Nanotubos de carbono de paredes múltiplas dopados com nitrogênio e decorados com nanopartículas de paládio e suas aplicações em reações de catálise
Autor(a) principal: | |
---|---|
Data de Publicação: | 2016 |
Tipo de documento: | Tese |
Idioma: | por |
Título da fonte: | Manancial - Repositório Digital da UFSM |
Texto Completo: | http://repositorio.ufsm.br/handle/1/11952 |
Resumo: | The present work describes the synthesis of a new catalyst of palladium nanoparticles supported on multi-walled carbon nanotubes containing nitrogen (Pd@CNxNCPM) 1 and its use in carbon-carbon coupling reactions (Suzuki and Heck) as well as reactions catalytic hydrogenation (reduction of double C-C bonds and nitro compounds reduction). The synthetic strategy employed afforded the simple way to obtain the catalyst with reaction in a short time and efficiently. To this was employed as the palladium precursor, the salt potassium hexacloropalladate IV and hydrazine monohydrate as the reducing agent, without the need for stabilizing agents for the control of nucleation and size of nanoparticle. The catalyst system was characterized as its morphology: dispersion, size and shape of nanoparticles by scanning electron microscopy. Also the catalyst was performed Raman spectroscopy and determination of amount of palladium. After characterization the catalyst, it was tested for coupling reactions of carbon-carbon: Suzuki and Heck leading to the formation of their products with 70-> 95% for Suzuki coupling and 75-> 95% for Heck. For the synthesis in question were used 0.5 mol% of catalyst (based amount of palladium) for Suzuki and 10 mol% for Heck. It should be noted that the catalyst shown stable in the reaction conditions tested, and observed the possibility of reuse of this system for additional reaction cycles without loss of efficiency for the Suzuki coupling. Also, the catalyst was efficient and chemoselectiv for catalytic hydrogenations of unsaturated carbon-carbon bonds and nitro compounds leading to their products in good yields. Thus, the synthesized catalyst proved versatile and can be used in reactions of carbon-carbon coupling well as in catalytic reduction may also be recovered and reused, which provides an environmentally friendly at the same characteristic. |
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2017-11-01T13:26:07Z2017-11-01T13:26:07Z2016-02-05http://repositorio.ufsm.br/handle/1/11952The present work describes the synthesis of a new catalyst of palladium nanoparticles supported on multi-walled carbon nanotubes containing nitrogen (Pd@CNxNCPM) 1 and its use in carbon-carbon coupling reactions (Suzuki and Heck) as well as reactions catalytic hydrogenation (reduction of double C-C bonds and nitro compounds reduction). The synthetic strategy employed afforded the simple way to obtain the catalyst with reaction in a short time and efficiently. To this was employed as the palladium precursor, the salt potassium hexacloropalladate IV and hydrazine monohydrate as the reducing agent, without the need for stabilizing agents for the control of nucleation and size of nanoparticle. The catalyst system was characterized as its morphology: dispersion, size and shape of nanoparticles by scanning electron microscopy. Also the catalyst was performed Raman spectroscopy and determination of amount of palladium. After characterization the catalyst, it was tested for coupling reactions of carbon-carbon: Suzuki and Heck leading to the formation of their products with 70-> 95% for Suzuki coupling and 75-> 95% for Heck. For the synthesis in question were used 0.5 mol% of catalyst (based amount of palladium) for Suzuki and 10 mol% for Heck. It should be noted that the catalyst shown stable in the reaction conditions tested, and observed the possibility of reuse of this system for additional reaction cycles without loss of efficiency for the Suzuki coupling. Also, the catalyst was efficient and chemoselectiv for catalytic hydrogenations of unsaturated carbon-carbon bonds and nitro compounds leading to their products in good yields. Thus, the synthesized catalyst proved versatile and can be used in reactions of carbon-carbon coupling well as in catalytic reduction may also be recovered and reused, which provides an environmentally friendly at the same characteristic.O presente trabalho apresenta a síntese de um novo catalisador de nanopartículas de paládio suportadas em nanotubos de carbono de paredes múltiplas contendo nitrogênio (Pd@CNxNCPM) 1 e sua utilização em reações de acoplamento carbono-carbono (Suzuki e Heck) bem como em reações de Hidrogenações catalíticas (reduções de duplas ligações C-C e redução de nitrocompostos). A estratégia sintética utilizada permitiu a obtenção do catalisador de maneira simples, em curto tempo reacional e de maneira eficiente e sem a presença de agentes estabilizantes externos. Para isso foi empregado como precursor de paládio o sal hexacloropaladato IV de potássio e como agente redutor, hidrazina monohidratada sem a necessidade de agentes estabilizantes para o controle da nucleação e tamanho de nanopartículas. O sistema catalítico foi caracterizado quanto sua morfologia: dispersão, tamanho e forma de nanopartículas através de microscopia eletrônica de varredura. Também foi realizada espectroscopia Raman do catalisador bem como determinação do teor de paládio. Após devidamente analisado o catalisador, o mesmo foi testado para reações de acoplamento carbono-carbono de Suzuki e Heck levando a formação dos respectivos produtos com rendimentos de 70-> 95% para os acoplamentos de Suzuki e 75-> 95% para Heck. Para as sínteses em questão foram usados 0,5 mol% de catalisador (baseados na massa de paládio) para Suzuki e 10 mol% para Heck. Cabe salientar que o catalisador se mostra estável nas condições reacionais testadas, sendo observada a possibilidade de reuso deste sistema por ciclos reacionais adicionais, sem perdas de eficiência para o acoplamento de Suzuki. Ainda, o catalisador se mostrou eficiente para hidrogenações catalíticas quimiosseletivas de ligações de carbono-carbono insaturadas e nitrocompostos levando aos respectivos produtos em bons rendimentos. Dessa forma o catalisador sintetizado se mostrou versátil, sendo possível ser utilizado em reações de acoplamento carbono-carbono bem como em reduções catalíticas, também pode ser recuperado e reutilizado, o que confere ao mesmo uma característica ambientalmente correta.Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPESporUniversidade Federal de Santa MariaCentro de Ciências Naturais e ExatasPrograma de Pós-Graduação em QuímicaUFSMBrasilQuímicaAttribution-NonCommercial-NoDerivatives 4.0 Internationalhttp://creativecommons.org/licenses/by-nc-nd/4.0/info:eu-repo/semantics/openAccessNanotubos de carbono dopados com nitrogênioNanopartículas de paládioCatáliseMulti walled carbon nanotubes doped with nitrogenPaladium nanoparticlesCatalysisCNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICANanotubos de carbono de paredes múltiplas dopados com nitrogênio e decorados com nanopartículas de paládio e suas aplicações em reações de catáliseMulti walled carbon nanotubes doped with nitrogen and decorated with paladium nanoparticles and their apllications in catalysis reactionsinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisRodrigues, Oscar Endrigo Dorneleshttp://lattes.cnpq.br/6536519955416085Emmerich, Daniel Jacinthohttp://lattes.cnpq.br/8251907460764870Alves, Elenilson Freitashttp://lattes.cnpq.br/5541226399395863Giacomelli, Cristianohttp://lattes.cnpq.br/1429116139250396Ilha, Viniciushttp://lattes.cnpq.br/3882671719676564http://lattes.cnpq.br/6558536357135507Vargas, Josimar10060000000060009fef019-ac43-4d8b-83d3-3565e4686d7b2fe4fd27-125e-435a-a95b-56a041287414a62807af-3e21-47f7-ac84-903d01d9d3f8187c6d50-eb76-4941-9300-bfb6050501d47dc7675e-3956-47d1-a76a-e3797351c4a7a297d48a-1e32-4b0b-884b-f34573af5115reponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALTES_PPGQUÍMICA_2016_VARGAS_JOSIMAR.pdfTES_PPGQUÍMICA_2016_VARGAS_JOSIMAR.pdfTese de Doutoradoapplication/pdf8204719http://repositorio.ufsm.br/bitstream/1/11952/1/TES_PPGQU%c3%8dMICA_2016_VARGAS_JOSIMAR.pdf7eba519c0ed2ae98cde3b803d758c625MD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Nanotubos de carbono de paredes múltiplas dopados com nitrogênio e decorados com nanopartículas de paládio e suas aplicações em reações de catálise |
dc.title.alternative.eng.fl_str_mv |
Multi walled carbon nanotubes doped with nitrogen and decorated with paladium nanoparticles and their apllications in catalysis reactions |
title |
Nanotubos de carbono de paredes múltiplas dopados com nitrogênio e decorados com nanopartículas de paládio e suas aplicações em reações de catálise |
spellingShingle |
Nanotubos de carbono de paredes múltiplas dopados com nitrogênio e decorados com nanopartículas de paládio e suas aplicações em reações de catálise Vargas, Josimar Nanotubos de carbono dopados com nitrogênio Nanopartículas de paládio Catálise Multi walled carbon nanotubes doped with nitrogen Paladium nanoparticles Catalysis CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
title_short |
Nanotubos de carbono de paredes múltiplas dopados com nitrogênio e decorados com nanopartículas de paládio e suas aplicações em reações de catálise |
title_full |
Nanotubos de carbono de paredes múltiplas dopados com nitrogênio e decorados com nanopartículas de paládio e suas aplicações em reações de catálise |
title_fullStr |
Nanotubos de carbono de paredes múltiplas dopados com nitrogênio e decorados com nanopartículas de paládio e suas aplicações em reações de catálise |
title_full_unstemmed |
Nanotubos de carbono de paredes múltiplas dopados com nitrogênio e decorados com nanopartículas de paládio e suas aplicações em reações de catálise |
title_sort |
Nanotubos de carbono de paredes múltiplas dopados com nitrogênio e decorados com nanopartículas de paládio e suas aplicações em reações de catálise |
author |
Vargas, Josimar |
author_facet |
Vargas, Josimar |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Rodrigues, Oscar Endrigo Dorneles |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/6536519955416085 |
dc.contributor.referee1.fl_str_mv |
Emmerich, Daniel Jacintho |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/8251907460764870 |
dc.contributor.referee2.fl_str_mv |
Alves, Elenilson Freitas |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/5541226399395863 |
dc.contributor.referee3.fl_str_mv |
Giacomelli, Cristiano |
dc.contributor.referee3Lattes.fl_str_mv |
http://lattes.cnpq.br/1429116139250396 |
dc.contributor.referee4.fl_str_mv |
Ilha, Vinicius |
dc.contributor.referee4Lattes.fl_str_mv |
http://lattes.cnpq.br/3882671719676564 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/6558536357135507 |
dc.contributor.author.fl_str_mv |
Vargas, Josimar |
contributor_str_mv |
Rodrigues, Oscar Endrigo Dorneles Emmerich, Daniel Jacintho Alves, Elenilson Freitas Giacomelli, Cristiano Ilha, Vinicius |
dc.subject.por.fl_str_mv |
Nanotubos de carbono dopados com nitrogênio Nanopartículas de paládio Catálise |
topic |
Nanotubos de carbono dopados com nitrogênio Nanopartículas de paládio Catálise Multi walled carbon nanotubes doped with nitrogen Paladium nanoparticles Catalysis CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
dc.subject.eng.fl_str_mv |
Multi walled carbon nanotubes doped with nitrogen Paladium nanoparticles Catalysis |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA |
description |
The present work describes the synthesis of a new catalyst of palladium nanoparticles supported on multi-walled carbon nanotubes containing nitrogen (Pd@CNxNCPM) 1 and its use in carbon-carbon coupling reactions (Suzuki and Heck) as well as reactions catalytic hydrogenation (reduction of double C-C bonds and nitro compounds reduction). The synthetic strategy employed afforded the simple way to obtain the catalyst with reaction in a short time and efficiently. To this was employed as the palladium precursor, the salt potassium hexacloropalladate IV and hydrazine monohydrate as the reducing agent, without the need for stabilizing agents for the control of nucleation and size of nanoparticle. The catalyst system was characterized as its morphology: dispersion, size and shape of nanoparticles by scanning electron microscopy. Also the catalyst was performed Raman spectroscopy and determination of amount of palladium. After characterization the catalyst, it was tested for coupling reactions of carbon-carbon: Suzuki and Heck leading to the formation of their products with 70-> 95% for Suzuki coupling and 75-> 95% for Heck. For the synthesis in question were used 0.5 mol% of catalyst (based amount of palladium) for Suzuki and 10 mol% for Heck. It should be noted that the catalyst shown stable in the reaction conditions tested, and observed the possibility of reuse of this system for additional reaction cycles without loss of efficiency for the Suzuki coupling. Also, the catalyst was efficient and chemoselectiv for catalytic hydrogenations of unsaturated carbon-carbon bonds and nitro compounds leading to their products in good yields. Thus, the synthesized catalyst proved versatile and can be used in reactions of carbon-carbon coupling well as in catalytic reduction may also be recovered and reused, which provides an environmentally friendly at the same characteristic. |
publishDate |
2016 |
dc.date.issued.fl_str_mv |
2016-02-05 |
dc.date.accessioned.fl_str_mv |
2017-11-01T13:26:07Z |
dc.date.available.fl_str_mv |
2017-11-01T13:26:07Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/doctoralThesis |
format |
doctoralThesis |
status_str |
publishedVersion |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/11952 |
url |
http://repositorio.ufsm.br/handle/1/11952 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.relation.cnpq.fl_str_mv |
100600000000 |
dc.relation.confidence.fl_str_mv |
600 |
dc.relation.authority.fl_str_mv |
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dc.rights.driver.fl_str_mv |
Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/ info:eu-repo/semantics/openAccess |
rights_invalid_str_mv |
Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/ |
eu_rights_str_mv |
openAccess |
dc.publisher.none.fl_str_mv |
Universidade Federal de Santa Maria Centro de Ciências Naturais e Exatas |
dc.publisher.program.fl_str_mv |
Programa de Pós-Graduação em Química |
dc.publisher.initials.fl_str_mv |
UFSM |
dc.publisher.country.fl_str_mv |
Brasil |
dc.publisher.department.fl_str_mv |
Química |
publisher.none.fl_str_mv |
Universidade Federal de Santa Maria Centro de Ciências Naturais e Exatas |
dc.source.none.fl_str_mv |
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Universidade Federal de Santa Maria (UFSM) |
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UFSM |
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UFSM |
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Manancial - Repositório Digital da UFSM |
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