Síntese do ácido fosfotúngstico e otimização da reação de esterificação do ácido oléico com etanol

Detalhes bibliográficos
Autor(a) principal: Soares, Mário Rodrigo dos Santos
Data de Publicação: 2013
Tipo de documento: Dissertação
Idioma: por
Título da fonte: Repositório Institucional da UFMT
Texto Completo: http://ri.ufmt.br/handle/1/1618
Resumo: In this work the synthesis of phosphotungstic acid and optimization of esterification reaction of oleic acid with ethanol were investigated. The synthesis of the catalyst H3PW12O40 by conventional and microwave assisted methods were performed. The catalysts synthesized and a commercial were characterized by thermal analyses, XRD, FTIR, SEM and of surface area measurements, being observed characteristic properties of the H3PW12O40. The esterification reactions were performed with a commercial H3PW12O40 catalyst and also with H2SO4. The optimization of conversion in the reaction was carried out by means of two-level factorial designs. Initially, an exploratory 24 factorial design was carried out in order to identify main factors (molar ratio oleic acid:ethanol, amount of catalyst, temperature and time) affecting % conversion of ester. After that, the 24 factorial design was expanded and adjusted resulting in 25 factorials designs. In one of them, the reactions were carried out including the type of catalyst as a factor to enable a comparative evaluation of both H3PW12O40 and H2SO4. The temperature was the main factor affecting the conversion which increased 27.2 % in media when the temperature changes from 45 to 75 oC. Therefore, the temperature was fixed at 75 oC and the other 25 factorial design, including the heating source conventional or by ultrasound was performed. In this factorial design was observed that the ultrasound-assisted reactions had shown an averaged increasing of 5,5 % in the conversion. The maximum conversion was around 80 % with both of catalysts. Finally, based in the results of factorial designs, experiments with higher temperature, amount of catalyst and time were carried out and a conversion of around 90 % was achieved. The molar ratio of oleic acid:ethanol did not significantly affect the conversion in all conditions investigated. Under the optimized condition the conversion obtained in the heterogeneous reaction with H3PW12O40 was the same of the homogeneous reaction catalyzed by H2SO4. Also, it was carried out a preliminary study of recovery of the catalyst where the characterization by XRD, FTIR, thermal analyses and SEM showed that the recovered catalyst presents the same structural, spectroscopic and thermal properties than a typical of H3PW12O40. The catalyst recovered and treated at 300 °C was employed in a conventional esterification reaction and the conversion equivalent to that one with catalyst used for the first time was found.
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spelling Síntese do ácido fosfotúngstico e otimização da reação de esterificação do ácido oléico com etanol.CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA.In this work the synthesis of phosphotungstic acid and optimization of esterification reaction of oleic acid with ethanol were investigated. The synthesis of the catalyst H3PW12O40 by conventional and microwave assisted methods were performed. The catalysts synthesized and a commercial were characterized by thermal analyses, XRD, FTIR, SEM and of surface area measurements, being observed characteristic properties of the H3PW12O40. The esterification reactions were performed with a commercial H3PW12O40 catalyst and also with H2SO4. The optimization of conversion in the reaction was carried out by means of two-level factorial designs. Initially, an exploratory 24 factorial design was carried out in order to identify main factors (molar ratio oleic acid:ethanol, amount of catalyst, temperature and time) affecting % conversion of ester. After that, the 24 factorial design was expanded and adjusted resulting in 25 factorials designs. In one of them, the reactions were carried out including the type of catalyst as a factor to enable a comparative evaluation of both H3PW12O40 and H2SO4. The temperature was the main factor affecting the conversion which increased 27.2 % in media when the temperature changes from 45 to 75 oC. Therefore, the temperature was fixed at 75 oC and the other 25 factorial design, including the heating source conventional or by ultrasound was performed. In this factorial design was observed that the ultrasound-assisted reactions had shown an averaged increasing of 5,5 % in the conversion. The maximum conversion was around 80 % with both of catalysts. Finally, based in the results of factorial designs, experiments with higher temperature, amount of catalyst and time were carried out and a conversion of around 90 % was achieved. The molar ratio of oleic acid:ethanol did not significantly affect the conversion in all conditions investigated. Under the optimized condition the conversion obtained in the heterogeneous reaction with H3PW12O40 was the same of the homogeneous reaction catalyzed by H2SO4. Also, it was carried out a preliminary study of recovery of the catalyst where the characterization by XRD, FTIR, thermal analyses and SEM showed that the recovered catalyst presents the same structural, spectroscopic and thermal properties than a typical of H3PW12O40. The catalyst recovered and treated at 300 °C was employed in a conventional esterification reaction and the conversion equivalent to that one with catalyst used for the first time was found.Neste trabalho investigou-se a síntese do ácido fosfotúngstico e a otimização da reação de esterificação do ácido oléico com etanol. A síntese do catalisador ácido fosfotúngstico foi realizada pelo método convencional e por método assistido por microondas. Os catalisadores sintetizados e um comercial foram caracterizados por análises térmicas, DRX, FTIR, MEV e medidas de área de superfície, sendo observadas as propriedades características do H3PW12O40. As reações de esterificação foram realizadas com catalisador comercial de H3PW12O40 e também com H2SO4. A otimização da conversão na reação foi conduzida por meio de planejamentos fatoriais de dois níveis. Inicialmente, foi realizado um planejamento fatorial 24 exploratório com o intuito de verificar quais fatores (razão molar ácido oléico:etanol, quantidade de catalisador, temperatura e tempo) afetam a % de conversão. Em seguida o planejamento 24 foi ampliado e ajustado resultando em dois planejamentos fatoriais 25. Em um deles as reações foram realizadas acrescentando o fator tipo de catalisador, para avaliar comparativamente o efeito do H3PW12O40 e do H2SO4. A temperatura foi o fator que mais afetou a reação, pois passando de 45 para 75 oC verificou-se que conversão aumenta, em média 27,2 %. Desta forma, fixou-se a temperatura em 75 oC e realizou-se outro planejamento 25 incluindo-se o fator fonte de aquecimento, convencional ou por ultrassom. Neste planejamento foi observado que as reações assistidas por ultrassom apresentaram aumento médio de 5,5 % na conversão e atingiu-se conversão máxima em torno de 80 %, com os dois catalisadores. No final, baseado nos resultados dos planejamentos fatoriais foram realizados experimentos com aumento da temperatura, da quantidade de catalisador e do tempo sendo que a conversão máxima alcançada foi em torno de 90 %.A razão molar ácido oléico:etanol não afetou significativamente a conversão em todas as condições investigadas. Na condição otimizada, a conversão obtida na reação heterogênea com H3PW12O40 foi a mesma que a reação homogênea catalisada pelo H2SO4. Também foi realizado um estudo preliminar de recuperação do catalisador onde a caracterização por DRX, FTIR, análises térmicas e MEV mostrou que o catalisador recuperado apresenta propriedades estruturais, espectroscópicas e térmicas típicos do H3PW12O40. O catalisador recuperado e tratado a 300 oC foi empregado na reação de esterificação e a conversão alcançada foi semelhante àquela obtida com o catalisador usado pela primeira vez.Universidade Federal de Mato GrossoBrasilInstituto de Ciências Exatas e da Terra (ICET)UFMT CUC - CuiabáPrograma de Pós-Graduação em QuímicaTerezo, Ailton Joséhttp://lattes.cnpq.br/3542217308732577Terezo, Ailton José674.006.399-00http://lattes.cnpq.br/3542217308732577Baroni, Adriano Cesar de Morais.http://lattes.cnpq.br/4367207586000817674.006.399-00Sousa Junior, Paulo Teixeira de150.811.331-91http://lattes.cnpq.br/9217526978424330Soares, Mário Rodrigo dos Santos2019-11-28T13:44:56Z2013-08-262019-11-28T13:44:56Z2013-05-24info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisSOARES, Mário Rodrigo dos Santos. Síntese do ácido fosfotúngstico e otimização da reação de esterificação do ácido oléico com etanol. 2013. 88 f. Dissertação (Mestrado em Química) - Universidade Federal de Mato Grosso, Instituto de Ciências Exatas e da Terra, Cuiabá, 2013.http://ri.ufmt.br/handle/1/1618porinfo:eu-repo/semantics/openAccessreponame:Repositório Institucional da UFMTinstname:Universidade Federal de Mato Grosso (UFMT)instacron:UFMT2019-11-30T06:03:41Zoai:localhost:1/1618Repositório InstitucionalPUBhttp://ri.ufmt.br/oai/requestjordanbiblio@gmail.comopendoar:2019-11-30T06:03:41Repositório Institucional da UFMT - Universidade Federal de Mato Grosso (UFMT)false
dc.title.none.fl_str_mv Síntese do ácido fosfotúngstico e otimização da reação de esterificação do ácido oléico com etanol
title Síntese do ácido fosfotúngstico e otimização da reação de esterificação do ácido oléico com etanol
spellingShingle Síntese do ácido fosfotúngstico e otimização da reação de esterificação do ácido oléico com etanol
Soares, Mário Rodrigo dos Santos
.
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
.
title_short Síntese do ácido fosfotúngstico e otimização da reação de esterificação do ácido oléico com etanol
title_full Síntese do ácido fosfotúngstico e otimização da reação de esterificação do ácido oléico com etanol
title_fullStr Síntese do ácido fosfotúngstico e otimização da reação de esterificação do ácido oléico com etanol
title_full_unstemmed Síntese do ácido fosfotúngstico e otimização da reação de esterificação do ácido oléico com etanol
title_sort Síntese do ácido fosfotúngstico e otimização da reação de esterificação do ácido oléico com etanol
author Soares, Mário Rodrigo dos Santos
author_facet Soares, Mário Rodrigo dos Santos
author_role author
dc.contributor.none.fl_str_mv Terezo, Ailton José
http://lattes.cnpq.br/3542217308732577
Terezo, Ailton José
674.006.399-00
http://lattes.cnpq.br/3542217308732577
Baroni, Adriano Cesar de Morais
.
http://lattes.cnpq.br/4367207586000817
674.006.399-00
Sousa Junior, Paulo Teixeira de
150.811.331-91
http://lattes.cnpq.br/9217526978424330
dc.contributor.author.fl_str_mv Soares, Mário Rodrigo dos Santos
dc.subject.por.fl_str_mv .
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
.
topic .
CNPQ::CIENCIAS EXATAS E DA TERRA::QUIMICA
.
description In this work the synthesis of phosphotungstic acid and optimization of esterification reaction of oleic acid with ethanol were investigated. The synthesis of the catalyst H3PW12O40 by conventional and microwave assisted methods were performed. The catalysts synthesized and a commercial were characterized by thermal analyses, XRD, FTIR, SEM and of surface area measurements, being observed characteristic properties of the H3PW12O40. The esterification reactions were performed with a commercial H3PW12O40 catalyst and also with H2SO4. The optimization of conversion in the reaction was carried out by means of two-level factorial designs. Initially, an exploratory 24 factorial design was carried out in order to identify main factors (molar ratio oleic acid:ethanol, amount of catalyst, temperature and time) affecting % conversion of ester. After that, the 24 factorial design was expanded and adjusted resulting in 25 factorials designs. In one of them, the reactions were carried out including the type of catalyst as a factor to enable a comparative evaluation of both H3PW12O40 and H2SO4. The temperature was the main factor affecting the conversion which increased 27.2 % in media when the temperature changes from 45 to 75 oC. Therefore, the temperature was fixed at 75 oC and the other 25 factorial design, including the heating source conventional or by ultrasound was performed. In this factorial design was observed that the ultrasound-assisted reactions had shown an averaged increasing of 5,5 % in the conversion. The maximum conversion was around 80 % with both of catalysts. Finally, based in the results of factorial designs, experiments with higher temperature, amount of catalyst and time were carried out and a conversion of around 90 % was achieved. The molar ratio of oleic acid:ethanol did not significantly affect the conversion in all conditions investigated. Under the optimized condition the conversion obtained in the heterogeneous reaction with H3PW12O40 was the same of the homogeneous reaction catalyzed by H2SO4. Also, it was carried out a preliminary study of recovery of the catalyst where the characterization by XRD, FTIR, thermal analyses and SEM showed that the recovered catalyst presents the same structural, spectroscopic and thermal properties than a typical of H3PW12O40. The catalyst recovered and treated at 300 °C was employed in a conventional esterification reaction and the conversion equivalent to that one with catalyst used for the first time was found.
publishDate 2013
dc.date.none.fl_str_mv 2013-08-26
2013-05-24
2019-11-28T13:44:56Z
2019-11-28T13:44:56Z
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.uri.fl_str_mv SOARES, Mário Rodrigo dos Santos. Síntese do ácido fosfotúngstico e otimização da reação de esterificação do ácido oléico com etanol. 2013. 88 f. Dissertação (Mestrado em Química) - Universidade Federal de Mato Grosso, Instituto de Ciências Exatas e da Terra, Cuiabá, 2013.
http://ri.ufmt.br/handle/1/1618
identifier_str_mv SOARES, Mário Rodrigo dos Santos. Síntese do ácido fosfotúngstico e otimização da reação de esterificação do ácido oléico com etanol. 2013. 88 f. Dissertação (Mestrado em Química) - Universidade Federal de Mato Grosso, Instituto de Ciências Exatas e da Terra, Cuiabá, 2013.
url http://ri.ufmt.br/handle/1/1618
dc.language.iso.fl_str_mv por
language por
dc.rights.driver.fl_str_mv info:eu-repo/semantics/openAccess
eu_rights_str_mv openAccess
dc.publisher.none.fl_str_mv Universidade Federal de Mato Grosso
Brasil
Instituto de Ciências Exatas e da Terra (ICET)
UFMT CUC - Cuiabá
Programa de Pós-Graduação em Química
publisher.none.fl_str_mv Universidade Federal de Mato Grosso
Brasil
Instituto de Ciências Exatas e da Terra (ICET)
UFMT CUC - Cuiabá
Programa de Pós-Graduação em Química
dc.source.none.fl_str_mv reponame:Repositório Institucional da UFMT
instname:Universidade Federal de Mato Grosso (UFMT)
instacron:UFMT
instname_str Universidade Federal de Mato Grosso (UFMT)
instacron_str UFMT
institution UFMT
reponame_str Repositório Institucional da UFMT
collection Repositório Institucional da UFMT
repository.name.fl_str_mv Repositório Institucional da UFMT - Universidade Federal de Mato Grosso (UFMT)
repository.mail.fl_str_mv jordanbiblio@gmail.com
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