Uso da RMN no estudo da despolimerização de poliuretano rígido
Autor(a) principal: | |
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Data de Publicação: | 2019 |
Tipo de documento: | Dissertação |
Idioma: | por |
Título da fonte: | Repositório Institucional da Universidade Federal do Espírito Santo (riUfes) |
Texto Completo: | http://repositorio.ufes.br/handle/10/11272 |
Resumo: | Polyurethanes (PUs) have been widely used in several trade sections. Thereby, large amounts of waste are produced and need to be correctly disposed off. Research on this theme has been helping industries to apply recycling processes that are cheap and efficient. In this work, the glycolysis of a rigid PU was performed using different catalysts. The catalysts used was: a tensoactive (CTAB), the NaOH, two ionics liquids (1-butyl-3-methylimidazole trichloromanganate and 1-butyl-3-methylimidazole trichlorozincate), and four Niobium salts (niobium pentoxide, niobium oxidehydrated, niobium pentachloride and niobium ammoniacal oxalate). 1H NMR technique was used to obtain the rate of PU depolymerization. Also was used the technique diffusion ordered spectroscopy 1H NMR (DOSY-NMR) that assisted in the identification composition of the mixture of products. In the glycolysis, glycerol (GCL) and diethylene glycol (DEG) were tested as glycolysis agents. The PU was synthesized to be free of additives in the depolymerization process, and its characterization was performed using infrared spectroscopy (FTIR) and 1H NMR spectroscopy analyses. The conversion rate provides information about which catalyst has the better catalytic activity. The use of NaOH as a catalyst presented conversion rate of 100 % in 30 min of reaction, as is already known in the literature, and the DOSY-NMR spectrum provided information about products that didn’t perceptible only by 1H NMR spectrum. Ionic liquids (LIs) as catalysts, presented conversion near of 80 % in 1h of reaction, which can be improved by modifying the reaction conditions. To determine the composition of the mixture of products in the depolymerization reaction, diffusion ordered spectroscopy 1H NMR (DOSY-NMR) was used. The Niobium salts had non-catalytic behavior, because they showed conversion rate lower than uncatalyzed reaction. DOSY-NMR indicated a complex mixture of reaction by-products, differently from the 1H NMR data, which indicated the formation of a simple diamine-terminated by-product. |
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SILVA FILHO, Eloi Alves daCunha Neto, ÁlvaroMaioli, Juliana ProlicianoFreitas, Marcos Benedito José Geraldo deAlmeida, Luiz Carlos Pimentel2019-06-27T02:05:06Z2019-06-262019-06-27T02:05:06Z2019-03-26Polyurethanes (PUs) have been widely used in several trade sections. Thereby, large amounts of waste are produced and need to be correctly disposed off. Research on this theme has been helping industries to apply recycling processes that are cheap and efficient. In this work, the glycolysis of a rigid PU was performed using different catalysts. The catalysts used was: a tensoactive (CTAB), the NaOH, two ionics liquids (1-butyl-3-methylimidazole trichloromanganate and 1-butyl-3-methylimidazole trichlorozincate), and four Niobium salts (niobium pentoxide, niobium oxidehydrated, niobium pentachloride and niobium ammoniacal oxalate). 1H NMR technique was used to obtain the rate of PU depolymerization. Also was used the technique diffusion ordered spectroscopy 1H NMR (DOSY-NMR) that assisted in the identification composition of the mixture of products. In the glycolysis, glycerol (GCL) and diethylene glycol (DEG) were tested as glycolysis agents. The PU was synthesized to be free of additives in the depolymerization process, and its characterization was performed using infrared spectroscopy (FTIR) and 1H NMR spectroscopy analyses. The conversion rate provides information about which catalyst has the better catalytic activity. The use of NaOH as a catalyst presented conversion rate of 100 % in 30 min of reaction, as is already known in the literature, and the DOSY-NMR spectrum provided information about products that didn’t perceptible only by 1H NMR spectrum. Ionic liquids (LIs) as catalysts, presented conversion near of 80 % in 1h of reaction, which can be improved by modifying the reaction conditions. To determine the composition of the mixture of products in the depolymerization reaction, diffusion ordered spectroscopy 1H NMR (DOSY-NMR) was used. The Niobium salts had non-catalytic behavior, because they showed conversion rate lower than uncatalyzed reaction. DOSY-NMR indicated a complex mixture of reaction by-products, differently from the 1H NMR data, which indicated the formation of a simple diamine-terminated by-product.Os poliuretanos (PUs) vem sendo utilizados cada vez mais em diversos setores do comércio. Com isso, grande quantidade de resíduos são gerados e precisam ser descartados de forma correta. As pesquisas neste campo vêm auxiliando indústrias a aplicarem processos de reciclagem que sejam baratos e com bons rendimentos. Neste trabalho, realizou-se a glicólise de um PU rígido empregando-se diferentes catalisadores. Os catalisadores utilizados foram: um tensoativo (CTAB), o NaOH, dois líquidos iônicos (tricloromanganato de 1-butil-3-metilimidazol e triclorozincato de 1-butil-3-metilimidazol), e quatro sais de Nióbios (óxido de nióbio, óxido de nióbio hidratado, cloreto de nióbio e oxalato amoniacal de nióbio). A técnica de RMN de 1H foi utilizada para a determinação da taxa de despolimerização do PU. Também foi utilizada a técnica RMN de 1H ordenada pela difusão (DOSY), que auxiliou na identificação da composição da mistura do produto. Na glicólise, foram testados glicerol (GCL) e dietileno glicol (DEG) como agente de glicólise. O PU foi sintetizado com a finalidade de se apresentar livre de aditivos no processo de despolimerização. A caracterização do PU foi feita por espectroscopia de infravermelho (FTIR) e de RMN de 1H. A taxa de conversão proporcionou sabermos qual catalisador tem melhor atividade catalítica. O NaOH como catalisador apresentou taxa de conversão de 100 % em 30 min de reação, como já é conhecido na literatura, e os espectros DOSY proporcionou observar produtos que não foram perceptíveis apenas pelo espectro de RMN de 1H. Os Líquidos Iônicos utilizados como catalisadores, apresentaram conversão de quase 80 % em 1h de reação, que podem ser melhorados modificando condições de reações. Os sais de Nióbio tiveram comportamento não catalítico, pois apresentaram taxa de conversão menor que a reação não catalisada. A RMN-DOSY indicou uma mistura complexa de subprodutos da reação, diferentemente do que os dados de RMN de 1H indicaram como sendo a formação de um subproduto simples com terminação de diamina.TextMAIOLI, Juliana Proliciano. Uso da RMN no estudo da despolimerização de poliuretano rígido. 2019. 71 f. Dissertação (Mestrado em Química) – Universidade Federal do Espírito Santo, Centro de Ciências Exatas, Vitória, 2019.http://repositorio.ufes.br/handle/10/11272porUniversidade Federal do Espírito SantoMestrado em QuímicaPrograma de Pós-Graduação em QuímicaUFESBRCentro de Ciências ExatasGlycolysisGlycerolGlicóliseGlicerolPoliuretanasRessonância magnética nuclearQuímica54Uso da RMN no estudo da despolimerização de poliuretano rígidoUsing NMR to study the depolymerization of rigid polyurethaneinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisinfo:eu-repo/semantics/openAccessreponame:Repositório Institucional da Universidade Federal do Espírito Santo (riUfes)instname:Universidade Federal do Espírito Santo (UFES)instacron:UFESORIGINALDissertação-Juliana Proliciano-Versão final.pdfapplication/pdf5458594http://repositorio.ufes.br/bitstreams/6ac29c67-0163-4420-8040-a7c954811d94/download82bb3a27a6640b75e9c16d3ea07bc6f1MD5110/112722024-06-28 17:52:23.64oai:repositorio.ufes.br:10/11272http://repositorio.ufes.brRepositório InstitucionalPUBhttp://repositorio.ufes.br/oai/requestopendoar:21082024-07-11T14:28:38.646887Repositório Institucional da Universidade Federal do Espírito Santo (riUfes) - Universidade Federal do Espírito Santo (UFES)false |
dc.title.none.fl_str_mv |
Uso da RMN no estudo da despolimerização de poliuretano rígido |
dc.title.alternative.none.fl_str_mv |
Using NMR to study the depolymerization of rigid polyurethane |
title |
Uso da RMN no estudo da despolimerização de poliuretano rígido |
spellingShingle |
Uso da RMN no estudo da despolimerização de poliuretano rígido Maioli, Juliana Proliciano Glycolysis Glycerol Glicólise Glicerol Química Poliuretanas Ressonância magnética nuclear 54 |
title_short |
Uso da RMN no estudo da despolimerização de poliuretano rígido |
title_full |
Uso da RMN no estudo da despolimerização de poliuretano rígido |
title_fullStr |
Uso da RMN no estudo da despolimerização de poliuretano rígido |
title_full_unstemmed |
Uso da RMN no estudo da despolimerização de poliuretano rígido |
title_sort |
Uso da RMN no estudo da despolimerização de poliuretano rígido |
author |
Maioli, Juliana Proliciano |
author_facet |
Maioli, Juliana Proliciano |
author_role |
author |
dc.contributor.advisor-co1.fl_str_mv |
SILVA FILHO, Eloi Alves da |
dc.contributor.advisor1.fl_str_mv |
Cunha Neto, Álvaro |
dc.contributor.author.fl_str_mv |
Maioli, Juliana Proliciano |
dc.contributor.referee1.fl_str_mv |
Freitas, Marcos Benedito José Geraldo de |
dc.contributor.referee2.fl_str_mv |
Almeida, Luiz Carlos Pimentel |
contributor_str_mv |
SILVA FILHO, Eloi Alves da Cunha Neto, Álvaro Freitas, Marcos Benedito José Geraldo de Almeida, Luiz Carlos Pimentel |
dc.subject.eng.fl_str_mv |
Glycolysis Glycerol |
topic |
Glycolysis Glycerol Glicólise Glicerol Química Poliuretanas Ressonância magnética nuclear 54 |
dc.subject.por.fl_str_mv |
Glicólise Glicerol |
dc.subject.cnpq.fl_str_mv |
Química |
dc.subject.br-rjbn.none.fl_str_mv |
Poliuretanas Ressonância magnética nuclear |
dc.subject.udc.none.fl_str_mv |
54 |
description |
Polyurethanes (PUs) have been widely used in several trade sections. Thereby, large amounts of waste are produced and need to be correctly disposed off. Research on this theme has been helping industries to apply recycling processes that are cheap and efficient. In this work, the glycolysis of a rigid PU was performed using different catalysts. The catalysts used was: a tensoactive (CTAB), the NaOH, two ionics liquids (1-butyl-3-methylimidazole trichloromanganate and 1-butyl-3-methylimidazole trichlorozincate), and four Niobium salts (niobium pentoxide, niobium oxidehydrated, niobium pentachloride and niobium ammoniacal oxalate). 1H NMR technique was used to obtain the rate of PU depolymerization. Also was used the technique diffusion ordered spectroscopy 1H NMR (DOSY-NMR) that assisted in the identification composition of the mixture of products. In the glycolysis, glycerol (GCL) and diethylene glycol (DEG) were tested as glycolysis agents. The PU was synthesized to be free of additives in the depolymerization process, and its characterization was performed using infrared spectroscopy (FTIR) and 1H NMR spectroscopy analyses. The conversion rate provides information about which catalyst has the better catalytic activity. The use of NaOH as a catalyst presented conversion rate of 100 % in 30 min of reaction, as is already known in the literature, and the DOSY-NMR spectrum provided information about products that didn’t perceptible only by 1H NMR spectrum. Ionic liquids (LIs) as catalysts, presented conversion near of 80 % in 1h of reaction, which can be improved by modifying the reaction conditions. To determine the composition of the mixture of products in the depolymerization reaction, diffusion ordered spectroscopy 1H NMR (DOSY-NMR) was used. The Niobium salts had non-catalytic behavior, because they showed conversion rate lower than uncatalyzed reaction. DOSY-NMR indicated a complex mixture of reaction by-products, differently from the 1H NMR data, which indicated the formation of a simple diamine-terminated by-product. |
publishDate |
2019 |
dc.date.accessioned.fl_str_mv |
2019-06-27T02:05:06Z |
dc.date.available.fl_str_mv |
2019-06-26 2019-06-27T02:05:06Z |
dc.date.issued.fl_str_mv |
2019-03-26 |
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 |
MAIOLI, Juliana Proliciano. Uso da RMN no estudo da despolimerização de poliuretano rígido. 2019. 71 f. Dissertação (Mestrado em Química) – Universidade Federal do Espírito Santo, Centro de Ciências Exatas, Vitória, 2019. |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufes.br/handle/10/11272 |
identifier_str_mv |
MAIOLI, Juliana Proliciano. Uso da RMN no estudo da despolimerização de poliuretano rígido. 2019. 71 f. Dissertação (Mestrado em Química) – Universidade Federal do Espírito Santo, Centro de Ciências Exatas, Vitória, 2019. |
url |
http://repositorio.ufes.br/handle/10/11272 |
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por |
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por |
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openAccess |
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Text |
dc.publisher.none.fl_str_mv |
Universidade Federal do Espírito Santo Mestrado em Química |
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Programa de Pós-Graduação em Química |
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UFES |
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BR |
dc.publisher.department.fl_str_mv |
Centro de Ciências Exatas |
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Universidade Federal do Espírito Santo Mestrado em Química |
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