Optimization of the time and temperature of the microwave-assisted amination of phenylene-PMO
Autor(a) principal: | |
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Data de Publicação: | 2015 |
Outros Autores: | , |
Tipo de documento: | Artigo |
Idioma: | eng |
Título da fonte: | Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos) |
Texto Completo: | http://hdl.handle.net/10773/20084 |
Resumo: | In this paper we report a study on the optimization of the amination of periodic mesoporous phenylene-silica (PMO) using microwave heating. The optimization was carried out for two key steps in the reaction, namely, (1) nitration of the bissilylated phenylene bridge, and (2) reduction of the nitro group to a primary amine. The temperatures of both reaction steps were varied between 37, 60, 75 and 90 degrees C. The reaction times studied were between 15 to 360 minutes. Microwave heating lead to significant reduction in the reaction times needed to achieve the maximum degree of nitration and amination compared to conventional means. After 15 minutes of reaction at 60 degrees C, a nitrogen density similar to that obtained for the same material synthesized conventionally was observed, and after 240 minutes of reaction time at 60 degrees C the nitrogen density was exceeded. A complete reduction of the nitro to the amine groups was observed after 15 minutes of reaction at 60 degrees C, which demonstrates the great potential of microwave irradiation in enhancing the kinetics of the post-synthesis functionalization of PMO materials, while preserving the molecular and mesoporous orders. |
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Optimization of the time and temperature of the microwave-assisted amination of phenylene-PMOPERIODIC MESOPOROUS ORGANOSILICASORGANIC-SYNTHESISSILICAHYBRIDSWALLSIn this paper we report a study on the optimization of the amination of periodic mesoporous phenylene-silica (PMO) using microwave heating. The optimization was carried out for two key steps in the reaction, namely, (1) nitration of the bissilylated phenylene bridge, and (2) reduction of the nitro group to a primary amine. The temperatures of both reaction steps were varied between 37, 60, 75 and 90 degrees C. The reaction times studied were between 15 to 360 minutes. Microwave heating lead to significant reduction in the reaction times needed to achieve the maximum degree of nitration and amination compared to conventional means. After 15 minutes of reaction at 60 degrees C, a nitrogen density similar to that obtained for the same material synthesized conventionally was observed, and after 240 minutes of reaction time at 60 degrees C the nitrogen density was exceeded. A complete reduction of the nitro to the amine groups was observed after 15 minutes of reaction at 60 degrees C, which demonstrates the great potential of microwave irradiation in enhancing the kinetics of the post-synthesis functionalization of PMO materials, while preserving the molecular and mesoporous orders.ROYAL SOC CHEMISTRY2017-12-07T19:34:56Z2015-01-01T00:00:00Z2015info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/articleapplication/pdfhttp://hdl.handle.net/10773/20084eng2046-206910.1039/c4ra12364fLourenco, Mirtha A. O.Gomes, Jose R. B.Ferreira, Paulainfo:eu-repo/semantics/openAccessreponame:Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos)instname:Agência para a Sociedade do Conhecimento (UMIC) - FCT - Sociedade da Informaçãoinstacron:RCAAP2024-02-22T11:39:15Zoai:ria.ua.pt:10773/20084Portal AgregadorONGhttps://www.rcaap.pt/oai/openaireopendoar:71602024-03-20T02:54:47.341383Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos) - Agência para a Sociedade do Conhecimento (UMIC) - FCT - Sociedade da Informaçãofalse |
dc.title.none.fl_str_mv |
Optimization of the time and temperature of the microwave-assisted amination of phenylene-PMO |
title |
Optimization of the time and temperature of the microwave-assisted amination of phenylene-PMO |
spellingShingle |
Optimization of the time and temperature of the microwave-assisted amination of phenylene-PMO Lourenco, Mirtha A. O. PERIODIC MESOPOROUS ORGANOSILICAS ORGANIC-SYNTHESIS SILICA HYBRIDS WALLS |
title_short |
Optimization of the time and temperature of the microwave-assisted amination of phenylene-PMO |
title_full |
Optimization of the time and temperature of the microwave-assisted amination of phenylene-PMO |
title_fullStr |
Optimization of the time and temperature of the microwave-assisted amination of phenylene-PMO |
title_full_unstemmed |
Optimization of the time and temperature of the microwave-assisted amination of phenylene-PMO |
title_sort |
Optimization of the time and temperature of the microwave-assisted amination of phenylene-PMO |
author |
Lourenco, Mirtha A. O. |
author_facet |
Lourenco, Mirtha A. O. Gomes, Jose R. B. Ferreira, Paula |
author_role |
author |
author2 |
Gomes, Jose R. B. Ferreira, Paula |
author2_role |
author author |
dc.contributor.author.fl_str_mv |
Lourenco, Mirtha A. O. Gomes, Jose R. B. Ferreira, Paula |
dc.subject.por.fl_str_mv |
PERIODIC MESOPOROUS ORGANOSILICAS ORGANIC-SYNTHESIS SILICA HYBRIDS WALLS |
topic |
PERIODIC MESOPOROUS ORGANOSILICAS ORGANIC-SYNTHESIS SILICA HYBRIDS WALLS |
description |
In this paper we report a study on the optimization of the amination of periodic mesoporous phenylene-silica (PMO) using microwave heating. The optimization was carried out for two key steps in the reaction, namely, (1) nitration of the bissilylated phenylene bridge, and (2) reduction of the nitro group to a primary amine. The temperatures of both reaction steps were varied between 37, 60, 75 and 90 degrees C. The reaction times studied were between 15 to 360 minutes. Microwave heating lead to significant reduction in the reaction times needed to achieve the maximum degree of nitration and amination compared to conventional means. After 15 minutes of reaction at 60 degrees C, a nitrogen density similar to that obtained for the same material synthesized conventionally was observed, and after 240 minutes of reaction time at 60 degrees C the nitrogen density was exceeded. A complete reduction of the nitro to the amine groups was observed after 15 minutes of reaction at 60 degrees C, which demonstrates the great potential of microwave irradiation in enhancing the kinetics of the post-synthesis functionalization of PMO materials, while preserving the molecular and mesoporous orders. |
publishDate |
2015 |
dc.date.none.fl_str_mv |
2015-01-01T00:00:00Z 2015 2017-12-07T19:34:56Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/article |
format |
article |
status_str |
publishedVersion |
dc.identifier.uri.fl_str_mv |
http://hdl.handle.net/10773/20084 |
url |
http://hdl.handle.net/10773/20084 |
dc.language.iso.fl_str_mv |
eng |
language |
eng |
dc.relation.none.fl_str_mv |
2046-2069 10.1039/c4ra12364f |
dc.rights.driver.fl_str_mv |
info:eu-repo/semantics/openAccess |
eu_rights_str_mv |
openAccess |
dc.format.none.fl_str_mv |
application/pdf |
dc.publisher.none.fl_str_mv |
ROYAL SOC CHEMISTRY |
publisher.none.fl_str_mv |
ROYAL SOC CHEMISTRY |
dc.source.none.fl_str_mv |
reponame:Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos) instname:Agência para a Sociedade do Conhecimento (UMIC) - FCT - Sociedade da Informação instacron:RCAAP |
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Agência para a Sociedade do Conhecimento (UMIC) - FCT - Sociedade da Informação |
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RCAAP |
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RCAAP |
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Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos) |
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Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos) |
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Repositório Científico de Acesso Aberto de Portugal (Repositórios Cientìficos) - Agência para a Sociedade do Conhecimento (UMIC) - FCT - Sociedade da Informação |
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1799137600659783680 |