Influência de líquidos iônicos na extração de fenóis da fração aquosa do bio-óleo da semente de goiaba (Psidium guajava L.) por ultrassom e micro-ondas

Detalhes bibliográficos
Autor(a) principal: Cerqueira, Solange da Conceição Almeida
Data de Publicação: 2020
Tipo de documento: Tese
Idioma: por
Título da fonte: Repositório Institucional da UFS
Texto Completo: https://ri.ufs.br/jspui/handle/riufs/14819
Resumo: The present work sought to develop a method of extracting phenolic compounds present in the aqueous fraction of bio-oil arising from the pyrolysis process of guava seeds. The separation between the organic phase and the aqueous phase was carried out by decantation, after the pyrolysis process of approximately 300 g of biomass at 600 ° C and nitrogen flow of 100 mL min-1 . The conventional liquidliquid extraction method (LLE) was applied using ethyl acetate as a solvent, and methodologies for ultrasound-assisted liquid-liquid extraction (UALLE) and microwave-assisted liquid-liquid extraction (MALLE) were developed. The experiments to study these systems were carried out in batches, according to a statistical factorial design (22 ). Initially, a previous study of the variables temperature and potency in UALLE and volume of solvent and potency in MALLE was carried out to determine the extraction conditions, whose variable evaluated was the concentration of phenol monomers. Finally, a second planning was carried out for both methods in order to evaluate the percentage of ionic liquid (LI) and pH for the extraction of phenols present in the aqueous fraction. By gas chromatography/mass spectrometry it was possible to quantify 12 phenol monomers in this study (phenol, o-cresol, m-cresol, p-cresol, 2,5 dimethylphenol, 4-ethylphenol, guaiacol, o-catechol, 4-methylcatechol, m-catechol, 2,6 dimethoxyphenol and eugenol) and by UV-vis the analysis of total phenols. MALLE proved to be more efficient in relation to LLE and UALLE, with extractions greater than 125% and 53%, respectively. In the study of the extraction of phenols using ethyl acetate combined with LIs, the ionic liquid bis (trifluoromethylsulfonyl) imidate of 1-butyl-3-methylimidazolium (BMIM.NTF2) showed to be more efficient for the extraction of phenols in relation to hexafluorophosphate of 1-butyl-3- methylimidazolium (BMIM.PF6). The extraction of phenols was influenced by the pH of the aqueous fraction, with greater extraction at pH ≤7 and showed recoveries above 80% in both techniques. The microwave assisted extraction process used 6 times less time than ultrasound extraction to obtain extracts with similar concentrations.
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spelling Cerqueira, Solange da Conceição AlmeidaFreitas, Lisiane dos Santos2021-11-30T14:32:31Z2021-11-30T14:32:31Z2020-04-28CERQUEIRA, Solange da Conceição Almeida. Influência de líquidos iônicos na extração de fenóis da fração aquosa do bio-óleo da semente de goiaba (Psidium guajava L.) por ultrassom e micro-ondas. 2020. 142 f. Tese (Doutorado em Química) - Universidade Federal de Sergipe, São Cristóvão, 2020.https://ri.ufs.br/jspui/handle/riufs/14819The present work sought to develop a method of extracting phenolic compounds present in the aqueous fraction of bio-oil arising from the pyrolysis process of guava seeds. The separation between the organic phase and the aqueous phase was carried out by decantation, after the pyrolysis process of approximately 300 g of biomass at 600 ° C and nitrogen flow of 100 mL min-1 . The conventional liquidliquid extraction method (LLE) was applied using ethyl acetate as a solvent, and methodologies for ultrasound-assisted liquid-liquid extraction (UALLE) and microwave-assisted liquid-liquid extraction (MALLE) were developed. The experiments to study these systems were carried out in batches, according to a statistical factorial design (22 ). Initially, a previous study of the variables temperature and potency in UALLE and volume of solvent and potency in MALLE was carried out to determine the extraction conditions, whose variable evaluated was the concentration of phenol monomers. Finally, a second planning was carried out for both methods in order to evaluate the percentage of ionic liquid (LI) and pH for the extraction of phenols present in the aqueous fraction. By gas chromatography/mass spectrometry it was possible to quantify 12 phenol monomers in this study (phenol, o-cresol, m-cresol, p-cresol, 2,5 dimethylphenol, 4-ethylphenol, guaiacol, o-catechol, 4-methylcatechol, m-catechol, 2,6 dimethoxyphenol and eugenol) and by UV-vis the analysis of total phenols. MALLE proved to be more efficient in relation to LLE and UALLE, with extractions greater than 125% and 53%, respectively. In the study of the extraction of phenols using ethyl acetate combined with LIs, the ionic liquid bis (trifluoromethylsulfonyl) imidate of 1-butyl-3-methylimidazolium (BMIM.NTF2) showed to be more efficient for the extraction of phenols in relation to hexafluorophosphate of 1-butyl-3- methylimidazolium (BMIM.PF6). The extraction of phenols was influenced by the pH of the aqueous fraction, with greater extraction at pH ≤7 and showed recoveries above 80% in both techniques. The microwave assisted extraction process used 6 times less time than ultrasound extraction to obtain extracts with similar concentrations.O presente trabalho buscou desenvolver um método de extração de compostos fenólicos presentes na fração aquosa do bio-óleo advindo do processo de pirólise das sementes de goiaba. A separação entre a fase orgânica e a fase aquosa foi realizada por decantação, após o processo de pirólise de aproximadamente 300 g de biomassa à 600 °C e fluxo de nitrogênio de 100 mL min-1 . Foi aplicado o método de extração líquido-líquido (LLE) convencional utilizando acetato de etila como solvente, e desenvolvidas metodologias de extração líquido-líquido assistida por ultrassom (UALLE) e extração líquido-líquido assistida por microondas (MALLE). Os experimentos para estudo destes sistemas foram realizados em batelada, de acordo com um planejamento fatorial estatístico (22 ). Inicialmente foi realizado um estudo prévio das variáveis temperatura e potência na UALLE e volume de solvente e potência na MALLE para a determinação das condições de extração, cuja variável avaliada foi concentração de monômeros de fenóis. Por fim foi realizado um segundo planejamento para ambos os métodos com a finalidade de avaliar a porcentagem de líquido iônico (LI) e pH para a extração de fenóis presentes na fração aquosa. Por cromatografia gasosa/espectrometria de massas foi possível quantificar 12 monômeros de fenóis neste estudo (fenol, o-cresol, m-cresol, p-cresol, 2,5 dimetilfenol, 4- etilfenol, guaiacol, o-catecol, 4-metilcatecol, m-catecol, 2,6 dimetoxifenol e eugenol) e por UV-vis a análise de fenóis totais. A MALLE se mostrou mais eficientes em relação a LLE e a UALLE, com extrações superiores a 125% e 53%, respectivamente. No estudo da extração de fenóis usando acetato de etila combinado a LIs, o líquido iônico bis(trifluormetilsulfonil) imidato de 1-butil-3- metilimidazólio (BMIM.NTF2) apresentou ser mais eficiente para a extração dos fenóis em relação ao hexafluorfosfato de 1-butil-3-metilimidazólio (BMIM.PF6). A extração de fenóis foi influenciada pelo pH da fração aquosa, com maior extração em pH ≤7 e apresentaram recuperações acima de 80% em ambas as técnicas. O processo de extração assistida por micro-ondas utilizou um tempo 6 vezes menor que a extração por ultrassom para obter extratos com concentrações semelhantes.São Cristóvão, SEporQuímicaFenóisLíquidosMicro-ondasUltrassomPiróliseBMIM.NTF2BMIM.PF6Micro-ondasFração aquosa da pirólisePhenolsMicrowavesUltrasoundAqueous pyrolysis fractionCIENCIAS EXATAS E DA TERRA::QUIMICAInfluência de líquidos iônicos na extração de fenóis da fração aquosa do bio-óleo da semente de goiaba (Psidium guajava L.) por ultrassom e micro-ondasInfluence of ionic liquids in the extraction of phenols from aqueous fraction bio-oil of guava seed (Psidium guajava l.) by ultrasound and microwaveinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisPós-Graduação em QuímicaUniversidade Federal de Sergipereponame:Repositório Institucional da UFSinstname:Universidade Federal de Sergipe (UFS)instacron:UFSinfo:eu-repo/semantics/openAccessTEXTSOLANGE_CONCEICAO_ALMEIDA_CERQUEIRA.pdf.txtSOLANGE_CONCEICAO_ALMEIDA_CERQUEIRA.pdf.txtExtracted texttext/plain230998https://ri.ufs.br/jspui/bitstream/riufs/14819/3/SOLANGE_CONCEICAO_ALMEIDA_CERQUEIRA.pdf.txtec3ee186ef8347e1ad5c9b2e1071e46fMD53THUMBNAILSOLANGE_CONCEICAO_ALMEIDA_CERQUEIRA.pdf.jpgSOLANGE_CONCEICAO_ALMEIDA_CERQUEIRA.pdf.jpgGenerated Thumbnailimage/jpeg1491https://ri.ufs.br/jspui/bitstream/riufs/14819/4/SOLANGE_CONCEICAO_ALMEIDA_CERQUEIRA.pdf.jpg762c67fc0a215436e16e5669ddd51792MD54LICENSElicense.txtlicense.txttext/plain; charset=utf-81475https://ri.ufs.br/jspui/bitstream/riufs/14819/1/license.txt098cbbf65c2c15e1fb2e49c5d306a44cMD51ORIGINALSOLANGE_CONCEICAO_ALMEIDA_CERQUEIRA.pdfSOLANGE_CONCEICAO_ALMEIDA_CERQUEIRA.pdfapplication/pdf3570468https://ri.ufs.br/jspui/bitstream/riufs/14819/2/SOLANGE_CONCEICAO_ALMEIDA_CERQUEIRA.pdfb6122e6fee4f9d20d5bd902a881ac0e3MD52riufs/148192021-11-30 11:32:31.911oai:ufs.br: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Repositório InstitucionalPUBhttps://ri.ufs.br/oai/requestrepositorio@academico.ufs.bropendoar:2021-11-30T14:32:31Repositório Institucional da UFS - Universidade Federal de Sergipe (UFS)false
dc.title.pt_BR.fl_str_mv Influência de líquidos iônicos na extração de fenóis da fração aquosa do bio-óleo da semente de goiaba (Psidium guajava L.) por ultrassom e micro-ondas
dc.title.alternative.eng.fl_str_mv Influence of ionic liquids in the extraction of phenols from aqueous fraction bio-oil of guava seed (Psidium guajava l.) by ultrasound and microwave
title Influência de líquidos iônicos na extração de fenóis da fração aquosa do bio-óleo da semente de goiaba (Psidium guajava L.) por ultrassom e micro-ondas
spellingShingle Influência de líquidos iônicos na extração de fenóis da fração aquosa do bio-óleo da semente de goiaba (Psidium guajava L.) por ultrassom e micro-ondas
Cerqueira, Solange da Conceição Almeida
Química
Fenóis
Líquidos
Micro-ondas
Ultrassom
Pirólise
BMIM.NTF2
BMIM.PF6
Micro-ondas
Fração aquosa da pirólise
Phenols
Microwaves
Ultrasound
Aqueous pyrolysis fraction
CIENCIAS EXATAS E DA TERRA::QUIMICA
title_short Influência de líquidos iônicos na extração de fenóis da fração aquosa do bio-óleo da semente de goiaba (Psidium guajava L.) por ultrassom e micro-ondas
title_full Influência de líquidos iônicos na extração de fenóis da fração aquosa do bio-óleo da semente de goiaba (Psidium guajava L.) por ultrassom e micro-ondas
title_fullStr Influência de líquidos iônicos na extração de fenóis da fração aquosa do bio-óleo da semente de goiaba (Psidium guajava L.) por ultrassom e micro-ondas
title_full_unstemmed Influência de líquidos iônicos na extração de fenóis da fração aquosa do bio-óleo da semente de goiaba (Psidium guajava L.) por ultrassom e micro-ondas
title_sort Influência de líquidos iônicos na extração de fenóis da fração aquosa do bio-óleo da semente de goiaba (Psidium guajava L.) por ultrassom e micro-ondas
author Cerqueira, Solange da Conceição Almeida
author_facet Cerqueira, Solange da Conceição Almeida
author_role author
dc.contributor.author.fl_str_mv Cerqueira, Solange da Conceição Almeida
dc.contributor.advisor1.fl_str_mv Freitas, Lisiane dos Santos
contributor_str_mv Freitas, Lisiane dos Santos
dc.subject.por.fl_str_mv Química
Fenóis
Líquidos
Micro-ondas
Ultrassom
Pirólise
BMIM.NTF2
BMIM.PF6
Micro-ondas
Fração aquosa da pirólise
topic Química
Fenóis
Líquidos
Micro-ondas
Ultrassom
Pirólise
BMIM.NTF2
BMIM.PF6
Micro-ondas
Fração aquosa da pirólise
Phenols
Microwaves
Ultrasound
Aqueous pyrolysis fraction
CIENCIAS EXATAS E DA TERRA::QUIMICA
dc.subject.eng.fl_str_mv Phenols
Microwaves
Ultrasound
Aqueous pyrolysis fraction
dc.subject.cnpq.fl_str_mv CIENCIAS EXATAS E DA TERRA::QUIMICA
description The present work sought to develop a method of extracting phenolic compounds present in the aqueous fraction of bio-oil arising from the pyrolysis process of guava seeds. The separation between the organic phase and the aqueous phase was carried out by decantation, after the pyrolysis process of approximately 300 g of biomass at 600 ° C and nitrogen flow of 100 mL min-1 . The conventional liquidliquid extraction method (LLE) was applied using ethyl acetate as a solvent, and methodologies for ultrasound-assisted liquid-liquid extraction (UALLE) and microwave-assisted liquid-liquid extraction (MALLE) were developed. The experiments to study these systems were carried out in batches, according to a statistical factorial design (22 ). Initially, a previous study of the variables temperature and potency in UALLE and volume of solvent and potency in MALLE was carried out to determine the extraction conditions, whose variable evaluated was the concentration of phenol monomers. Finally, a second planning was carried out for both methods in order to evaluate the percentage of ionic liquid (LI) and pH for the extraction of phenols present in the aqueous fraction. By gas chromatography/mass spectrometry it was possible to quantify 12 phenol monomers in this study (phenol, o-cresol, m-cresol, p-cresol, 2,5 dimethylphenol, 4-ethylphenol, guaiacol, o-catechol, 4-methylcatechol, m-catechol, 2,6 dimethoxyphenol and eugenol) and by UV-vis the analysis of total phenols. MALLE proved to be more efficient in relation to LLE and UALLE, with extractions greater than 125% and 53%, respectively. In the study of the extraction of phenols using ethyl acetate combined with LIs, the ionic liquid bis (trifluoromethylsulfonyl) imidate of 1-butyl-3-methylimidazolium (BMIM.NTF2) showed to be more efficient for the extraction of phenols in relation to hexafluorophosphate of 1-butyl-3- methylimidazolium (BMIM.PF6). The extraction of phenols was influenced by the pH of the aqueous fraction, with greater extraction at pH ≤7 and showed recoveries above 80% in both techniques. The microwave assisted extraction process used 6 times less time than ultrasound extraction to obtain extracts with similar concentrations.
publishDate 2020
dc.date.issued.fl_str_mv 2020-04-28
dc.date.accessioned.fl_str_mv 2021-11-30T14:32:31Z
dc.date.available.fl_str_mv 2021-11-30T14:32:31Z
dc.type.status.fl_str_mv info:eu-repo/semantics/publishedVersion
dc.type.driver.fl_str_mv info:eu-repo/semantics/doctoralThesis
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dc.identifier.citation.fl_str_mv CERQUEIRA, Solange da Conceição Almeida. Influência de líquidos iônicos na extração de fenóis da fração aquosa do bio-óleo da semente de goiaba (Psidium guajava L.) por ultrassom e micro-ondas. 2020. 142 f. Tese (Doutorado em Química) - Universidade Federal de Sergipe, São Cristóvão, 2020.
dc.identifier.uri.fl_str_mv https://ri.ufs.br/jspui/handle/riufs/14819
identifier_str_mv CERQUEIRA, Solange da Conceição Almeida. Influência de líquidos iônicos na extração de fenóis da fração aquosa do bio-óleo da semente de goiaba (Psidium guajava L.) por ultrassom e micro-ondas. 2020. 142 f. Tese (Doutorado em Química) - Universidade Federal de Sergipe, São Cristóvão, 2020.
url https://ri.ufs.br/jspui/handle/riufs/14819
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