Síntese e caracterização de redes poliméricas a base de poli(dimetilsiloxano) e metacrilato de 2-(dimetilamino)etila para adsorção de íons cobre(II) de soluções aquosas
| 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 de Alfenas
|
| Programa de Pós-Graduação: |
Programa de Pós-Graduação em Química
|
| Departamento: |
Instituto de Química
|
| País: |
Brasil
|
| Palavras-chave em Português: | |
| Área do conhecimento CNPq: | |
| Link de acesso: | https://repositorio.unifal-mg.edu.br/handle/123456789/981 |
Resumo: | Two novel organic-inorganic hybrid adsorbents based on poly(dimethylsiloxane) (PDMS) and 2-(dimethylamino)ethyl methacrylate (DMAEMA) were prepared and applied for the removal of copper(II) ions in aqueous media. The materials were characterized by Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), swelling measurements and nuclear magnetic resonance (NMR). Semi-interpenetrating polymer networks (semi-IPNs) were prepared with 1:0.5 weight ratio for PDMS:PDMAEMA in 1:0.4 and 1:1 molar ratios of PDMS and the crosslinker agent (3-chloropropyl)trimethoxysilane (CPTMS), respectively. Only the network with the highest amount of CPTMS was stable in water. This semi-IPN was able to adsorb about 34 % in mass of water, indicating that was obtained a material with higher hydrophilic character. The adsorption experiments results of copper(II) ions at room temperature reveal a high pH-dependence, reaching uptake capacity of 0.40 mmol g-¹ at pH 5 within 36 h. The adsorbent-adsorbate system was described by the pseudo-first order kinetic model and Sips adsorption model. Furthermore, reuse experiments suggested that PDMS/PDMAEMA semi-IPN could be a potential recyclable adsorbent in the treatment of aqueous systems. The second hybrid adsorbent was prepared by the polycondensation of poly(dimethylsiloxane) containing silanol terminals groups and methoxy groups of a previous prepared copolymer, the poly[vinyltrimethoxysilane-co-2-(dimethylamino)ethyl methacrylate]. This adsorbent reached the swelling equilibrium at 23 % in mass of water, after approximately 18 days. The saturation of the active sites of the material was observed at pH 5, after 3 days, with each gram of material capable of adsorbing 0.48 mmol of copper(II) ions. The fractionaryorder and Sips model provided the best fit to the experimental data in kinetic and equilibrium studies of the adsorption process, respectively. Moreover, the reusability for this cross-linked organic–inorganic hybrid adsorbent was studied through usage-regeneration cycles without significant loss in its initial activity. |
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Silva, Fábio Antônio Belinellihttp://lattes.cnpq.br/4560803280050919Molina, Eduardo FerreiraAlmeida, Eduardo Tonon DeSchiavon, Marco AntônioLuccas, Pedro OrivalPissetti, Fábio Luizhttp://lattes.cnpq.br/59208410605926502017-06-13T17:59:29Z2016-04-01SILVA, Fábio Antônio Belinelli. Síntese e caracterização de redes poliméricas a base de poli(dimetilsiloxano) e metacrilato de 2-(dimetilamino)etila para adsorção de íons cobre(II) de soluções aquosas. 2016. 81 f. Tese (Doutorado em Química) - Universidade Federal de Alfenas, Alfenas, MG, 2016.https://repositorio.unifal-mg.edu.br/handle/123456789/981Two novel organic-inorganic hybrid adsorbents based on poly(dimethylsiloxane) (PDMS) and 2-(dimethylamino)ethyl methacrylate (DMAEMA) were prepared and applied for the removal of copper(II) ions in aqueous media. The materials were characterized by Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), swelling measurements and nuclear magnetic resonance (NMR). Semi-interpenetrating polymer networks (semi-IPNs) were prepared with 1:0.5 weight ratio for PDMS:PDMAEMA in 1:0.4 and 1:1 molar ratios of PDMS and the crosslinker agent (3-chloropropyl)trimethoxysilane (CPTMS), respectively. Only the network with the highest amount of CPTMS was stable in water. This semi-IPN was able to adsorb about 34 % in mass of water, indicating that was obtained a material with higher hydrophilic character. The adsorption experiments results of copper(II) ions at room temperature reveal a high pH-dependence, reaching uptake capacity of 0.40 mmol g-¹ at pH 5 within 36 h. The adsorbent-adsorbate system was described by the pseudo-first order kinetic model and Sips adsorption model. Furthermore, reuse experiments suggested that PDMS/PDMAEMA semi-IPN could be a potential recyclable adsorbent in the treatment of aqueous systems. The second hybrid adsorbent was prepared by the polycondensation of poly(dimethylsiloxane) containing silanol terminals groups and methoxy groups of a previous prepared copolymer, the poly[vinyltrimethoxysilane-co-2-(dimethylamino)ethyl methacrylate]. This adsorbent reached the swelling equilibrium at 23 % in mass of water, after approximately 18 days. The saturation of the active sites of the material was observed at pH 5, after 3 days, with each gram of material capable of adsorbing 0.48 mmol of copper(II) ions. The fractionaryorder and Sips model provided the best fit to the experimental data in kinetic and equilibrium studies of the adsorption process, respectively. Moreover, the reusability for this cross-linked organic–inorganic hybrid adsorbent was studied through usage-regeneration cycles without significant loss in its initial activity.Dois novos adsorventes híbridos orgânico-inorgânicos a base de poli(dimetilsiloxano) (PDMS) e metacrilato de 2-(dimetilamino)etila (DMAEMA) foram preparados e aplicados na remoção de íons cobre(II) em meio aquoso. Os materiais obtidos foram caracterizados por espectroscopia na região do infravermelho (FTIR), calorimetria exploratória diferencial (DSC), análise termogravimétrica (TGA), microscopia eletrônica de varredura (MEV), ensaios de intumescimento e ressonância magnética nuclear (RMN). Redes poliméricas semiinterpenetrantes (semi-IPNs) foram obtidas numa razão em massa de 1:0,5 entre PDMS:PDMAEMA em razões molares de 1:0,4 e 1:1 entre PDMS e o agente reticulante (3-cloropropil)trimetoxissilano (CPTMS). Somente a rede com a maior quantidade de CPTMS foi estável em água. Esta semi-IPN foi capaz de adsorver cerca de 34% em massa de água, indicando que foi obtido um material com maior caráter hidrofílico. Os resultados dos experimentos de adsorção de íons cobre(II) à temperatura ambiente evidenciam uma elevada dependência do pH, atingindo a capacidade de remoção de 0,40 mmol g-¹ num pH = 5 no prazo de 36 h. O sistema adsorvente-adsorvato foi descrito pelo modelo cinético de pseudoprimeira ordem e modelo de adsorção de Sips. Além disso, os testes de reutilização sugeriram que a semi-IPN PDMS/PDMAEMA tem um potencial como adsorvente reciclável no tratamento de sistemas aquosos. O segundo adsorvente híbrido foi preparado por uma policondensação entre poli(dimetilsiloxano) com terminações silanóis e grupos metóxidos de um copolímero, o poli[viniltrimetoxissilano-co-metacrilato de 2-(dimetilamino)etila]. Este adsorvente atingiu o equilíbrio de intumescimento com 23 % em massa de água, após aproximadamente 18 dias. Nos estudos de adsorção, a saturação dos sítios ativos do material foi observada em pH = 5, após 3 dias, onde cada grama de material foi capaz de adsorver 0,48 mmol de íons cobre(II). Os modelos de ordem fracionária e de Sips forneceram os melhores ajustes para os dados experimentais nos estudos cinéticos e de equilíbrio, respectivamente. Além disso, a reutilização para este adsorvente híbrido orgânico-inorgânico reticulado foi estudada por ciclos de usoregeneração, sem perda significativa em sua atividade inicial.Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPESapplication/pdfporUniversidade Federal de AlfenasPrograma de Pós-Graduação em QuímicaUNIFAL-MGBrasilInstituto de Químicainfo:eu-repo/semantics/openAccesshttp://creativecommons.org/licenses/by-nc-nd/4.0/DimetilpolisiloxanosMetacrilatosAdsorçãoPolimerizaçãoQUIMICA::QUIMICA INORGANICASíntese e caracterização de redes poliméricas a base de poli(dimetilsiloxano) e metacrilato de 2-(dimetilamino)etila para adsorção de íons cobre(II) de soluções aquosasinfo:eu-repo/semantics/doctoralThesisinfo:eu-repo/semantics/publishedVersion132825307882678230660060060031391270652389310962075167498588264571reponame:Repositório Institucional da Universidade Federal de Alfenas - RiUnifalinstname:Universidade Federal de Alfenas (UNIFAL)instacron:UNIFALSilva, Fábio Antônio BelinelliLICENSElicense.txtlicense.txttext/plain; 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| dc.title.pt-BR.fl_str_mv |
Síntese e caracterização de redes poliméricas a base de poli(dimetilsiloxano) e metacrilato de 2-(dimetilamino)etila para adsorção de íons cobre(II) de soluções aquosas |
| title |
Síntese e caracterização de redes poliméricas a base de poli(dimetilsiloxano) e metacrilato de 2-(dimetilamino)etila para adsorção de íons cobre(II) de soluções aquosas |
| spellingShingle |
Síntese e caracterização de redes poliméricas a base de poli(dimetilsiloxano) e metacrilato de 2-(dimetilamino)etila para adsorção de íons cobre(II) de soluções aquosas Silva, Fábio Antônio Belinelli Dimetilpolisiloxanos Metacrilatos Adsorção Polimerização QUIMICA::QUIMICA INORGANICA |
| title_short |
Síntese e caracterização de redes poliméricas a base de poli(dimetilsiloxano) e metacrilato de 2-(dimetilamino)etila para adsorção de íons cobre(II) de soluções aquosas |
| title_full |
Síntese e caracterização de redes poliméricas a base de poli(dimetilsiloxano) e metacrilato de 2-(dimetilamino)etila para adsorção de íons cobre(II) de soluções aquosas |
| title_fullStr |
Síntese e caracterização de redes poliméricas a base de poli(dimetilsiloxano) e metacrilato de 2-(dimetilamino)etila para adsorção de íons cobre(II) de soluções aquosas |
| title_full_unstemmed |
Síntese e caracterização de redes poliméricas a base de poli(dimetilsiloxano) e metacrilato de 2-(dimetilamino)etila para adsorção de íons cobre(II) de soluções aquosas |
| title_sort |
Síntese e caracterização de redes poliméricas a base de poli(dimetilsiloxano) e metacrilato de 2-(dimetilamino)etila para adsorção de íons cobre(II) de soluções aquosas |
| author |
Silva, Fábio Antônio Belinelli |
| author_facet |
Silva, Fábio Antônio Belinelli |
| author_role |
author |
| dc.contributor.author.fl_str_mv |
Silva, Fábio Antônio Belinelli |
| dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/4560803280050919 |
| dc.contributor.referee1.fl_str_mv |
Molina, Eduardo Ferreira |
| dc.contributor.referee2.fl_str_mv |
Almeida, Eduardo Tonon De |
| dc.contributor.referee3.fl_str_mv |
Schiavon, Marco Antônio |
| dc.contributor.referee4.fl_str_mv |
Luccas, Pedro Orival |
| dc.contributor.advisor1.fl_str_mv |
Pissetti, Fábio Luiz |
| dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/5920841060592650 |
| contributor_str_mv |
Molina, Eduardo Ferreira Almeida, Eduardo Tonon De Schiavon, Marco Antônio Luccas, Pedro Orival Pissetti, Fábio Luiz |
| dc.subject.por.fl_str_mv |
Dimetilpolisiloxanos Metacrilatos Adsorção Polimerização |
| topic |
Dimetilpolisiloxanos Metacrilatos Adsorção Polimerização QUIMICA::QUIMICA INORGANICA |
| dc.subject.cnpq.fl_str_mv |
QUIMICA::QUIMICA INORGANICA |
| description |
Two novel organic-inorganic hybrid adsorbents based on poly(dimethylsiloxane) (PDMS) and 2-(dimethylamino)ethyl methacrylate (DMAEMA) were prepared and applied for the removal of copper(II) ions in aqueous media. The materials were characterized by Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), swelling measurements and nuclear magnetic resonance (NMR). Semi-interpenetrating polymer networks (semi-IPNs) were prepared with 1:0.5 weight ratio for PDMS:PDMAEMA in 1:0.4 and 1:1 molar ratios of PDMS and the crosslinker agent (3-chloropropyl)trimethoxysilane (CPTMS), respectively. Only the network with the highest amount of CPTMS was stable in water. This semi-IPN was able to adsorb about 34 % in mass of water, indicating that was obtained a material with higher hydrophilic character. The adsorption experiments results of copper(II) ions at room temperature reveal a high pH-dependence, reaching uptake capacity of 0.40 mmol g-¹ at pH 5 within 36 h. The adsorbent-adsorbate system was described by the pseudo-first order kinetic model and Sips adsorption model. Furthermore, reuse experiments suggested that PDMS/PDMAEMA semi-IPN could be a potential recyclable adsorbent in the treatment of aqueous systems. The second hybrid adsorbent was prepared by the polycondensation of poly(dimethylsiloxane) containing silanol terminals groups and methoxy groups of a previous prepared copolymer, the poly[vinyltrimethoxysilane-co-2-(dimethylamino)ethyl methacrylate]. This adsorbent reached the swelling equilibrium at 23 % in mass of water, after approximately 18 days. The saturation of the active sites of the material was observed at pH 5, after 3 days, with each gram of material capable of adsorbing 0.48 mmol of copper(II) ions. The fractionaryorder and Sips model provided the best fit to the experimental data in kinetic and equilibrium studies of the adsorption process, respectively. Moreover, the reusability for this cross-linked organic–inorganic hybrid adsorbent was studied through usage-regeneration cycles without significant loss in its initial activity. |
| publishDate |
2016 |
| dc.date.issued.fl_str_mv |
2016-04-01 |
| dc.date.accessioned.fl_str_mv |
2017-06-13T17:59:29Z |
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info:eu-repo/semantics/doctoralThesis |
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info:eu-repo/semantics/publishedVersion |
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doctoralThesis |
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publishedVersion |
| dc.identifier.citation.fl_str_mv |
SILVA, Fábio Antônio Belinelli. Síntese e caracterização de redes poliméricas a base de poli(dimetilsiloxano) e metacrilato de 2-(dimetilamino)etila para adsorção de íons cobre(II) de soluções aquosas. 2016. 81 f. Tese (Doutorado em Química) - Universidade Federal de Alfenas, Alfenas, MG, 2016. |
| dc.identifier.uri.fl_str_mv |
https://repositorio.unifal-mg.edu.br/handle/123456789/981 |
| identifier_str_mv |
SILVA, Fábio Antônio Belinelli. Síntese e caracterização de redes poliméricas a base de poli(dimetilsiloxano) e metacrilato de 2-(dimetilamino)etila para adsorção de íons cobre(II) de soluções aquosas. 2016. 81 f. Tese (Doutorado em Química) - Universidade Federal de Alfenas, Alfenas, MG, 2016. |
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https://repositorio.unifal-mg.edu.br/handle/123456789/981 |
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por |
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por |
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1328253078826782306 |
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600 600 600 |
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3139127065238931096 |
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2075167498588264571 |
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info:eu-repo/semantics/openAccess http://creativecommons.org/licenses/by-nc-nd/4.0/ |
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openAccess |
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http://creativecommons.org/licenses/by-nc-nd/4.0/ |
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application/pdf |
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Universidade Federal de Alfenas |
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Programa de Pós-Graduação em Química |
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UNIFAL-MG |
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Brasil |
| dc.publisher.department.fl_str_mv |
Instituto de Química |
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Universidade Federal de Alfenas |
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Repositório Institucional da Universidade Federal de Alfenas - RiUnifal |
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https://repositorio.unifal-mg.edu.br/bitstreams/a7794846-0018-49a5-8f32-210ef1606be1/download https://repositorio.unifal-mg.edu.br/bitstreams/5ba0ea9a-8e1a-42b3-b75c-d6ca4c98c090/download https://repositorio.unifal-mg.edu.br/bitstreams/c9db419e-4d40-49e4-a3e2-bd8a5215d653/download https://repositorio.unifal-mg.edu.br/bitstreams/14e4314f-0893-48c7-be06-63b28d8bd107/download https://repositorio.unifal-mg.edu.br/bitstreams/a27dde18-c10d-4559-9799-d0e8d1f88dba/download https://repositorio.unifal-mg.edu.br/bitstreams/cec2551c-cbf3-4b14-957b-94f5e30ae2d2/download https://repositorio.unifal-mg.edu.br/bitstreams/4125e52f-0bfc-4198-930b-d59fe2e81945/download |
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| bitstream.checksumAlgorithm.fl_str_mv |
MD5 MD5 MD5 MD5 MD5 MD5 MD5 |
| repository.name.fl_str_mv |
Repositório Institucional da Universidade Federal de Alfenas - RiUnifal - Universidade Federal de Alfenas (UNIFAL) |
| repository.mail.fl_str_mv |
repositorio@unifal-mg.edu.br |
| _version_ |
1859830900911505408 |