttps://repositorio.ufmg.br/oairepositorio@ufmg.bropendoar:2025-09-08T23:48:42Repositório Institucional da UFMG - Universidade Federal de Minas Gerais (UFMG)false
dc.title.none.fl_str_mv Preparação e caracterização de nanocompósitos poliméricos baseados em poliuretano termorrígido e nanotubos de carbono de paredes múltiplas
title Preparação e caracterização de nanocompósitos poliméricos baseados em poliuretano termorrígido e nanotubos de carbono de paredes múltiplas
spellingShingle Preparação e caracterização de nanocompósitos poliméricos baseados em poliuretano termorrígido e nanotubos de carbono de paredes múltiplas
Mayara Cele Gonçalves Santos
Poliuretanas Propriedades mecânicas
Físico-química
Compósitos poliméricos
Nanotubos de carbono
Propriedades mecanicas
Nanotecnologia
Poliuretano termorrígido elastomérico
Nanocompósitos
Dispersão de nanotubos de carbono modificados
Propriedades mecânicas
Nanotubos de carbono
title_short Preparação e caracterização de nanocompósitos poliméricos baseados em poliuretano termorrígido e nanotubos de carbono de paredes múltiplas
title_full Preparação e caracterização de nanocompósitos poliméricos baseados em poliuretano termorrígido e nanotubos de carbono de paredes múltiplas
title_fullStr Preparação e caracterização de nanocompósitos poliméricos baseados em poliuretano termorrígido e nanotubos de carbono de paredes múltiplas
title_full_unstemmed Preparação e caracterização de nanocompósitos poliméricos baseados em poliuretano termorrígido e nanotubos de carbono de paredes múltiplas
title_sort Preparação e caracterização de nanocompósitos poliméricos baseados em poliuretano termorrígido e nanotubos de carbono de paredes múltiplas
author Mayara Cele Gonçalves Santos
author_facet Mayara Cele Gonçalves Santos
author_role author
dc.contributor.author.fl_str_mv Mayara Cele Gonçalves Santos
dc.subject.por.fl_str_mv Poliuretanas Propriedades mecânicas
Físico-química
Compósitos poliméricos
Nanotubos de carbono
Propriedades mecanicas
Nanotecnologia
topic Poliuretanas Propriedades mecânicas
Físico-química
Compósitos poliméricos
Nanotubos de carbono
Propriedades mecanicas
Nanotecnologia
Poliuretano termorrígido elastomérico
Nanocompósitos
Dispersão de nanotubos de carbono modificados
Propriedades mecânicas
Nanotubos de carbono
dc.subject.other.none.fl_str_mv Poliuretano termorrígido elastomérico
Nanocompósitos
Dispersão de nanotubos de carbono modificados
Propriedades mecânicas
Nanotubos de carbono
description The main goal of this work is to verify the improvement of thermal and mechanical properties on an elastomeric thermoset polyurethane matrix through the preparation of polymeric nanocomposites with multi-walled carbon nanotubes (unmodified and chemically modified). For that, stable suspensions of nanotubes were prepared (with different concentrations) in poly (tetramethylene ether glycol) with the employment of a roll mill with micrometric separation. It were used carbon nanotubes synthesized at UFMG (Laboratory of Nanomaterials/ Physics Department) that have been modified by acid treatment and by the insertion of isocyanate groups. Images obtained by scanning and transmission electronic microscopies showed that the developed procedures did not cause significant change in the aspect ratio of the nanotubes. Thermogravimetric data indicated that the amount of oxygenated and isocyanate groups placed on the surface of the nanotubes were of the order 7% and 36%, respectively. In a subsequent step, the nanotube/polyol suspensions were reacted with 2,4-toluene diisocyanate and 1,4-butanediol for the production of polyurethane prepolymers. The processing conditions and the quantity of reagents had been developed for keep the free NCO contents in the prepolymers in the range from 7.2 to 7.8. The nanocomposites were prepared by the prepolymer reaction (via free NCO groups) with the 4,4-methylene-bis-ortho-chloroaniline cure agent. Images at different scales obtained by optical, and scanning and transmission electronic microscopies demonstrated that, despite of the existence of millimeter aggregated of nanotubes, the nanofiller was dispersed at the micro and nanometric scales. In all composites there are small regions with aggregated nanotubes, besides of small bundles and isolated nanotubes throughout the matrix. The nanotubes were covered by the matrix, suggesting good adhesion filler/PUE, especially in the composites prepared with acid and isocyanate modified nanotubes. The nanotubes are "sewing" the PUE matrix. This is an important feature for their effect as mechanical reinforcement. Thermogravimetry results showed that MWCNTs dont have (in any concentration or type of nanotube) major influence on the thermal stability and degradation mechanism of the polymeric matrix. The tensile, tear and hardness tests showed that the produced nanocomposites presented significant improvements in all analyzed properties. The best results were verified for the composite prepared with 0.26 wt% of isocyanate-modified nanotubes. In this composite it was verified an increase of 17% in elasticity modulus, and 23% in tear resistance with maintenance of the tensile strength alongation at break, tenacity and hardness. The procedures of modification of nanotubes surface, dispersion in polyol and preparation of the prepolymer developed in this study allowed the production of nanocomposites without major impact on the value chain of the polymer and that can be used in applications requiring large mechanical loads.
publishDate 2015
dc.date.issued.fl_str_mv 2015-07-30
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2025-09-08T23:48:42Z
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