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Item 1. Plote os gráficos de TGA das matérias primas e do produto final produzido. Apresente as informações que podem ser retiradas do gráfico. Gráfico I: Taxa de degradação do EMA-GMA puro – 10°C/min em N2 Fonte: Autores (2020) Gráfico II: Taxa de degradação da borracha natural pura – 10°C/min em N2 Fonte: Autores (2020) Gráfico III: Taxa de degradação do Poli(ácido lático) – 10°C/min em N2 Fonte: Autores (2020) Gráfico IV: Taxa de degradação do compósito (PLA/NR/EMA-GMA) – 10°C/min em N2 Fonte: Autores (2020) A partir dos gráficos de Análise Termogravimétrica (TGA) é possível identificar se há a presença de substâncias voláteis, realizar a análise da composição e a temperatura inicial de degradação dos materiais, além de identificar se há presença de substâncias inorgânicas (materiais refratários). Tendo isso em vista e após a análise dos gráficos, é possível verificar que não há presença de voláteis na matéria prima, nem no produto, já que foi necessário uma elevada temperatura de ignição para a ocorrência das reações. Através da análise dos gráficos pode-se concluir que a decomposição das substâncias em questão ocorre em um único estágio, sendo possível utilizar a curva para definir os limites de estabilidade da amostra, determinar a estequiometria da reação e investigar a cinética da reação. Verifica-se também que a degradação térmica ocorreu na faixa de temperatura de 300 a 500 ºC, durante a qual ocorreu a perda de praticamente 100% de massa, ou seja, há baixa resistência térmica envolvida nas quatro situações. Tabela I: Perda de Massa e intervalo de temperatura do processo de degradação Fonte: Os autores (2020) Item 2. Plote os gráficos de DSC do PLA puro. Apresente as informações que podem ser retiradas do gráfico. A Calorimetria Exploratória Diferencial (DSC - do inglês "Differential Scanning Calorimetry"), é a análise na qual se acompanha a variação da energia entre a amostra e a referência (Cláudia Bernal, Andréa Boldarini, SuseteTrazzi e Eder Tadeu, 2002). Em um experimento de Calorimetria Exploratória Diferencial, mede-se a variação de entalpia que ocorre entre a amostra e a referência durante o processo de aquecimento/resfriamento, e eles ainda pontuam que para um processo endotérmico, com absorção de calor, observa-se a diminuição na temperatura da amostra e a inflexão na curva. Gráfico V- Análise DSC para PLA puro- 1º corrida de aquecimento Fonte: Os autores (2020) Os dados de DSC foram obtidos em atmosfera inerte (N2) com taxa de aquecimento a 10ºC por minuto. O círculo em laranja no gráfico apresenta um ponto onde há mudança de linha de base sem pico, os círculos na cor verde apresentam picos endotérmicos (onde há absorção de calor) e os círculos de cor vermelha mostram picos exotérmicos (onde há liberação de calor). Esses picos representados estão associados também a eventos físico-químicos dos materiais. Quando se tem picos “para baixo” normalmente estão relacionados à fusão e ebulição do material com característica endotérmica por exemplo. Esse segundo pico inferior demonstra uma cristalização que ocorre antes da fusão. Tabela 2- Caráter Exotérmico e Endotérmico dos picos DTA, de acordo com sua origem física ou química Fonte: Revista virtual Quimica Nova, vol 25, São Paulo (Set/Out 2002) Gráfico VI- Análise DSC para PLA puro – 1º corrida de resfriamento Fonte: Os autores (2020) Durante a 1º corrida em fase de resfriamento observa-se que a curva do gráfico se mostra de certa forma constante, isso acontece pois quando a amostra atinge a temperatura de Fusão ou de Ebulição por exemplo, ele mantém sua temperatura “estacionada” por um período, o que significa que essa amostra está absorvendo energia para fazer a mudança de estado físico. Durante esse momento não há nenhum pico de cristalização a quente. Segundo Klein (2009), quando é realizado o resfriamento de um polímero semicristalino a partir de seu estado fundido, isto é, acima da temperatura de fusão, o mesmo atinge uma temperatura na qual um grande número de cadeias poliméricas inicia uma ordenação espacial formando uma estrutura cristalina. Isto se reflete em toda a massa polimérica produzindo-se a cristalização da massa fundida. A cristalização pode correr de duas maneiras, de forma isotérmica, quando a temperatura é abaixada rapidamente até um dado valor de Tc, estabilizada e mantida constante até que toda a cristalização ocorra, ou de forma dinâmica quando a temperatura é reduzida a uma taxa constante. A cristalização neste caso ocorrerá dentro de uma aixa de temperatura, onde se tem a máxima taxa de conversão da cristalização. A cristalização isotérmica é a mais estudada, mas a dinâmica é a que está mais próxima dos sistemas industriais de solidificação Gráfico VII- Gráfico de análise DSC para PLA puro- 2º corrida de aquecimento Fonte: Os autores (2020) Na segunda corrida o material foi fundido e cristalizado novamente, por esse motivo apagam-se memórias das propriedades dos materiais e ele se comporta de maneira mais regular, sem tensões residuais do processo, pode-se observar que os picos não estão “tão acentuados. Através da análise dos gráficos é possível se identificar a temperatura de transição vítrea (Tg), temperatura de fusão (Tm) e a cristalização a frio (Tcc), sendo: Tabela 3 – Resultados das análises de DSC para primeiro e segundo aquecimento 1ª corrida 2ª corrida Tc (°C) 59,4 63,4 Tcc (°C) 92,4 96,1 Tm (°C) 169,8 168,6 Fonte: Os autores (2020) Segundo Ana Cristina Malheiros (2012), a temperatura de transição vítrea revela a mudança de um comportamento rígido para um comportamento de amolecimento do material. Os polímeros termoendurecíveis não apresentam fusão, eles apenas se degradam a elevadas temperaturas de forma irreversível. Por isto, a sua temperatura de transição vítrea é controlada pelo grau de reticulação da estrutura, e surgem, geralmente, alterações muito menos acentuadas quando comparados com os termoplásticos. Nos polímeros as propriedades mecânicas são extremamente dependentes da temperatura e do tempo de exposição. Os polímeros são viscoelásticos, ou seja, apresentam algumas propriedades dos líquidos viscosos e dos sólidos elásticos. A temperaturas baixas, a mobilidade das cadeias é muito pequena e o estado amorfo permanece. No caso de temperaturas altas, o polímero comporta-se como uma borracha, as cadeias poliméricas podem adquirir mobilidade suficiente para dar início ao processo de cristalização. Nesta região, e durante um arrefecimento lento, o polímero exibe grandes alongamentos quando lhe é aplicada carga e pode resistir a grandes extensões da ordem dos 100% ou mais sem deformações permanentes (Bower 2002). Segundo Tammann (1933), a temperatura de transição vítrea é a temperatura em que a fragilidade desaparece, ou seja, uma temperatura na qual a propensão a surgirem fendas é menor. Várias propriedades se alteram bruscamente na Tg. Acima da temperatura de transição vítrea, os polímeros têm comportamento do tipo borracha, facilmente deformáveis, tornando-se dúcteis. Quando a temperatura de um polímero cai abaixo da Tg, os átomos das cadeias poliméricas estão como congelados numa dada posição, ou seja, não se dá o movimento rotacional ou translacional, e o polímero comporta-se de maneira cada vez mais frágil. Muitos fatores podem alterar a Tg de um polímero, entre eles estão a estrutura química, o grau de cura e a massa molar. (da Silva et al. 2007). Quanto a Cristalização a frio, Marcelo Silveira Rabello, diz que esse fenômeno é originado do rearranjo das regiões amorfas numa fase cristalina, e ocorre quando temperaturas inadequadas são utilizadas durante a etapa de aquecimento das pré-formas ou quando o material utilizado apresenta alta tendência para cristalização. Embora a cristalização a frio seja indesejável durante o reaquecimento da pré-forma e antes do sopro, sua ocorrência durante a fase de soproestiramento é importante, pois o material semicristalino possui melhores propriedades mecânicas e de barreira. Da mesma forma, durantea termoformagem do PET a cristalização a frio pode ser desejável para a obtenção de produtos mais rígidos e mais resistentes ao calor por exemplo. A temperatura de fusão (Tm) é a temperatura na quais as cadeias poliméricas saem de sua estrutura cristalina se tornando um líquido sem ordem estabelecida. Neste ponto, a energia do sistema atinge o nível necessário para vencer as forças intermoleculares secundárias entre as cadeias da fase cristalina, destruindo a estrutura regular de empacotamento, mudando do estado de borracha para o estado viscoso (Spadetti et all, 2017). Segundo Klein (2009), este evento térmico só ocorre em materiais com um mínimo de cristalinidade. Em materiais totalmente amorfos este evento não ocorre, mas um outro evento chamado amolecimento. Trata-se de uma mudança termodinâmica de primeira ordem, afetando variáveis como volume específico e entalpia. A temperatura de fusão de materiais semicristalinos é um parâmetro muito importante tanto na aplicação quanto no processamento do material, também para se estabelecer os parâmetros do processo e prever as condições de temperatura na qual este material pode ser aplicado. Item 3) De acordo com os dados retirados de ambas análises (TGA e DSC), defina a faixa de temperatura para configurar os parâmetros de processamento e quais os cuidados que devem ser tomados com as matérias primas antes e durante o processamento Ao transferir os dados das análises termogravimétricas, pode se observar que a faixa de temperatura tem relação direta com a configuração elementar das amostras. No ensaio de TGA, a faixa de temperatura tem relação com a quantidade de elementos voláteis, umidade e de materiais orgânicos, que são queimados antes de chegar em 500ºC. Nos ensaios que necessitam eliminar a amostra para sua análise, é importante se atentar que a amostra não possua elementos voláteis em sua composição, também será necessário fazer a secagem do material, pode ser por meio de estufa em mais ou menos 110ºC, para que a presença de umidade seja totalmente eliminada. Em análises de DSC, para a definição da faixa de temperatura em relação à entalpia, é observado onde ocorre à temperatura de fusão cristalina do PLA, os picos de entalpia podem ocorrer em diversos pontos, então se deve adotar a análise das reações desde a temperatura inicial desejada, e a presença de líquidos e voláteis também interferem no diagrama. Então por isso também é importante secagem e eliminação de partículas heterogêneas. REFERÊNCIAS BIBLIOGRÁFICAS Bernal, Cláudia. Boldarini, Andréa Couto. Breviglieri, Trazzi. Cavalheiro, Éder Tadeu. Departamento de Química, Universidade Federal de São Carlos. INFLUÊNCIA DE ALGUNS PARÂMETROS EXPERIMENTAIS NOS RESULTADOS DE ANÁLISES CALORIMÉTRICAS DIFERENCIAIS – DSC. Quimica Nova, volume 25, nº 5. São Paulo, Setembro/outubro, 2002. Disponível em:< https://www.scielo.br/scielo.php?pid=S0100-40422002000500023&script=sci_arttext>. Acesso em 26/05/2020 às 22h15min. Carbolite Gero. Loss on ignition (LOI)/Loss on dry (LOD) Thermogravimetric analysis (TGA). Disponível em: <https://www.carbolite-gero.com/applications/heating-applications/loss-on-drying-ignition/> Acesso em 01/06/2020 ás 09:40 Klein, Catia. Síntese e caracterização de poliésteres termoplásticos. Disponivel em: http://tede2.pucrs.br/tede2/bitstream/tede/3148/1/418870.pdf. Acesso em 30/05/2020 às 10h42. Malheiro, Ana Cristina. Efeito da temperatura de cura na temperatura de transição vítrea de um adesivo estrutural. Dissertação do MIEM. Faculdade de Engenharia da Universidade do Porto, Mestrado Integrado em Engenharia Mecânica. Janeiro de 2012. Disponível em:< https://repositorio-aberto.up.pt/bitstream/10216/63347/1/000151156.pdf. Acesso em 27/05/2020 às 13h02min. Rabello, Marcelo Silveira. Wellen, Renate Maria. Estudo da cristalização a frio do poli (tereftalato de etileno) (PET) para produção de embalagens. Revista Eletrônica de Materiais e Processos, Vol. 3, No 2 (2008). Disponível em:< http://www2.ufcg.edu.br/revista-remap/index.php/REMAP/article/viewArticle/71>. Acesso em: 26/05/2020 às 22h40min. Spadetti, Carolini. Filho, Eloi. Sena, Geovane. Melo, Carlos. Propriedades térmicas e mecânicas dos compósitos de Polipropileno pós-consumo reforçados com fibras de celulose. Disponível em: https://www.scielo.br/pdf/po/v27nspe/0104-1428-po-0104-14282320.pdf. Acesso em 30/05/2020 às 10h18. Poli(ácido lático) Temperatura (°C) 30.93159 30.92878 30.919250000000002 30.912790000000001 30.906420000000001 30.904219999999999 30.898319999999998 30.893439999999998 30.884460000000001 30.88457 30.8765 30.878299999999999 30.872450000000001 30.865939999999998 30.865570000000002 30.85744 30.854469999999999 30.84732 30.84695 30.845849999999999 30.834060000000001 30.833559999999999 30.829689999999999 30.826550000000001 30.818200000000001 30.812750000000001 30.814800000000002 30.813859999999998 30.80979 30.802980000000002 30.801400000000001 30.800999999999998 30.79926 30.79486 30.795580000000001 30.801359999999999 30.794049999999999 30.79618 30.79731 30.8 30.798559999999998 30.80114 30.798249999999999 30.800940000000001 30.808050000000001 30.813890000000001 30.810659999999999 30.81954 30.820489999999999 30.823260000000001 30.833320000000001 30.841940000000001 30.849440000000001 30.859200000000001 30.862760000000002 30.870370000000001 30.878630000000001 30.89002 30.897880000000001 30.911380000000001 30.927489999999999 30.93948 30.952439999999999 30.96584 30.978719999999999 30.994499999999999 31.004090000000001 31.02112 31.04 0700000000001 31.061720000000001 31.077110000000001 31.09252 31.115559999999999 31.13467 31.153870000000001 31.172090000000001 31.197240000000001 31.221800000000002 31.250150000000001 31.27252 31.29543 31.326329999999999 31.35351 31.378699999999998 31.408449999999998 31.43468 31.46463 31.494890000000002 31.528179999999999 31.562950000000001 31.598600000000001 31.629169999999998 31.668019999999999 31.70092 31.736719999999998 31.773440000000001 31.81118 31.847490000000001 31.889559999999999 31.926839999999999 31.965579999999999 32.015680000000003 32.055059999999997 32.092199999999998 32.142380000000003 32.185479999999998 32.230759999999997 32.283450000000002 32.324420000000003 32.375480000000003 32.423070000000003 32.475589999999997 32.522129999999997 32.565600000000003 32.625349999999997 32.679819999999999 32.729799999999997 32.783850000000001 32.83296 32.88944 32.947220000000002 33.005899999999997 33.064070000000001 33.120539999999998 33.18074 33.238639999999997 33.297139999999999 33.355980000000002 33.41921 33.48749999999999 7 33.550739999999998 33.611800000000002 33.680109999999999 33.743099999999998 33.813479999999998 33.884999999999998 33.94641 34.015329999999999 34.087420000000002 34.155760000000001 34.224510000000002 34.29909 34.368459999999999 34.43835 34.508049999999997 34.58614 34.660870000000003 34.72587 34.809280000000001 34.88496 34.958219999999997 35.03792 35.118949999999998 35.197420000000001 35.27843 35.357520000000001 35.43638 35.522219999999997 35.601239999999997 35.681840000000001 35.762650000000001 35.849310000000003 35.929000000000002 36.011299999999999 36.092089999999999 36.177639999999997 36.261420000000001 36.353149999999999 36.437159999999999 36.523319999999998 36.605960000000003 36.700589999999998 36.782040000000002 36.871319999999997 36.963799999999999 37.049869999999999 37.139530000000001 37.233319999999999 37.323610000000002 37.417160000000003 37.504640000000002 37.595370000000003 37.687379999999997 37.780679999999997 37.877040000000001 37.967010000000002 38.063279999999999 38 .158679999999997 38.252029999999998 38.350949999999997 38.440899999999999 38.537280000000003 38.634520000000002 38.730139999999999 38.826529999999998 38.928939999999997 39.02422 39.121450000000003 39.22063 39.316310000000001 39.418410000000002 39.510379999999998 39.611499999999999 39.7072 39.805230000000002 39.905279999999998 40.001579999999997 40.106839999999998 40.203600000000002 40.307099999999998 40.405839999999998 40.503390000000003 40.603569999999998 40.702449999999999 40.8071540.909080000000003 41.010080000000002 41.107460000000003 41.204740000000001 41.307659999999998 41.412320000000001 41.517040000000001 41.616880000000002 41.722079999999998 41.814900000000002 41.919589999999999 42.022860000000001 42.12122000 0000001 42.224960000000003 42.334299999999999 42.434519999999999 42.537039999999998 42.637259999999998 42.738680000000002 42.840899999999998 42.947119999999998 43.044159999999998 43.15211 43.256480000000003 43.348840000000003 43.456200000000003 43.559179999999998 43.658099999999997 43.767380000000003 43.86562 43.964579999999998 44.069499999999998 44.172739999999997 44.275739999999999 44.37388 44.478839999999998 44.581679999999999 44.684280000000001 44.782980000000002 44.888649999999998 44.994680000000002 45.09543 45.195180000000001 45.300510000000003 45.399900000000002 45.49718 45.602960000000003 45.707680000000003 45.808990000000001 45.902979999999999 46.008800000000001 46.11542 46.217260000000003 46.316600000000001 46.415790000000001 46.518720000000002 46.618479999999998 46.715470000000003 46.81756 46.918610000000001 47.020389999999999 47.119120000000002 47.21942 47.317889999999998 47.413890000000002 47.517919999999997 47.613439999999997 47.713079999999998 47.807200000000002 47.911439999999999 48.013640000000002 48.108280000000001 48.208100000000002 48.310940000000002 48.406999999999996 48.506500000000003 48.602519999999998 48.701309999999999 48.80086 48.893799999999999 48.99033 49.086970000000001 49.18824 49.283 180000000002 49.373939999999997 49.473939999999999 49.570540000000001 49.666600000000003 49.76153 49.859099999999998 49.952779999999997 50.047739999999997 50.142870000000002 50.234780000000001 50.329859999999996 50.429839999999999 50.52563 50.613840000000003 50.707909999999998 50.805329999999998 50.893239999999999 50.985619999999997 51.077240000000003 51.177 51.270339999999997 51.363320000000002 51.448120000000003 51.542819999999999 51.636539999999997 51.73104 51.818939999999998 51.912790000000001 52.00929 52.096899999999998 52.190899999999999 52.278170000000003 52.36674 52.462560000000003 52.551540000000003 52.637419999999999 52.725119999999997 52.820630000000001 52.910040000000002 53.00123 53.091560000000001 53.183889999999998 53.271169999999998 53.357689999999998 53.444249999999997 53.532350000000001 53.619 53.707259999999998 53.796680000000002 53.882150000000003 53.970680000000002 54.057639999999999 54.146000000000001 54.229759999999999 54.313 389999999998 54.406759999999998 54.491680000000002 54.578049999999998 54.660739999999997 54.750140000000002 54.835599999999999 54.921840000000003 55.00376 55.093739999999997 55.177799999999998 55.25864 55.346829999999997 55.427930000000003 55.515059999999998 55.598559999999999 55.681159999999998 55.767760000000003 55.853589999999997 55.93526 56.017740000000003 56.09834 56.180929999999996 56.264679999999998 56.353059999999999 56.436439999999997 56.515180000000001 56.594760000000001 56.6785 56.759630000000001 56.836840000000002 56.9208 57.005380000000002 57.088299999999997 57.171720000000001 57.253129999999999 57.333370000000002 57.412260000000003 57.492240000000002 57.571480000000001 57.652589999999996 57.733179999999997 57.812950000000001 57.893949999999997 57.974780000000003 58.055160000000001 58.1389 58.216799999999999 58.29562 58.37359 58.461129999999997 58.535339999999998 58.612189999999998 58.689880000000002 58.766350000000003 58.850960000000001 58.927979999999998 59.012099999999997 59.087499999999999 59.163200000000003 59.239449999999998 59.326369999999997 59.398899999999998 59.484059999999999 59.559570000000001 59.637970000000003 59.710209999999996 59.789259999999999 59.870800000000003 59.948860000000003 60.022950000000002 60.103000000000002 60.181710000000002 60.25996 60.334319999999998 60.413469999999997 60.486249999999998 60.570219999999999 60.64385 60.722549999999998 60.80124 60.874899999999997 60.955689999999997 61.027709999999999 61.10369 61.186839999999997 61.267110000000002 61.340260000000001 61.416640000000001 61.491140000000001 61.56221 61.643239999999999 61.716749999999998 61.796239999999997 61.87473 61.954419999999999 62.02657 62.105159999999998 62.18242 62.258989999999997 62.331800000000001 62.40869 62.482500000000002 62.558120000000002 62.635370000000002 62.717219999999998 62.78783 62.867240000000002 62.941980000000001 63.017699999999998 63.09778 63.164119999999997 63.241109999999999 63.317430000000002 63.396880000000003 63.470799999999997 63.542380000000001 63.623620000000003 63.702219999999997 63.7789 63.853400000000001 63.932169999999999 64.010840000000002 64.084760000000003 64.159660000000002 64.237160000000003 64.315899999999999 64.388869999999997 64.46669 64.543530000000004 64.617090000000005 64.69247 64.767219999999995 64.841329999999999 64.919929999999994 64.995900000000006 65.070009999999996 65.145920000000004 65.227500000000006 65.300370000000001 65.37724 65.455299999999994 65.526300000000006 65.610060000000004 65.686089999999993 65.760350000000003 65.838499999999996 65.915090000000006 65.992009999999993 66.067920000000001 66.142719999999997 66.220500000000001 66.292389 999999997 66.374009999999998 66.450630000000004 66.526510000000002 66.603999999999999 66.680189999999996 66.752799999999993 66.832459999999998 66.912000000000006 66.983879999999999 67.062389999999994 67.136499999999998 67.215050000000005 67.291020000000003 67.37 0199999999997 67.446600000000004 67.526740000000004 67.60078 67.680800000000005 67.760009999999994 67.832530000000006 67.908810000000003 67.985979999999998 68.063659999999999 68.139219999999995 68.217920000000007 68.295240000000007 68.370750000000001 68.454179999999994 68.532759999999996 68.611260000000001 68.687100000000001 68.771879999999996 68.84599 68.924760000000006 68.995999999999995 69.081119999999999 69.1554 69.235050000000001 69.310820000000007 69.397660000000002 69.475899999999996 69.552120000000002 69.631489999999999 69.71396 69.791309999999996 69.866569999999996 69.949100000000001 70.027119999999996 70.106620000000007 70.186220000000006 70.264989999999997 70.346500000000006 70.425439999999995 70.49909999999 9999 70.582560000000001 70.66028 70.743350000000007 70.819779999999994 70.904660000000007 70.985699999999994 71.066159999999996 71.145139999999998 71.223150000000004 71.304349999999999 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