S?ntese de peneiras moleculares MCM-41 ativas em cat?lise b?sica para a produ??o de chalconas
Ano de defesa: | 2006 |
---|---|
Autor(a) principal: | |
Orientador(a): | |
Banca de defesa: | |
Tipo de documento: | Dissertação |
Tipo de acesso: | Acesso aberto |
Idioma: | por |
Instituição de defesa: |
Universidade Federal Rural do Rio de Janeiro
|
Programa de Pós-Graduação: |
Programa de P?s-Gradua??o em Engenharia Qu?mica
|
Departamento: |
Instituto de Tecnologia
|
País: |
Brasil
|
Palavras-chave em Português: | |
Palavras-chave em Inglês: | |
Área do conhecimento CNPq: | |
Link de acesso: | https://tede.ufrrj.br/jspui/handle/tede/345 |
Resumo: | Samples of MCM-41 mesoporous molecular sieves were synthesized from a gel presenting the following molar composition: 1,0 SiO2: 0,12 CTABr: 0,28 TMAOH: 100 H2O. The gel was hydrothermally treated or at 100?C for 24 hours or at 150?C for 5 days, forming Si-MCM-41 samples. After, calcining at 540?C, for removing surfactant, freeing the porosity, these samples were functionalized by reaction with two amines sources: 3-trimethoxysilylpropylamine and 3-trimethoxysilylpropylenediamine. The grafting process was shown to be very efficient, incorporing amounts of propylamine and etilenediaminepropyl groups near theoretical values. These samples were characterized by X ray diffraction (XRD), potentiometer titration, thermogravimetric analysis (TGA) and scanning electronic microscopy (SEM). From these analyses, it could be seen the samples presented well ordered MCM-41 structures with different pore size. The samples obtained from the 150?C for 5 days synthesis was formed by 2 ?m particles while the one obtained from 100?C for 24 hours synthesis was formed by particles lower than 1 ?m. The samples were catalytically evaluated by using the Claisen-Schmidt reaction, carried out at different temperatures (105, 140 and 165?C), to form chalcone and substituted chalconas. For the samples presenting propylamine groups grafted on their surface, it was observed that the activity increased with temperature increased. However, the etilenediaminepropyl grafted sample presented a maximum in activity at a temperature of 140?C. This reduction could be explained considering that these samples presented two basic sites very near each other, capable of promoting bimolecular degradation reaction, forming carbonaceous deposits in the sample surface, deactivating them. A dark color in the reaction medium evidenced secondary compounds formation. It was observed, also, that the samples presenting higher pore size were more catalytic actives and that this activity difference was more evident at higher temperatures. |
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Fernandes, Lindoval Domiciano837.359.257-15http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4791022T5087.635.177-10http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4706687Y5Magalh?es, Juliano Borges Teixeira2016-04-26T19:51:53Z2006-10-092006-02-06MAGALH?ES, Juliano Borges Teixeira. S?ntese de peneiras moleculares MCM-41 ativas em cat?lise b?sica para a produ??o de chalconas. 2006. 51 f. Disserta??o (Mestrado em Engenharia Qu?mica) - Instituto de Tecnologia, Universidade Federal Rural do Rio de Janeiro, Serop?dica - RJ, 2006.https://tede.ufrrj.br/jspui/handle/tede/345Samples of MCM-41 mesoporous molecular sieves were synthesized from a gel presenting the following molar composition: 1,0 SiO2: 0,12 CTABr: 0,28 TMAOH: 100 H2O. The gel was hydrothermally treated or at 100?C for 24 hours or at 150?C for 5 days, forming Si-MCM-41 samples. After, calcining at 540?C, for removing surfactant, freeing the porosity, these samples were functionalized by reaction with two amines sources: 3-trimethoxysilylpropylamine and 3-trimethoxysilylpropylenediamine. The grafting process was shown to be very efficient, incorporing amounts of propylamine and etilenediaminepropyl groups near theoretical values. These samples were characterized by X ray diffraction (XRD), potentiometer titration, thermogravimetric analysis (TGA) and scanning electronic microscopy (SEM). From these analyses, it could be seen the samples presented well ordered MCM-41 structures with different pore size. The samples obtained from the 150?C for 5 days synthesis was formed by 2 ?m particles while the one obtained from 100?C for 24 hours synthesis was formed by particles lower than 1 ?m. The samples were catalytically evaluated by using the Claisen-Schmidt reaction, carried out at different temperatures (105, 140 and 165?C), to form chalcone and substituted chalconas. For the samples presenting propylamine groups grafted on their surface, it was observed that the activity increased with temperature increased. However, the etilenediaminepropyl grafted sample presented a maximum in activity at a temperature of 140?C. This reduction could be explained considering that these samples presented two basic sites very near each other, capable of promoting bimolecular degradation reaction, forming carbonaceous deposits in the sample surface, deactivating them. A dark color in the reaction medium evidenced secondary compounds formation. It was observed, also, that the samples presenting higher pore size were more catalytic actives and that this activity difference was more evident at higher temperatures.Neste trabalho, amostras de peneiras moleculares mesoporosas tipo MCM-41 foram sintetizadas a partir de um gel de s?ntese apresentando a seguinte composi??o molar: 1,0 SiO2: 0,12 CTABr: 0,28 TMAOH: 100 H2O. Este gel foi tratado hidrotermicamente ou 100?C por 24 horas ou 150?C por 5 dias para formar as amostras de Si-MCM-41. Ap?s a calcina??o a 540?C, para a remo??o do tensoativo e libera??o dos poros, estas amostras foram funcionalizadas atrav?s de rea??o com duas fontes de amina: 3-aminopropil(trimetoxi)silano e 3-etilenodiaminopropil(trimetoxi)silano. O processo de ancoramento se mostrou eficiente com a incorpora??o de grupamentos aminopropila e etilenodiaminopropila em quantidades pr?ximas da te?rica. Essas amostras foram caracterizadas por difra??o de raios X (DRX), titula??o potenciom?trica, an?lise termogravim?trica (ATG) e microscopia eletr?nica de varredura (MEV). Atrav?s dessas, pode-se observar que os catalisadores apresentavam estruturas bem ordenadas da peneira molecular MCM-41 possuindo diferentes tamanhos de poros. A amostra sintetizada a 150?C por 5 dias era formada por part?culas de 2 ?m, enquanto que aquelas sintetizadas a 100?C por 24 horas era formada por part?culas menores que 1 ?m. As amostras foram avaliadas cataliticamente utilizando-se a rea??o de Claisen-Schmidt, em diferentes temperaturas (105, 140 e 165?C), para a forma??o de chalconas simples e substitu?das. Foi observado que todas as amostras eram ativas para a produ??o de chalconas. Para as amostras contendo grupamentos aminopropila, ancorados em sua superf?cie, foi observado um aumento de atividade com o aumento da temperatura. No entanto, as amostras com grupamentos etilenodiaminopropila apresentaram um m?ximo de atividade a 140?C. Esta redu??o de atividade para a temperatura mais alta pode ser explicada considerando que estas amostras apresentavam dois s?tios b?sicos pr?ximos podendo promover rea??es bimoleculares de degrada??o, formando dep?sitos de coque na superf?cie do catalisador, desativando-o. Uma colora??o escura no meio reacional indicou a forma??o de compostos secund?rios. Observou-se, tamb?m, que as amostras apresentando di?metros de poros maiores eram mais ativas e que esta diferen?a de atividade era mais evidente para temperaturas mais altas.Made available in DSpace on 2016-04-26T19:51:53Z (GMT). No. of bitstreams: 1 2006-Juliano Borges Teixeira Magalhaes.pdf: 2030252 bytes, checksum: b190baa8022bcbf3c72cc6b6e7021ca0 (MD5) Previous issue date: 2006-02-06CAPES - Coordena??o de Aperfei?oamento de Pessoal de N?vel Superiorapplication/pdfhttps://tede.ufrrj.br/retrieve/3841/2006%20-%20Juliano%20Borges%20Teixeira%20Magalh%c3%a3es.pdf.jpghttps://tede.ufrrj.br/retrieve/18160/2006%20-%20Juliano%20Borges%20Teixeira%20Magalh%c3%a3es.pdf.jpghttps://tede.ufrrj.br/retrieve/24456/2006%20-%20Juliano%20Borges%20Teixeira%20Magalh%c3%a3es.pdf.jpghttps://tede.ufrrj.br/retrieve/30863/2006%20-%20Juliano%20Borges%20Teixeira%20Magalh%c3%a3es.pdf.jpghttps://tede.ufrrj.br/retrieve/37218/2006%20-%20Juliano%20Borges%20Teixeira%20Magalh%c3%a3es.pdf.jpghttps://tede.ufrrj.br/retrieve/43623/2006%20-%20Juliano%20Borges%20Teixeira%20Magalh%c3%a3es.pdf.jpghttps://tede.ufrrj.br/retrieve/49985/2006%20-%20Juliano%20Borges%20Teixeira%20Magalh%c3%a3es.pdf.jpghttps://tede.ufrrj.br/retrieve/56407/2006%20-%20Juliano%20Borges%20Teixeira%20Magalh%c3%a3es.pdf.jpgporUniversidade Federal Rural do Rio de JaneiroPrograma de P?s-Gradua??o em Engenharia Qu?micaUFRRJBrasilInstituto de Tecnologiacatalisadores b?sicosMCM-41Chalconasbasic catalystsChalconesEngenharia Qu?micaS?ntese de peneiras moleculares MCM-41 ativas em cat?lise b?sica para a produ??o de chalconasSynthesis of MCM-41 mesoporous molecular sieves actives in the basic catalysis to form chalconesinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisinfo:eu-repo/semantics/openAccessreponame:Biblioteca Digital de Teses e Dissertações da UFRRJinstname:Universidade Federal Rural do Rio de Janeiro (UFRRJ)instacron:UFRRJTHUMBNAIL2006 - Juliano Borges Teixeira Magalh?es.pdf.jpg2006 - Juliano Borges Teixeira Magalh?es.pdf.jpgimage/jpeg3398http://localhost:8080/tede/bitstream/tede/345/17/2006+-+Juliano+Borges+Teixeira+Magalh%C3%A3es.pdf.jpg224bd5c75204b22e7868e23e9c59ac3eMD517TEXT2006 - Juliano Borges Teixeira Magalh?es.pdf.txt2006 - Juliano Borges Teixeira Magalh?es.pdf.txttext/plain124928http://localhost:8080/tede/bitstream/tede/345/16/2006+-+Juliano+Borges+Teixeira+Magalh%C3%A3es.pdf.txtfdbac8927c116c8297df248f43635c93MD516ORIGINAL2006 - Juliano Borges Teixeira Magalh?es.pdf2006 - Juliano Borges Teixeira Magalh?es.pdfapplication/pdf2027747http://localhost:8080/tede/bitstream/tede/345/1/2006+-+Juliano+Borges+Teixeira+Magalh%C3%A3es.pdfd4139fb99e62130593b192cb7485fc61MD51tede/3452022-06-08 13:04:28.014oai:localhost:tede/345Biblioteca Digital de Teses e Dissertaçõeshttps://tede.ufrrj.br/PUBhttps://tede.ufrrj.br/oai/requestbibliot@ufrrj.br||bibliot@ufrrj.bropendoar:2022-06-08T16:04:28Biblioteca Digital de Teses e Dissertações da UFRRJ - Universidade Federal Rural do Rio de Janeiro (UFRRJ)false |
dc.title.por.fl_str_mv |
S?ntese de peneiras moleculares MCM-41 ativas em cat?lise b?sica para a produ??o de chalconas |
dc.title.alternative.eng.fl_str_mv |
Synthesis of MCM-41 mesoporous molecular sieves actives in the basic catalysis to form chalcones |
title |
S?ntese de peneiras moleculares MCM-41 ativas em cat?lise b?sica para a produ??o de chalconas |
spellingShingle |
S?ntese de peneiras moleculares MCM-41 ativas em cat?lise b?sica para a produ??o de chalconas Magalh?es, Juliano Borges Teixeira catalisadores b?sicos MCM-41 Chalconas basic catalysts Chalcones Engenharia Qu?mica |
title_short |
S?ntese de peneiras moleculares MCM-41 ativas em cat?lise b?sica para a produ??o de chalconas |
title_full |
S?ntese de peneiras moleculares MCM-41 ativas em cat?lise b?sica para a produ??o de chalconas |
title_fullStr |
S?ntese de peneiras moleculares MCM-41 ativas em cat?lise b?sica para a produ??o de chalconas |
title_full_unstemmed |
S?ntese de peneiras moleculares MCM-41 ativas em cat?lise b?sica para a produ??o de chalconas |
title_sort |
S?ntese de peneiras moleculares MCM-41 ativas em cat?lise b?sica para a produ??o de chalconas |
author |
Magalh?es, Juliano Borges Teixeira |
author_facet |
Magalh?es, Juliano Borges Teixeira |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Fernandes, Lindoval Domiciano |
dc.contributor.advisor1ID.fl_str_mv |
837.359.257-15 |
dc.contributor.advisor1Lattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4791022T5 |
dc.contributor.authorID.fl_str_mv |
087.635.177-10 |
dc.contributor.authorLattes.fl_str_mv |
http://buscatextual.cnpq.br/buscatextual/visualizacv.do?id=K4706687Y5 |
dc.contributor.author.fl_str_mv |
Magalh?es, Juliano Borges Teixeira |
contributor_str_mv |
Fernandes, Lindoval Domiciano |
dc.subject.por.fl_str_mv |
catalisadores b?sicos MCM-41 Chalconas |
topic |
catalisadores b?sicos MCM-41 Chalconas basic catalysts Chalcones Engenharia Qu?mica |
dc.subject.eng.fl_str_mv |
basic catalysts Chalcones |
dc.subject.cnpq.fl_str_mv |
Engenharia Qu?mica |
description |
Samples of MCM-41 mesoporous molecular sieves were synthesized from a gel presenting the following molar composition: 1,0 SiO2: 0,12 CTABr: 0,28 TMAOH: 100 H2O. The gel was hydrothermally treated or at 100?C for 24 hours or at 150?C for 5 days, forming Si-MCM-41 samples. After, calcining at 540?C, for removing surfactant, freeing the porosity, these samples were functionalized by reaction with two amines sources: 3-trimethoxysilylpropylamine and 3-trimethoxysilylpropylenediamine. The grafting process was shown to be very efficient, incorporing amounts of propylamine and etilenediaminepropyl groups near theoretical values. These samples were characterized by X ray diffraction (XRD), potentiometer titration, thermogravimetric analysis (TGA) and scanning electronic microscopy (SEM). From these analyses, it could be seen the samples presented well ordered MCM-41 structures with different pore size. The samples obtained from the 150?C for 5 days synthesis was formed by 2 ?m particles while the one obtained from 100?C for 24 hours synthesis was formed by particles lower than 1 ?m. The samples were catalytically evaluated by using the Claisen-Schmidt reaction, carried out at different temperatures (105, 140 and 165?C), to form chalcone and substituted chalconas. For the samples presenting propylamine groups grafted on their surface, it was observed that the activity increased with temperature increased. However, the etilenediaminepropyl grafted sample presented a maximum in activity at a temperature of 140?C. This reduction could be explained considering that these samples presented two basic sites very near each other, capable of promoting bimolecular degradation reaction, forming carbonaceous deposits in the sample surface, deactivating them. A dark color in the reaction medium evidenced secondary compounds formation. It was observed, also, that the samples presenting higher pore size were more catalytic actives and that this activity difference was more evident at higher temperatures. |
publishDate |
2006 |
dc.date.available.fl_str_mv |
2006-10-09 |
dc.date.issued.fl_str_mv |
2006-02-06 |
dc.date.accessioned.fl_str_mv |
2016-04-26T19:51:53Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
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info:eu-repo/semantics/masterThesis |
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masterThesis |
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publishedVersion |
dc.identifier.citation.fl_str_mv |
MAGALH?ES, Juliano Borges Teixeira. S?ntese de peneiras moleculares MCM-41 ativas em cat?lise b?sica para a produ??o de chalconas. 2006. 51 f. Disserta??o (Mestrado em Engenharia Qu?mica) - Instituto de Tecnologia, Universidade Federal Rural do Rio de Janeiro, Serop?dica - RJ, 2006. |
dc.identifier.uri.fl_str_mv |
https://tede.ufrrj.br/jspui/handle/tede/345 |
identifier_str_mv |
MAGALH?ES, Juliano Borges Teixeira. S?ntese de peneiras moleculares MCM-41 ativas em cat?lise b?sica para a produ??o de chalconas. 2006. 51 f. Disserta??o (Mestrado em Engenharia Qu?mica) - Instituto de Tecnologia, Universidade Federal Rural do Rio de Janeiro, Serop?dica - RJ, 2006. |
url |
https://tede.ufrrj.br/jspui/handle/tede/345 |
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por |
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UFRRJ |
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Brasil |
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Instituto de Tecnologia |
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Universidade Federal Rural do Rio de Janeiro |
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