Síntese e caracterização de Poli(L-co-DL ácido lático-co-policaprolactona)uretana.
Ano de defesa: | 2018 |
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Autor(a) principal: | |
Orientador(a): | |
Banca de defesa: | |
Tipo de documento: | Dissertação |
Tipo de acesso: | Acesso aberto |
Idioma: | por |
Instituição de defesa: |
Universidade Federal de São Carlos
Câmpus Sorocaba |
Programa de Pós-Graduação: |
Programa de Pós-Graduação em Ciência dos Materiais - PPGCM-So
|
Departamento: |
Não Informado pela instituição
|
País: |
Não Informado pela instituição
|
Palavras-chave em Português: | |
Palavras-chave em Inglês: | |
Área do conhecimento CNPq: | |
Link de acesso: | https://repositorio.ufscar.br/handle/ufscar/10193 |
Resumo: | Polyurethanes are applied for many purposes. This wide use is due to the versatility of these polymers, consisting of flexible and rigid segments, whose combination determines their characteristics. Therefore, the main objective of this work was to synthesize a biocompatible and biosorbable polyurethane, with an adequates properties to be used as a scaffold in meniscus regeneration. Prepolymer was obtained by bulk polymerization of L-lactide, D,L-lactide, polycaprolactone diol monomers. The initiator used was Tin II 2-ethylhexanoate. Materials was added to a flask under N2 atmosphere and immersed in an oil bath at 150 ºC, with stirring during 24 hours. Polyurethanes were obtained by solution polymerization of the prepolymer to a previous stage with 1,6-hexamethylene diisocyanate at a molar ratio of 1:8. Two polyurethanes were formed, using 2,1x10-4 mol of prepolymer and another one using 4,2x10-4 mol of prepolymer. The polyurethane synthesis was prepared on a flask under N2 atmosphere and immersed in oil at 70ºC with stirring during 6 hours. The average molecular weight of prepolymer was 104 g/mol obtained by GPC. Prepolymer and polyurethane were analyzed by FTIR and 1H NMR where results showed the presence of polycaprolactone, L and D,L-lactic acid and urethane groups in the polyurethane. Glass transition temperature, crystallization temperature and melt temperature were obtained by DSC analysis. The amount of prepolymer used in the polyurethane synthesis generated a difference on temperatures obtained by DSC analysis. The crystallinity of the polyurethanes were also verified by XRD. In the DMA analysis was observed that the polyurethane films melting around 60°C. It was observed also at DSC analysis. The DMA results corroborated with those of the XRD for the difference in crystallinity between the polyurethane films, the PU-C is more crystalline than the others. The TG and DTG analysis of polyurethanes demonstrated the presence of three stages of weight loss, with the Tonset changing with crystallinity value. The cell viability assay, based on the cytotoxicity of the polyurethanes, has shown that it is possible to proliferate cells in polyurethane synthetized. Therefore due to the characteristics presented by this polyurethane it could be applied as polymeric biomaterial in the field of tissue engineering. |
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Brandolise, Carolini SilvaDuek, Eliana Aparecida de Rezendehttp://lattes.cnpq.br/4147198882685212Komatsu, Danielhttp://lattes.cnpq.br/2620060426867863http://lattes.cnpq.br/00663067557583922018-06-19T17:14:21Z2018-06-19T17:14:21Z2018-03-27BRANDOLISE, Carolini Silva. Síntese e caracterização de Poli(L-co-DL ácido lático-co-policaprolactona)uretana.. 2018. Dissertação (Mestrado em Ciência dos Materiais) – Universidade Federal de São Carlos, Sorocaba, 2018. Disponível em: https://repositorio.ufscar.br/handle/ufscar/10193.https://repositorio.ufscar.br/handle/ufscar/10193Polyurethanes are applied for many purposes. This wide use is due to the versatility of these polymers, consisting of flexible and rigid segments, whose combination determines their characteristics. Therefore, the main objective of this work was to synthesize a biocompatible and biosorbable polyurethane, with an adequates properties to be used as a scaffold in meniscus regeneration. Prepolymer was obtained by bulk polymerization of L-lactide, D,L-lactide, polycaprolactone diol monomers. The initiator used was Tin II 2-ethylhexanoate. Materials was added to a flask under N2 atmosphere and immersed in an oil bath at 150 ºC, with stirring during 24 hours. Polyurethanes were obtained by solution polymerization of the prepolymer to a previous stage with 1,6-hexamethylene diisocyanate at a molar ratio of 1:8. Two polyurethanes were formed, using 2,1x10-4 mol of prepolymer and another one using 4,2x10-4 mol of prepolymer. The polyurethane synthesis was prepared on a flask under N2 atmosphere and immersed in oil at 70ºC with stirring during 6 hours. The average molecular weight of prepolymer was 104 g/mol obtained by GPC. Prepolymer and polyurethane were analyzed by FTIR and 1H NMR where results showed the presence of polycaprolactone, L and D,L-lactic acid and urethane groups in the polyurethane. Glass transition temperature, crystallization temperature and melt temperature were obtained by DSC analysis. The amount of prepolymer used in the polyurethane synthesis generated a difference on temperatures obtained by DSC analysis. The crystallinity of the polyurethanes were also verified by XRD. In the DMA analysis was observed that the polyurethane films melting around 60°C. It was observed also at DSC analysis. The DMA results corroborated with those of the XRD for the difference in crystallinity between the polyurethane films, the PU-C is more crystalline than the others. The TG and DTG analysis of polyurethanes demonstrated the presence of three stages of weight loss, with the Tonset changing with crystallinity value. The cell viability assay, based on the cytotoxicity of the polyurethanes, has shown that it is possible to proliferate cells in polyurethane synthetized. Therefore due to the characteristics presented by this polyurethane it could be applied as polymeric biomaterial in the field of tissue engineering.As poliuretanas são aplicadas em diversos fins. Esta ampla utilização se dá pela versatilidade destes polímeros, constituído de segmentos flexíveis e rígidos, cuja combinação determina as propriedades características dos materiais em diversas aplicações. O objetivo deste trabalho é sintetizar uma poliuretana biocompatível e bioreabsorvível, com características adequadas para ser aplicada futuramente como arcabouço na regeneração tecidual de menisco. A poliuretana foi obtida através de dois estágios de sínteses, o primeiro para a produção do pré-polímero e o segundo para a produção da poliuretana. O pré-polímero foi obtido por polimerização em massa dos monômeros L-lactídeo, DL-lactídeo e policaprolactona-diol a 150°C por 24 horas. Por sua vez, as poliuretanas foram obtidas por polimerização em solução do pré-polímero, do estágio anterior, com o 1,6-hexametileno diisocianato, em uma relação molar 1:8. As sínteses ocorreram a 70°C por 6 horas. Duas delas foram a partir de 2,1x10-4 mol do pré-polímero e outra com 4,2x10-4 mol. O pré-polímero apresentou massa molar numérica média da ordem de 104 Da, obtida por GPC. O pré-polímero e as poliuretanas foram submetidos a caracterizações FTIR e RMN 1H. Os resultados por FTIR mostraram a presença dos grupos principais da policaprolactona e do L e DL ácido lático, confirmados pelo RMN 1H. Da mesma forma para a poliuretana, os resultados do FTIR mostraram a formação do grupo uretana, confirmado pelo RMN 1H. Por meio da DSC dos pré-polímeros e das poliuretanas foi possível obter os valores de temperatura de transição vítrea, de cristalização e de fusão. Notando diferenças entre as poliuretanas quanto a apresentação desses eventos, devido à quantidade de mol utilizada na síntese. As cristalinidades das poliuretanas foram verificadas também por DRX, relacionando esta técnica com o ensaio de DSC, a fim de verificar qual poliuretana possui maior cristalinidade. Ao realizar o ensaio de DMA observou-se que os filmes das poliuretanas amoleceram ao atingir temperaturas por volta de 60°C, relacionando aos eventos observados no DSC. Os resultados do ensaio de DMA corroboram com os do DRX quanto à diferença de cristalinidade entre os filmes de poliuretana, demonstrando que a PU-C possui maior cristalinidade que as demais. As curvas de TG e as de DTG das poliuretanas demonstraram a presença de três estágios de perda de massa, com o Tonset diferindo-se entre as poliuretanas, conforme há o aumento de cristalinidade. O ensaio de viabilidade celular, com base na citotoxidade das poliuretanas, demonstrou que é possível proliferar células sobre as mesmas. Em função das características apresentadas pelo material desenvolvido, é possível uma futura aplicação do mesmo como biomaterial polimérico no campo da engenharia tecidual.Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)porUniversidade Federal de São CarlosCâmpus SorocabaPrograma de Pós-Graduação em Ciência dos Materiais - PPGCM-SoUFSCarPoliuretanaL-lactídeoDL-lactídeoPolicaprolactona-diolBiomateriaisL-lactideDL-lactideMateriais biomédicosPolyurethanePolycaprolactone-diolBiomaterialsBiomedical materialsENGENHARIAS::ENGENHARIA BIOMEDICA::ENGENHARIA MEDICA::BIOMATERIAIS E MATERIAIS BIOCOMPATIVEISENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICA::MATERIAIS NAO METALICOS::POLIMEROS, APLICACOESSíntese e caracterização de Poli(L-co-DL ácido lático-co-policaprolactona)uretana.Synthesis and characterization of Poly(L-co-DL lactic acid-co-polycaprolactone)urethane.info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisOnlineinfo:eu-repo/semantics/openAccessreponame:Repositório Institucional da UFSCARinstname:Universidade Federal de São Carlos (UFSCAR)instacron:UFSCARORIGINALDISSERTAÇÃO_Carolini Silva Brandolise.pdfDISSERTAÇÃO_Carolini Silva Brandolise.pdfapplication/pdf3018462https://{{ getenv "DSPACE_HOST" "repositorio.ufscar.br" }}/bitstream/ufscar/10193/1/DISSERTA%c3%87%c3%83O_Carolini%20Silva%20Brandolise.pdff39ba46b05966a6cc1a1d6ab897a1fc3MD51Carta assinada.pdfCarta assinada.pdfapplication/pdf206751https://{{ getenv "DSPACE_HOST" "repositorio.ufscar.br" }}/bitstream/ufscar/10193/3/Carta%20assinada.pdf8d369763b37c9d361c3d2dc1518ccbb8MD53LICENSElicense.txtlicense.txttext/plain; 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dc.title.por.fl_str_mv |
Síntese e caracterização de Poli(L-co-DL ácido lático-co-policaprolactona)uretana. |
dc.title.alternative.eng.fl_str_mv |
Synthesis and characterization of Poly(L-co-DL lactic acid-co-polycaprolactone)urethane. |
title |
Síntese e caracterização de Poli(L-co-DL ácido lático-co-policaprolactona)uretana. |
spellingShingle |
Síntese e caracterização de Poli(L-co-DL ácido lático-co-policaprolactona)uretana. Brandolise, Carolini Silva Poliuretana L-lactídeo DL-lactídeo Policaprolactona-diol Biomateriais L-lactide DL-lactide Materiais biomédicos Polyurethane Polycaprolactone-diol Biomaterials Biomedical materials ENGENHARIAS::ENGENHARIA BIOMEDICA::ENGENHARIA MEDICA::BIOMATERIAIS E MATERIAIS BIOCOMPATIVEIS ENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICA::MATERIAIS NAO METALICOS::POLIMEROS, APLICACOES |
title_short |
Síntese e caracterização de Poli(L-co-DL ácido lático-co-policaprolactona)uretana. |
title_full |
Síntese e caracterização de Poli(L-co-DL ácido lático-co-policaprolactona)uretana. |
title_fullStr |
Síntese e caracterização de Poli(L-co-DL ácido lático-co-policaprolactona)uretana. |
title_full_unstemmed |
Síntese e caracterização de Poli(L-co-DL ácido lático-co-policaprolactona)uretana. |
title_sort |
Síntese e caracterização de Poli(L-co-DL ácido lático-co-policaprolactona)uretana. |
author |
Brandolise, Carolini Silva |
author_facet |
Brandolise, Carolini Silva |
author_role |
author |
dc.contributor.authorlattes.por.fl_str_mv |
http://lattes.cnpq.br/0066306755758392 |
dc.contributor.author.fl_str_mv |
Brandolise, Carolini Silva |
dc.contributor.advisor1.fl_str_mv |
Duek, Eliana Aparecida de Rezende |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/4147198882685212 |
dc.contributor.advisor-co1.fl_str_mv |
Komatsu, Daniel |
dc.contributor.advisor-co1Lattes.fl_str_mv |
http://lattes.cnpq.br/2620060426867863 |
contributor_str_mv |
Duek, Eliana Aparecida de Rezende Komatsu, Daniel |
dc.subject.por.fl_str_mv |
Poliuretana L-lactídeo DL-lactídeo Policaprolactona-diol Biomateriais L-lactide DL-lactide Materiais biomédicos |
topic |
Poliuretana L-lactídeo DL-lactídeo Policaprolactona-diol Biomateriais L-lactide DL-lactide Materiais biomédicos Polyurethane Polycaprolactone-diol Biomaterials Biomedical materials ENGENHARIAS::ENGENHARIA BIOMEDICA::ENGENHARIA MEDICA::BIOMATERIAIS E MATERIAIS BIOCOMPATIVEIS ENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICA::MATERIAIS NAO METALICOS::POLIMEROS, APLICACOES |
dc.subject.eng.fl_str_mv |
Polyurethane Polycaprolactone-diol Biomaterials Biomedical materials |
dc.subject.cnpq.fl_str_mv |
ENGENHARIAS::ENGENHARIA BIOMEDICA::ENGENHARIA MEDICA::BIOMATERIAIS E MATERIAIS BIOCOMPATIVEIS ENGENHARIAS::ENGENHARIA DE MATERIAIS E METALURGICA::MATERIAIS NAO METALICOS::POLIMEROS, APLICACOES |
description |
Polyurethanes are applied for many purposes. This wide use is due to the versatility of these polymers, consisting of flexible and rigid segments, whose combination determines their characteristics. Therefore, the main objective of this work was to synthesize a biocompatible and biosorbable polyurethane, with an adequates properties to be used as a scaffold in meniscus regeneration. Prepolymer was obtained by bulk polymerization of L-lactide, D,L-lactide, polycaprolactone diol monomers. The initiator used was Tin II 2-ethylhexanoate. Materials was added to a flask under N2 atmosphere and immersed in an oil bath at 150 ºC, with stirring during 24 hours. Polyurethanes were obtained by solution polymerization of the prepolymer to a previous stage with 1,6-hexamethylene diisocyanate at a molar ratio of 1:8. Two polyurethanes were formed, using 2,1x10-4 mol of prepolymer and another one using 4,2x10-4 mol of prepolymer. The polyurethane synthesis was prepared on a flask under N2 atmosphere and immersed in oil at 70ºC with stirring during 6 hours. The average molecular weight of prepolymer was 104 g/mol obtained by GPC. Prepolymer and polyurethane were analyzed by FTIR and 1H NMR where results showed the presence of polycaprolactone, L and D,L-lactic acid and urethane groups in the polyurethane. Glass transition temperature, crystallization temperature and melt temperature were obtained by DSC analysis. The amount of prepolymer used in the polyurethane synthesis generated a difference on temperatures obtained by DSC analysis. The crystallinity of the polyurethanes were also verified by XRD. In the DMA analysis was observed that the polyurethane films melting around 60°C. It was observed also at DSC analysis. The DMA results corroborated with those of the XRD for the difference in crystallinity between the polyurethane films, the PU-C is more crystalline than the others. The TG and DTG analysis of polyurethanes demonstrated the presence of three stages of weight loss, with the Tonset changing with crystallinity value. The cell viability assay, based on the cytotoxicity of the polyurethanes, has shown that it is possible to proliferate cells in polyurethane synthetized. Therefore due to the characteristics presented by this polyurethane it could be applied as polymeric biomaterial in the field of tissue engineering. |
publishDate |
2018 |
dc.date.accessioned.fl_str_mv |
2018-06-19T17:14:21Z |
dc.date.available.fl_str_mv |
2018-06-19T17:14:21Z |
dc.date.issued.fl_str_mv |
2018-03-27 |
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.citation.fl_str_mv |
BRANDOLISE, Carolini Silva. Síntese e caracterização de Poli(L-co-DL ácido lático-co-policaprolactona)uretana.. 2018. Dissertação (Mestrado em Ciência dos Materiais) – Universidade Federal de São Carlos, Sorocaba, 2018. Disponível em: https://repositorio.ufscar.br/handle/ufscar/10193. |
dc.identifier.uri.fl_str_mv |
https://repositorio.ufscar.br/handle/ufscar/10193 |
identifier_str_mv |
BRANDOLISE, Carolini Silva. Síntese e caracterização de Poli(L-co-DL ácido lático-co-policaprolactona)uretana.. 2018. Dissertação (Mestrado em Ciência dos Materiais) – Universidade Federal de São Carlos, Sorocaba, 2018. Disponível em: https://repositorio.ufscar.br/handle/ufscar/10193. |
url |
https://repositorio.ufscar.br/handle/ufscar/10193 |
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 São Carlos Câmpus Sorocaba |
dc.publisher.program.fl_str_mv |
Programa de Pós-Graduação em Ciência dos Materiais - PPGCM-So |
dc.publisher.initials.fl_str_mv |
UFSCar |
publisher.none.fl_str_mv |
Universidade Federal de São Carlos Câmpus Sorocaba |
dc.source.none.fl_str_mv |
reponame:Repositório Institucional da UFSCAR instname:Universidade Federal de São Carlos (UFSCAR) instacron:UFSCAR |
instname_str |
Universidade Federal de São Carlos (UFSCAR) |
instacron_str |
UFSCAR |
institution |
UFSCAR |
reponame_str |
Repositório Institucional da UFSCAR |
collection |
Repositório Institucional da UFSCAR |
bitstream.url.fl_str_mv |
https://{{ getenv "DSPACE_HOST" "repositorio.ufscar.br" }}/bitstream/ufscar/10193/1/DISSERTA%c3%87%c3%83O_Carolini%20Silva%20Brandolise.pdf https://{{ getenv "DSPACE_HOST" "repositorio.ufscar.br" }}/bitstream/ufscar/10193/3/Carta%20assinada.pdf https://{{ getenv "DSPACE_HOST" "repositorio.ufscar.br" }}/bitstream/ufscar/10193/4/license.txt https://{{ getenv "DSPACE_HOST" "repositorio.ufscar.br" }}/bitstream/ufscar/10193/5/DISSERTA%c3%87%c3%83O_Carolini%20Silva%20Brandolise.pdf.txt https://{{ getenv "DSPACE_HOST" "repositorio.ufscar.br" }}/bitstream/ufscar/10193/6/Carta%20assinada.pdf.txt https://{{ getenv "DSPACE_HOST" "repositorio.ufscar.br" }}/bitstream/ufscar/10193/7/DISSERTA%c3%87%c3%83O_Carolini%20Silva%20Brandolise.pdf.jpg https://{{ getenv "DSPACE_HOST" "repositorio.ufscar.br" }}/bitstream/ufscar/10193/8/Carta%20assinada.pdf.jpg |
bitstream.checksum.fl_str_mv |
f39ba46b05966a6cc1a1d6ab897a1fc3 8d369763b37c9d361c3d2dc1518ccbb8 ae0398b6f8b235e40ad82cba6c50031d 06f0ecc4c7f91cf17c168bc751e547f7 68b329da9893e34099c7d8ad5cb9c940 0cfa997043573fbacbb15e1af49f1d38 1c3833c984cc93f006193a02b51279bb |
bitstream.checksumAlgorithm.fl_str_mv |
MD5 MD5 MD5 MD5 MD5 MD5 MD5 |
repository.name.fl_str_mv |
Repositório Institucional da UFSCAR - Universidade Federal de São Carlos (UFSCAR) |
repository.mail.fl_str_mv |
|
_version_ |
1767351136429277184 |