Óxido de zinco dopado para produção de biodiesel
| Ano de defesa: | 2016 |
|---|---|
| Autor(a) principal: | |
| Orientador(a): | |
| Banca de defesa: | |
| Tipo de documento: | Tese |
| Tipo de acesso: | Acesso aberto |
| Idioma: | por |
| Instituição de defesa: |
Universidade Federal da Paraíba
Brasil Química Programa de Pós-Graduação em Química UFPB |
| Programa de Pós-Graduação: |
Não Informado pela instituição
|
| Departamento: |
Não Informado pela instituição
|
| País: |
Não Informado pela instituição
|
| Palavras-chave em Português: | |
| Link de acesso: | https://repositorio.ufpb.br/jspui/handle/tede/9190 |
Resumo: | Powders of pure zinc oxide (ZnO) and zinc oxide doped with 5% Al3+ (ZNAL) were obtained by the Pechini method using Zn(NO3)2.6H2O and Al(NO3)3.6H2O as precursors. The characterization was performed using XRD, Raman, FTIR and UV-Vis, and stoichiometry was confirmed by XRF. The results obtained by Raman and XRD indicated that Al3+ is completely incorporated into the ZnO crystal lattice. Attempts of doping ZnO with Fe3+ lead to a secondary phase which, according to ICCD 01-070-3377, was assigned to ZnFe2O4, for this reason this oxide was not used as a catalyst. Tests of pH variation with the oxides in acidic and basic media indicated that ZNAL presents a much larger basic character than ZnO. Using a 23 factorial design, ZnO and ZNAL were tested as catalysts for the ethanolic transesterification of cottonseed oil at temperature 130 and 200 °C, alcohol/oil ratio of 6:1 and 12:1 and 3% catalyst (w/w relative to the oil ). The reactions were performed in the Parr reactor for 4 hours and agitation of 600 rpm. 1H NMR and 13C NMR spectroscopies were used to characterize and evaluate the ethyl ester content produced during transesterifications indicating that 5% of Al3+ addition into the crystalline ZnO lattice significantly increased the catalytic potential of the oxide, reaching a higher conversion ratio of 81% when T = 130 °C and greater than 94% when T = 200 °C. The results analyzed by factorial design indicated that the type of catalyst and the temperature were the most determining factors in conversion rates. Using a kinetic study at temperatures of 130, 160, 180 and 200 °C and reaction times of 30, 60, 120 and 240 minutes, it was observed that the reactions catalyzed by ZnO had a linear behavior conversion rate, while reaction catalyzed by ZNAL reached rates greater than 80%of conversion after 30 minutes when T = 200 °C. It was also observed that the rate of ethanolic transesterification of cottonsed oil was influenced by mass transport phenomena when catalyzed by ZnO. For transesterifications catalysed by ZNAL a 1st order behavior was observed at T = 130 ° C and 2nd order was observed for the other temperatures. |
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Óxido de zinco dopado para produção de biodieselDopagemCatálise heterogêneaTransesterificaçãoCinética QuímicaDopingHeterogeneous catalysisTransesterificationChemical kineticsCIENCIAS EXATAS E DA TERRA::QUIMICAPowders of pure zinc oxide (ZnO) and zinc oxide doped with 5% Al3+ (ZNAL) were obtained by the Pechini method using Zn(NO3)2.6H2O and Al(NO3)3.6H2O as precursors. The characterization was performed using XRD, Raman, FTIR and UV-Vis, and stoichiometry was confirmed by XRF. The results obtained by Raman and XRD indicated that Al3+ is completely incorporated into the ZnO crystal lattice. Attempts of doping ZnO with Fe3+ lead to a secondary phase which, according to ICCD 01-070-3377, was assigned to ZnFe2O4, for this reason this oxide was not used as a catalyst. Tests of pH variation with the oxides in acidic and basic media indicated that ZNAL presents a much larger basic character than ZnO. Using a 23 factorial design, ZnO and ZNAL were tested as catalysts for the ethanolic transesterification of cottonseed oil at temperature 130 and 200 °C, alcohol/oil ratio of 6:1 and 12:1 and 3% catalyst (w/w relative to the oil ). The reactions were performed in the Parr reactor for 4 hours and agitation of 600 rpm. 1H NMR and 13C NMR spectroscopies were used to characterize and evaluate the ethyl ester content produced during transesterifications indicating that 5% of Al3+ addition into the crystalline ZnO lattice significantly increased the catalytic potential of the oxide, reaching a higher conversion ratio of 81% when T = 130 °C and greater than 94% when T = 200 °C. The results analyzed by factorial design indicated that the type of catalyst and the temperature were the most determining factors in conversion rates. Using a kinetic study at temperatures of 130, 160, 180 and 200 °C and reaction times of 30, 60, 120 and 240 minutes, it was observed that the reactions catalyzed by ZnO had a linear behavior conversion rate, while reaction catalyzed by ZNAL reached rates greater than 80%of conversion after 30 minutes when T = 200 °C. It was also observed that the rate of ethanolic transesterification of cottonsed oil was influenced by mass transport phenomena when catalyzed by ZnO. For transesterifications catalysed by ZNAL a 1st order behavior was observed at T = 130 ° C and 2nd order was observed for the other temperatures.Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPESPós de óxido de zinco puro (ZnO) e de óxido de zinco dopado com 5% de Al3+ (ZNAL) foram obtidos pelo método Pechini utilizando Zn(NO3)2.6H2O e Al(NO3)3.6H2O como precursores. A caracterização foi realizada através de DRX, Raman, FTIR e UV-Vis, tendo a estequiometria confirmada por FRX. Os resultados do estudo de caracterização por UV-vis e Raman, indicaram que Al3+ encontra-se completamente incorporado à rede cristalina do ZnO. Tentativas de dopagem com Fe3+ apresentaram fase secundária que, de acordo com a carta ICCD 01-070-3377, foi atribuída a ZnFe2O4, por esse motivo este óxido não foi utilizado como catlisador. Testes de variação de pH com os óxidos em meio ácido e básico indicaram que ZNAL apresenta um caráter básico muito maior do que ZnO. Utilizando um planejamento fatorial 23, ZnO e ZNAL foram testados como catalisadores na transesterificação etanólica do óleo de algodão em temperaturas de 130 e 200 oC, relações álcool/óleo 6:1 e 12:1 e 3% (m/m em relação ao óleo) de catalisador. As reações ocorreram em reator Parr com tempo de 4 horas e rotação de 600 rpm. As espectroscopias RMN 1H e 13C foram utilizadas para caracterizar e avaliar o teor de ésteres etílicos produzidos nas transesterificações indicando que a adição de 5% de Al3+ à rede cristalina do ZnO aumentou significativamente o potencial catalítico do óxido, chegando a um índice de conversão superior a 81% a T = 130 oC e maior que 94% a T = 200 oC. Os resultados analisados pelo planejamento fatorial indicaram que o tipo de catalisador e a temperatura foram os fatores mais determinantes nos índices de conversão. Através de um estudo cinético utilizando temperaturas de 130, 160, 180 e 200 oC e tempos reacionais de 30, 60, 120 e 240 minutos, observou-se que as reações catalisadas por ZnO tiveram um comportamento linear de índice de conversão, enquanto que, as catalisadas por ZNAL chegaram a índices superiores a 80% de conversão em apenas 30 minutos quando T = 200 oC. Também foi possível observar que as transesterificações etanólicas do óleo de algodão foram influenciadas pela transferência de massa, abaixo de 120 minutos de reação, quando catalisadas por ZnO. Para as etanólises catalisadas por ZNAL observou-se um comportamento de 1ª ordem quando T = 130 oC e de 2ª ordem nas demais temperaturas.Universidade Federal da ParaíbaBrasilQuímicaPrograma de Pós-Graduação em QuímicaUFPBSantos, Iêda Maria Garcia doshttp://lattes.cnpq.br/7060067415685353Pontes, Liliana de Fatima Bezerra Lira dehttp://lattes.cnpq.br/0438588394065892Maia, Ary da Silvahttp://lattes.cnpq.br/0234548596508203Pereira, Maria de Fatima2017-08-01T11:30:58Z2018-07-21T00:29:59Z2018-07-21T00:29:59Z2016-08-22info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisapplication/pdfPEREIRA, Maria de Fátima.Óxido de zinco dopado para produção de biodiesel. 2016. 120F. Tese (Doutorado em Química)- Universidade Federal da Paraíba, João Pessoa, 2016.https://repositorio.ufpb.br/jspui/handle/tede/9190porinfo:eu-repo/semantics/openAccessreponame:Repositório Institucional da UFPBinstname:Universidade Federal da Paraíba (UFPB)instacron:UFPB2018-09-06T02:07:31Zoai:repositorio.ufpb.br:tede/9190Repositório InstitucionalPUBhttps://repositorio.ufpb.br/oai/requestdiretoria@ufpb.br||bdtd@biblioteca.ufpb.bropendoar:25462018-09-06T02:07:31Repositório Institucional da UFPB - Universidade Federal da Paraíba (UFPB)false |
| dc.title.none.fl_str_mv |
Óxido de zinco dopado para produção de biodiesel |
| title |
Óxido de zinco dopado para produção de biodiesel |
| spellingShingle |
Óxido de zinco dopado para produção de biodiesel Pereira, Maria de Fatima Dopagem Catálise heterogênea Transesterificação Cinética Química Doping Heterogeneous catalysis Transesterification Chemical kinetics CIENCIAS EXATAS E DA TERRA::QUIMICA |
| title_short |
Óxido de zinco dopado para produção de biodiesel |
| title_full |
Óxido de zinco dopado para produção de biodiesel |
| title_fullStr |
Óxido de zinco dopado para produção de biodiesel |
| title_full_unstemmed |
Óxido de zinco dopado para produção de biodiesel |
| title_sort |
Óxido de zinco dopado para produção de biodiesel |
| author |
Pereira, Maria de Fatima |
| author_facet |
Pereira, Maria de Fatima |
| author_role |
author |
| dc.contributor.none.fl_str_mv |
Santos, Iêda Maria Garcia dos http://lattes.cnpq.br/7060067415685353 Pontes, Liliana de Fatima Bezerra Lira de http://lattes.cnpq.br/0438588394065892 Maia, Ary da Silva http://lattes.cnpq.br/0234548596508203 |
| dc.contributor.author.fl_str_mv |
Pereira, Maria de Fatima |
| dc.subject.por.fl_str_mv |
Dopagem Catálise heterogênea Transesterificação Cinética Química Doping Heterogeneous catalysis Transesterification Chemical kinetics CIENCIAS EXATAS E DA TERRA::QUIMICA |
| topic |
Dopagem Catálise heterogênea Transesterificação Cinética Química Doping Heterogeneous catalysis Transesterification Chemical kinetics CIENCIAS EXATAS E DA TERRA::QUIMICA |
| description |
Powders of pure zinc oxide (ZnO) and zinc oxide doped with 5% Al3+ (ZNAL) were obtained by the Pechini method using Zn(NO3)2.6H2O and Al(NO3)3.6H2O as precursors. The characterization was performed using XRD, Raman, FTIR and UV-Vis, and stoichiometry was confirmed by XRF. The results obtained by Raman and XRD indicated that Al3+ is completely incorporated into the ZnO crystal lattice. Attempts of doping ZnO with Fe3+ lead to a secondary phase which, according to ICCD 01-070-3377, was assigned to ZnFe2O4, for this reason this oxide was not used as a catalyst. Tests of pH variation with the oxides in acidic and basic media indicated that ZNAL presents a much larger basic character than ZnO. Using a 23 factorial design, ZnO and ZNAL were tested as catalysts for the ethanolic transesterification of cottonseed oil at temperature 130 and 200 °C, alcohol/oil ratio of 6:1 and 12:1 and 3% catalyst (w/w relative to the oil ). The reactions were performed in the Parr reactor for 4 hours and agitation of 600 rpm. 1H NMR and 13C NMR spectroscopies were used to characterize and evaluate the ethyl ester content produced during transesterifications indicating that 5% of Al3+ addition into the crystalline ZnO lattice significantly increased the catalytic potential of the oxide, reaching a higher conversion ratio of 81% when T = 130 °C and greater than 94% when T = 200 °C. The results analyzed by factorial design indicated that the type of catalyst and the temperature were the most determining factors in conversion rates. Using a kinetic study at temperatures of 130, 160, 180 and 200 °C and reaction times of 30, 60, 120 and 240 minutes, it was observed that the reactions catalyzed by ZnO had a linear behavior conversion rate, while reaction catalyzed by ZNAL reached rates greater than 80%of conversion after 30 minutes when T = 200 °C. It was also observed that the rate of ethanolic transesterification of cottonsed oil was influenced by mass transport phenomena when catalyzed by ZnO. For transesterifications catalysed by ZNAL a 1st order behavior was observed at T = 130 ° C and 2nd order was observed for the other temperatures. |
| publishDate |
2016 |
| dc.date.none.fl_str_mv |
2016-08-22 2017-08-01T11:30:58Z 2018-07-21T00:29:59Z 2018-07-21T00:29:59Z |
| 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 |
PEREIRA, Maria de Fátima.Óxido de zinco dopado para produção de biodiesel. 2016. 120F. Tese (Doutorado em Química)- Universidade Federal da Paraíba, João Pessoa, 2016. https://repositorio.ufpb.br/jspui/handle/tede/9190 |
| identifier_str_mv |
PEREIRA, Maria de Fátima.Óxido de zinco dopado para produção de biodiesel. 2016. 120F. Tese (Doutorado em Química)- Universidade Federal da Paraíba, João Pessoa, 2016. |
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https://repositorio.ufpb.br/jspui/handle/tede/9190 |
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por |
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Universidade Federal da Paraíba Brasil Química Programa de Pós-Graduação em Química UFPB |
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Universidade Federal da Paraíba Brasil Química Programa de Pós-Graduação em Química UFPB |
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