Thermoplastic starch nanocomposites reinforced with nanofibrillated cellulose: a study on processing and plasticization in the presence of water as a process plasticizer

Bibliographic Details
Main Author: Lipa, Annette Daphne Cochon
Publication Date: 2024
Format: Master thesis
Language: eng
Source: Biblioteca Digital de Teses e Dissertações da USP
Download full: https://www.teses.usp.br/teses/disponiveis/18/18158/tde-10022025-160621/
Summary: The effect of water on TPS preparation and properties is extremely relevant due to its hole as process plasticizer and desestruturation agent. Here we describe the investigation of the effect of residual water from nanofibrillated cellulose suspensions in the properties of cellulose/thermoplastic starch (TPS) composites. It was used corn starch, cellulose nanofibrils from eucalyptus and glycerol as plasticizer. The nanofibrillated cellulose used from its suspensions containing up to 4% solids was introduced directly to starch and glycerol and dried to residual water content of 15-25%. Excess water was removed prior to extrusion in an air circulation oven and processed with added glycerol (70 and 80% based on the dry weight of starch and glycerol) as the primary plasticizer and residual water acting as the processing plasticizer. The NFC content was 2.5, 5, 7.5, and 10% based on the dry weight of starchglycerol/NFC system. The results showed that all the formulations developed exhibited a significant reduction in moisture absorption as the NFC content increased. This effect was particularly pronounced in the formulation containing 20% glycerol and 10% NFC. Optical microscopy revealed a complete destructuring of the starch, evidenced by the absence of residual granules, a result that was further confirmed by scanning electron microscopy (SEM). The SEM analysis also demonstrated a remarkably homogeneous dispersion of the NFC within the matrix, with minimal agglomeration observed. The nanocomposites showed significant mechanical improvements across all formulations. At higher NFC concentrations, a transition from a ductile to a more brittle state was observed, with tensile strength doubling compared to formulations with lower NFC content, highlighting NFC\'s reinforcing capability despite reduced ductility. The developed material outperformed TPS without added water, exhibiting a lighter color and reduced thermal and chemical degradation. These findings confirm the effectiveness of the methodology and the essential role of residual water in material plasticization and structuring.
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spelling Thermoplastic starch nanocomposites reinforced with nanofibrillated cellulose: a study on processing and plasticization in the presence of water as a process plasticizerNanocompósitos de amido termoplástico reforçados com nanofibrilas de celulose: um estudo sobre o processamento e a plastificação na presença de água como plastificante de processoágua residualamido termoplásticocelulose nanofibriladaextrusãoextrusionnanofibrillated celuloseresidual waterthermoplastic starchThe effect of water on TPS preparation and properties is extremely relevant due to its hole as process plasticizer and desestruturation agent. Here we describe the investigation of the effect of residual water from nanofibrillated cellulose suspensions in the properties of cellulose/thermoplastic starch (TPS) composites. It was used corn starch, cellulose nanofibrils from eucalyptus and glycerol as plasticizer. The nanofibrillated cellulose used from its suspensions containing up to 4% solids was introduced directly to starch and glycerol and dried to residual water content of 15-25%. Excess water was removed prior to extrusion in an air circulation oven and processed with added glycerol (70 and 80% based on the dry weight of starch and glycerol) as the primary plasticizer and residual water acting as the processing plasticizer. The NFC content was 2.5, 5, 7.5, and 10% based on the dry weight of starchglycerol/NFC system. The results showed that all the formulations developed exhibited a significant reduction in moisture absorption as the NFC content increased. This effect was particularly pronounced in the formulation containing 20% glycerol and 10% NFC. Optical microscopy revealed a complete destructuring of the starch, evidenced by the absence of residual granules, a result that was further confirmed by scanning electron microscopy (SEM). The SEM analysis also demonstrated a remarkably homogeneous dispersion of the NFC within the matrix, with minimal agglomeration observed. The nanocomposites showed significant mechanical improvements across all formulations. At higher NFC concentrations, a transition from a ductile to a more brittle state was observed, with tensile strength doubling compared to formulations with lower NFC content, highlighting NFC\'s reinforcing capability despite reduced ductility. The developed material outperformed TPS without added water, exhibiting a lighter color and reduced thermal and chemical degradation. These findings confirm the effectiveness of the methodology and the essential role of residual water in material plasticization and structuring.O efeito da água na preparação e nas propriedades do amido termoplástico (TPS) foi altamente relevante devido ao seu papel como plastificante de processo e agente de desestruturação. Este estudo focou na análise do impacto da água residual presente em suspensões de celulose nanofibrilada (NFC) nas propriedades dos nanocompósitos de TPS/NFC. Foram utilizados amido de milho, celulose nanofibrilada obtida de eucalipto e glicerol como plastificante principal. A celulose nanofibrilada proveniente de suspensões contendo até 4% de sólidos foi diretamente incorporada à mistura de amido e glicerol. As misturas foram então secas para atingir um teor de água residual entre 15% e 25%. O excesso de água foi removido antes da extrusão utilizando um forno com circulação de ar forçado. As formulações incluíram glicerol adicional em 70% e 80% do peso seco com base no conteúdo total de amido e glicerol, que atuou como plastificante principal, enquanto a água residual serviu como plastificante de processo. Diferentes concentrações de NFC (2,5%, 5,0%, 7,5% e 10%) foram preparadas com base no peso seco do sistema amido-glicerol/NFC. Os resultados mostraram que todas as formulações desenvolvidas apresentaram uma redução significativa na absorção de umidade à medida que o teor de NFC aumentava. Esse efeito foi particularmente evidente na formulação contendo 20% de glicerol e 10% de NFC. A microscopia óptica revelou uma desestruturação completa do amido, evidenciada pela ausência de grânulos residuais, resultado que foi ainda confirmado por microscopia eletrônica de varredura (MEV). A análise por MEV também demonstrou uma dispersão notavelmente homogênea da NFC na matriz, com mínima aglomeração observada. Os nanocompósitos apresentaram melhorias mecânicas significativas em todas as formulações. Na maior concentração de NFC, houve transição de um estado dúctil para mais frágil, com o dobro de resistência à tração em relação a formulações com menos NFC, destacando o reforço da NFC, apesar da redução na ductilidade. O material desenvolvido superou o desempenho do TPS sem adição de água, apresentando coloração mais clara e menor degradação térmica e química. Esses resultados confirmam a eficácia da metodologia e o papel essencial da água residual na plastificação e estruturação do material.Biblioteca Digitais de Teses e Dissertações da USPCarvalho, Antonio José Felix deLipa, Annette Daphne Cochon2024-12-12info:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/masterThesisapplication/pdfhttps://www.teses.usp.br/teses/disponiveis/18/18158/tde-10022025-160621/reponame:Biblioteca Digital de Teses e Dissertações da USPinstname:Universidade de São Paulo (USP)instacron:USPLiberar o conteúdo para acesso público.info:eu-repo/semantics/openAccesseng2025-02-11T19:43:02Zoai:teses.usp.br:tde-10022025-160621Biblioteca Digital de Teses e Dissertaçõeshttp://www.teses.usp.br/PUBhttp://www.teses.usp.br/cgi-bin/mtd2br.plvirginia@if.usp.br|| atendimento@aguia.usp.br||virginia@if.usp.bropendoar:27212025-02-11T19:43:02Biblioteca Digital de Teses e Dissertações da USP - Universidade de São Paulo (USP)false
dc.title.none.fl_str_mv Thermoplastic starch nanocomposites reinforced with nanofibrillated cellulose: a study on processing and plasticization in the presence of water as a process plasticizer
Nanocompósitos de amido termoplástico reforçados com nanofibrilas de celulose: um estudo sobre o processamento e a plastificação na presença de água como plastificante de processo
title Thermoplastic starch nanocomposites reinforced with nanofibrillated cellulose: a study on processing and plasticization in the presence of water as a process plasticizer
spellingShingle Thermoplastic starch nanocomposites reinforced with nanofibrillated cellulose: a study on processing and plasticization in the presence of water as a process plasticizer
Lipa, Annette Daphne Cochon
água residual
amido termoplástico
celulose nanofibrilada
extrusão
extrusion
nanofibrillated celulose
residual water
thermoplastic starch
title_short Thermoplastic starch nanocomposites reinforced with nanofibrillated cellulose: a study on processing and plasticization in the presence of water as a process plasticizer
title_full Thermoplastic starch nanocomposites reinforced with nanofibrillated cellulose: a study on processing and plasticization in the presence of water as a process plasticizer
title_fullStr Thermoplastic starch nanocomposites reinforced with nanofibrillated cellulose: a study on processing and plasticization in the presence of water as a process plasticizer
title_full_unstemmed Thermoplastic starch nanocomposites reinforced with nanofibrillated cellulose: a study on processing and plasticization in the presence of water as a process plasticizer
title_sort Thermoplastic starch nanocomposites reinforced with nanofibrillated cellulose: a study on processing and plasticization in the presence of water as a process plasticizer
author Lipa, Annette Daphne Cochon
author_facet Lipa, Annette Daphne Cochon
author_role author
dc.contributor.none.fl_str_mv Carvalho, Antonio José Felix de
dc.contributor.author.fl_str_mv Lipa, Annette Daphne Cochon
dc.subject.por.fl_str_mv água residual
amido termoplástico
celulose nanofibrilada
extrusão
extrusion
nanofibrillated celulose
residual water
thermoplastic starch
topic água residual
amido termoplástico
celulose nanofibrilada
extrusão
extrusion
nanofibrillated celulose
residual water
thermoplastic starch
description The effect of water on TPS preparation and properties is extremely relevant due to its hole as process plasticizer and desestruturation agent. Here we describe the investigation of the effect of residual water from nanofibrillated cellulose suspensions in the properties of cellulose/thermoplastic starch (TPS) composites. It was used corn starch, cellulose nanofibrils from eucalyptus and glycerol as plasticizer. The nanofibrillated cellulose used from its suspensions containing up to 4% solids was introduced directly to starch and glycerol and dried to residual water content of 15-25%. Excess water was removed prior to extrusion in an air circulation oven and processed with added glycerol (70 and 80% based on the dry weight of starch and glycerol) as the primary plasticizer and residual water acting as the processing plasticizer. The NFC content was 2.5, 5, 7.5, and 10% based on the dry weight of starchglycerol/NFC system. The results showed that all the formulations developed exhibited a significant reduction in moisture absorption as the NFC content increased. This effect was particularly pronounced in the formulation containing 20% glycerol and 10% NFC. Optical microscopy revealed a complete destructuring of the starch, evidenced by the absence of residual granules, a result that was further confirmed by scanning electron microscopy (SEM). The SEM analysis also demonstrated a remarkably homogeneous dispersion of the NFC within the matrix, with minimal agglomeration observed. The nanocomposites showed significant mechanical improvements across all formulations. At higher NFC concentrations, a transition from a ductile to a more brittle state was observed, with tensile strength doubling compared to formulations with lower NFC content, highlighting NFC\'s reinforcing capability despite reduced ductility. The developed material outperformed TPS without added water, exhibiting a lighter color and reduced thermal and chemical degradation. These findings confirm the effectiveness of the methodology and the essential role of residual water in material plasticization and structuring.
publishDate 2024
dc.date.none.fl_str_mv 2024-12-12
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 https://www.teses.usp.br/teses/disponiveis/18/18158/tde-10022025-160621/
url https://www.teses.usp.br/teses/disponiveis/18/18158/tde-10022025-160621/
dc.language.iso.fl_str_mv eng
language eng
dc.relation.none.fl_str_mv
dc.rights.driver.fl_str_mv Liberar o conteúdo para acesso público.
info:eu-repo/semantics/openAccess
rights_invalid_str_mv Liberar o conteúdo para acesso público.
eu_rights_str_mv openAccess
dc.format.none.fl_str_mv application/pdf
dc.coverage.none.fl_str_mv
dc.publisher.none.fl_str_mv Biblioteca Digitais de Teses e Dissertações da USP
publisher.none.fl_str_mv Biblioteca Digitais de Teses e Dissertações da USP
dc.source.none.fl_str_mv
reponame:Biblioteca Digital de Teses e Dissertações da USP
instname:Universidade de São Paulo (USP)
instacron:USP
instname_str Universidade de São Paulo (USP)
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institution USP
reponame_str Biblioteca Digital de Teses e Dissertações da USP
collection Biblioteca Digital de Teses e Dissertações da USP
repository.name.fl_str_mv Biblioteca Digital de Teses e Dissertações da USP - Universidade de São Paulo (USP)
repository.mail.fl_str_mv virginia@if.usp.br|| atendimento@aguia.usp.br||virginia@if.usp.br
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