Aujourd’hui le développement de nouveaux matériaux polymères ayant de bonnes propriétés repose de plus en plus sur des procédés de mélange ou de compoundage de polymères au lieu de recourir à la synthèse de nouvelles molécules. L’action du mélange peut fortement influer sur la morphologie des matériaux polymères multi-constituants. Les extrudeuses bi-vis (TSE) sont souvent utilisées comme mélangeurs/réacteurs pour des procédés de mélange, de compoundage et d’extrusion réactive. Cependant, l’étude sur la qualité du mélange dans les TSE demeure un grand défi en raison de la complexité géométrique et du caractère transitoire de l’écoulement. Cette thèse a pour objet de développer un nouvel instrument en line pour mesurer en temps réel la distribution des temps de séjour (DTS) qui caractérise la performance du mélange axial et la capacité de convoyage de différents types d’éléments de vis basées sur l’analyse de l’écoulement transitoire et l’évaluation systématique de la théorie de mélange dans les TSE. Le mélange distributif des polymères fondus est caractérisé par la génération de l’aire des interfaces, un paramètre difficile à mesurer expérimentalement. Alors on fait appel à des simulations numériques de type CFD / The development of new materials with improved properties seems to rely nowadays more on blending and compounding than on the synthesis of chemically new polymers. Mixing may have a great effect on the morphology and structure of multi-component polymer materials. Twin-screw extruders (TSE) are widely used as mixers/reactors for blending, compounding, and reactive processing. This work aimed at developing a new instrument to measure in real time the residence time distribution (RTD) which characterizes the axial mixing and transport abilities of different screw elements based on the analysis of the transient flow pattern and systematic evaluation of mixing theory in TSE. Distributive mixing of polymer melts is characterized by the generation of interfacial area, which is experimentally much more difficult to measure. This 3D numerical simulation based on CFD is adopted

Aujourd’hui le développement de nouveaux matériaux polymères ayant de bonnes propriétés repose de plus en plus sur des procédés de mélange ou de compoundage de polymères au lieu de recourir à la synthèse de nouvelles molécules. L’action du mélange peut fortement influer sur la morphologie des matériaux polymères multi-constituants. Les extrudeuses bi-vis (TSE) sont souvent utilisées comme mélangeurs/réacteurs pour des procédés de mélange, de compoundage et d’extrusion réactive. Cependant, l’étude sur la qualité du mélange dans les TSE demeure un grand défi en raison de la complexité géométrique et du caractère transitoire de l’écoulement. Cette thèse a pour objet de développer un nouvel instrument en line pour mesurer en temps réel la distribution des temps de séjour (DTS) qui caractérise la performance du mélange axial et la capacité de convoyage de différents types d’éléments de vis basées sur l’analyse de l’écoulement transitoire et l’évaluation systématique de la théorie de mélange dans les TSE. Le mélange distributif des polymères fondus est caractérisé par la génération de l’aire des interfaces, un paramètre difficile à mesurer expérimentalement. Alors on fait appel à des simulations numériques de type CFD / The development of new materials with improved properties seems to rely nowadays more on blending and compounding than on the synthesis of chemically new polymers. Mixing may have a great effect on the morphology and structure of multi-component polymer materials. Twin-screw extruders (TSE) are widely used as mixers/reactors for blending, compounding, and reactive processing. This work aimed at developing a new instrument to measure in real time the residence time distribution (RTD) which characterizes the axial mixing and transport abilities of different screw elements based on the analysis of the transient flow pattern and systematic evaluation of mixing theory in TSE. Distributive mixing of polymer melts is characterized by the generation of interfacial area, which is experimentally much more difficult to measure. This 3D numerical simulation based on CFD is adopted

O objetivo deste trabalho é avaliar a viabilidade técnica do desenvolvimento de uma miniextrusora dupla-rosca corrotativa que, além de processar a matéria-prima, possa exercer a função de um cabeçote de impressão 3D. Os avanços tecnológicos na área da manufatura relacionados à impressão 3D têm gerado grande entusiasmo nos últimos 10 anos, na medida em que possibilitam a fabricação de formas geométricas de alta complexidade diretamente a partir de arquivos digitais, agilizando a cadeia de produção e reduzindo custos de ferramental associados. Apesar das inúmeras vantagens, a Manufatura Aditiva (MA) ainda é uma tecnologia em desenvolvimento e, portanto, apresenta desafios para que possa realmente atender às novas demandas criadas pela comunidade científica e industrial, muitos deles relacionados com a busca por novos materiais de impressão, com a melhoria dos materiais utilizados, das estratégias de deposição visando menor tempo de fabricação e maior precisão dimensional e com a ausência de padronização para os processos. As tendências no desenvolvimento de materiais para as técnicas de MA por extrusão apontam tanto para a elaboração de compósitos de matriz polimérica e blendas capazes de conferir propriedades mecânicas mais apropriadas às impressões e/ou proporcionar novas funcionalidades, quanto para o desenvolvimento de sistemas que possibilitem a deposição de matérias-primas diferenciadas ou a incorporação de soluções de pós-processamento para compor sistemas híbridos de manufatura. Nesse contexto, a principal motivação deste trabalho é a ausência de um equipamento para produção de compósitos poliméricos e blendas a partir pequenas quantidades de material em pó (cerca de 200 g) e que também seja capaz de estruturar objetos tridimensionais por meio da deposição de camadas sucessivas de material fundido. A fim de obter o conjunto de parâmetros geométricos e operacionais fundamentais para a definição e avaliação da miniextrusora dupla-rosca, houve a necessidade de se desenvolver um procedimento sistemático integrando conceitos de projeto de máquinas, processo de extrusão dupla-rosca e reologia aplicados ao contexto da MA. O método de projeto resultante considera requisitos funcionais e restrições geométricas específicas, conciliando a necessidade de manter uma folga constante entre as roscas com a desejada ação de autolimpeza obtida por meio da interpenetração das mesmas. A capacidade de processar o material viscoso com o torque fornecido às roscas, requisito crítico a ser atendido, foi avaliada teoricamente para o ABS (acrilonitrila butadieno estireno) virgem e validada experimentalmente para três sistemas baseados em ABS com auxílio de um reômetro de torque. Ao final do estudo, foi obtido um modelo geométrico virtual de dimensões reduzidas (69,6x75x201 mm) e na sequência foi construído um mock-up com auxílio da impressão 3D para avaliação das tolerâncias dimensionais, cinemática e funcionalidades básicas do conjunto. Estima-se que a miniextrusora projetada, operando a 10 rpm, seja capaz de processar até 0,2 kg/h e gerar 60% do calor necessário para a fusão (ABS), mostrando-se viável para aplicação como cabeçote intercambiável de impressão 3D destinado à pesquisa de novos materiais para MA. / The objective of this document is accessing the development feasibility of a mini co-rotating twin-screw extruder capable of mixing different materials and performing the function of 3D printhead. The technological progress in the manufacturing context related to 3D printing have generated great enthusiasm in the last 10 years, as it enables fabricating complex geometric shapes directly from digital files, speeding up production chain and reducing associated tooling costs. Despite the many advantages, Additive Manufacturing (AM) is still an emerging technology and must overcome challenges to effectively meet the new demands created by scientific and industrial communities, many of them related to the search for new building materials, improving current materials and deposition strategies, in order to achieve faster fabrication and increased dimensional precision, as well as the lack of process standardization. Tendencies towards material development to AM techniques based in extrusion points to the formulation of different polymer matrix composites and blends capable of imparting more appropriate mechanical properties to the 3D prints and/or provide new functionalities, as well as to the development of systems capable of depositing special raw materials or to the incorporation of post processing solutions composing hybrid manufacture systems. In that context, the main motivation for this work is the lack of an equipment for producing polymer composites and blends from small amounts of powder material (about 200 g) that is also capable of structuring three-dimensional objects depositing successive layers of fused material. In order to obtain the fundamental geometric and operational parameters set to define and access the mini twin-screw extruder, it was necessary to develop a systematic procedure integrating concepts from machine design, twin-screw extrusion and rheology applied to the AM context. The resulting design method considers specific functional requisites and geometric constraints, conciliating the need for a constant clearance between the screws and the desired self-cleaning action obtained with closely intermeshing screws. The capacity to process viscous material with the torque provided to the screws, a critical requisite to be met, was theoretically evaluated considering ABS resin (acrylonitrile butadiene styrene) and experimentally validated to three polymer systems based in ABS with a torque rheometer. At the end of the study, a virtual geometric model with reduced dimensions (69.6x75x201 mm) was obtained and then a mock-up was 3D printed in order to evaluate dimensional tolerances, cinematics and basic functionalities. It is estimated that the mini twin-screw extruder designed is able to process up to 0.2 kg/h running at 10 rpm and generate 60% of the heat necessary to melt the polymer (ABS), showing to be feasible to its application as an interchangeable 3D printhead for research of new materials in AM.

Esse trabalho apresenta um modelo termodinâmico de uma bomba multifásica do tipo duplo parafuso. Para uma dada condição de operação, o modelo calcula a potência consumida, as condições do fluido na descarga e o perfil de pressão ao longo da bomba. Ao invés de simular diretamente o escoamento dentro da bomba, simulou-se os processos que ocorrem dentro das suas câmaras. Para tanto, dividiu-se o processo de bombeamento multifásico em uma seqüência de processos simples, facilitando-se a construção do modelo no simulador de processos Hysys.Process v2.1. Os resultados de potência e temperatura de descarga obtidos com a simulação mostram uma boa concordância com valores experimentais, principalmente para FVG’s baixos. Para FVG’s elevados, o modelo passa a superestimar a potência consumida indicando que as fendas, nesses casos, já não se encontram totalmente preenchidas com líqüido. Dos resultados obtidos para o refluxo, conclui-se que, das equações sugeridas na literatura, aquelas para escoamento turbulento liso são mais adequadas para os números de Reynolds envolvidos. O perfil de pressão e a vazão de refluxo quando o escoamento é multifásico aproxima-se qualitativamente das medições experimentais. Estudou-se a influência de diversos parâmetros na eficiência exergética da bomba. Os resultados mostram que a otimização da eficiência depende das condições de operação da bomba: FVG, tipo de líqüido, diferença de pressão, entre outros. / The goal of this project was to develop a thermodynamic model of a twin-screw multiphase pump. With given operation conditions the model can determine the absorbed power, discharge conditions and the pressure profile along the screw. An alternative approach was suggested to overcome the complex flow problem and the processes inside the pump were simulated instead of direct simulation of the flow. For this purpose, the multiphase pumping process was divided in a sequence of simple processes so the model could be developed in an easier way. The power and temperature values calculated by the model are in good agreement with experimental data, mainly when the gas fraction is low. With higher gas fractions, the model overestimates the absorbed power indicating that screw gaps are not completely filled with liquid anymore. Concerning about the backflow rate, the results show that the equations for turbulent flow in smooth ducts fits better the Reynolds number range in the gaps. The pressure profile and backflow rate for multiphase flow agree qualitatively with experimental results. The influence of several parameters in the exergetic eficiency of the pump were analysed and results show that the efficiency optimization depends on pump operation conditions: gas fraction, liquid type, pressure difference and others.

Esse trabalho apresenta um modelo termodinâmico de uma bomba multifásica do tipo duplo parafuso. Para uma dada condição de operação, o modelo calcula a potência consumida, as condições do fluido na descarga e o perfil de pressão ao longo da bomba. Ao invés de simular diretamente o escoamento dentro da bomba, simulou-se os processos que ocorrem dentro das suas câmaras. Para tanto, dividiu-se o processo de bombeamento multifásico em uma seqüência de processos simples, facilitando-se a construção do modelo no simulador de processos Hysys.Process v2.1. Os resultados de potência e temperatura de descarga obtidos com a simulação mostram uma boa concordância com valores experimentais, principalmente para FVG’s baixos. Para FVG’s elevados, o modelo passa a superestimar a potência consumida indicando que as fendas, nesses casos, já não se encontram totalmente preenchidas com líqüido. Dos resultados obtidos para o refluxo, conclui-se que, das equações sugeridas na literatura, aquelas para escoamento turbulento liso são mais adequadas para os números de Reynolds envolvidos. O perfil de pressão e a vazão de refluxo quando o escoamento é multifásico aproxima-se qualitativamente das medições experimentais. Estudou-se a influência de diversos parâmetros na eficiência exergética da bomba. Os resultados mostram que a otimização da eficiência depende das condições de operação da bomba: FVG, tipo de líqüido, diferença de pressão, entre outros. / The goal of this project was to develop a thermodynamic model of a twin-screw multiphase pump. With given operation conditions the model can determine the absorbed power, discharge conditions and the pressure profile along the screw. An alternative approach was suggested to overcome the complex flow problem and the processes inside the pump were simulated instead of direct simulation of the flow. For this purpose, the multiphase pumping process was divided in a sequence of simple processes so the model could be developed in an easier way. The power and temperature values calculated by the model are in good agreement with experimental data, mainly when the gas fraction is low. With higher gas fractions, the model overestimates the absorbed power indicating that screw gaps are not completely filled with liquid anymore. Concerning about the backflow rate, the results show that the equations for turbulent flow in smooth ducts fits better the Reynolds number range in the gaps. The pressure profile and backflow rate for multiphase flow agree qualitatively with experimental results. The influence of several parameters in the exergetic eficiency of the pump were analysed and results show that the efficiency optimization depends on pump operation conditions: gas fraction, liquid type, pressure difference and others.

The objective of this work is to determine the effect of four process variables on the properties of blends composed of bisphenol-A polycarbonate (PC) and poly (butylene terephthalate) (PBT) polymers which are compounded using a large scale commercial extruder. The four variables studied are blend composition, specific energy consumption, residence time and shear rate. The last three factors were varied using the extruder screw speed and feed rate. The PC/PBT blends, commercially known as XENOY, were compounded using a WP ZSK 58 mm co-rotating twin screw extruder at the facility of SABIC Innovative Plastics in Cobourg Ontario. The extruder was instrumented to measure online the die pressure, specific energy consumption and blend temperature. The blends were characterized using differential scanning calorimetry, (DSC), scanning electron microscopy, (SEM), gel permeation chromatography, (GPC), and melt volume flow rate, (MVR). After processing, the blend properties determined were melting temperature, glass transition temperature, crystallinity, amorphous phase weight fraction, amorphous phase composition, phase morphology, PBT-rich-phase size, blend molecular weight distribution, and MVR. Using principles available in the literature, a linear regression model was developed to relate the process variables with the online measured properties and output blend properties. Fitting this model allowed the relative importance of each process variable to be estimated for each property. An attempt was also made to identify the general type of PC/PBT blend studied and how it compares with published PC/PBT blend data. It was found that the blends studied were well stabilized since there was no evidence of significant co-polymer formation during processing. Small decreases in molecular weight were attributed to mechanical degradation. Blending increased the crystallization and melting temperatures, as well as blend crystallinity. No practically significant difference in melting temperatures was observed between the different processing conditions. Analysis of glass transitions indicated that the blend components were partially miscible. The amorphous phase compositions were unaffected by blend composition or processing; however, the weight fraction PC-rich-phase present in the blend was strongly influenced by the screw speed. The phase structure of as-extruded blends could not be resolved using the SEM. Therefore, the blends were annealed to coarsen the phases. After annealing, a continuous PC-rich-phase and a discrete PBT-rich-phase were observed. The PBT phase size increased with increasing PBT content. No other statistically significant effects on phase size were observed but this is not conclusive due to the large scatter in the measurements. MVR was primarily influenced by blend composition and specific energy consumption, with the effects of composition being dominant. Further study using higher imaging resolution is required if the phase structures of as received blend pellets are to be characterized. Contrary to current practice, it is recommended that the Utracki-Jukes equation be used rather than the Fox equation for determining amorphous phase composition from glass transition data in PC/PBT blends.

The objective of this work is to determine the effect of four process variables on the properties of blends composed of bisphenol-A polycarbonate (PC) and poly (butylene terephthalate) (PBT) polymers which are compounded using a large scale commercial extruder. The four variables studied are blend composition, specific energy consumption, residence time and shear rate. The last three factors were varied using the extruder screw speed and feed rate. The PC/PBT blends, commercially known as XENOY, were compounded using a WP ZSK 58 mm co-rotating twin screw extruder at the facility of SABIC Innovative Plastics in Cobourg Ontario. The extruder was instrumented to measure online the die pressure, specific energy consumption and blend temperature. The blends were characterized using differential scanning calorimetry, (DSC), scanning electron microscopy, (SEM), gel permeation chromatography, (GPC), and melt volume flow rate, (MVR). After processing, the blend properties determined were melting temperature, glass transition temperature, crystallinity, amorphous phase weight fraction, amorphous phase composition, phase morphology, PBT-rich-phase size, blend molecular weight distribution, and MVR. Using principles available in the literature, a linear regression model was developed to relate the process variables with the online measured properties and output blend properties. Fitting this model allowed the relative importance of each process variable to be estimated for each property. An attempt was also made to identify the general type of PC/PBT blend studied and how it compares with published PC/PBT blend data. It was found that the blends studied were well stabilized since there was no evidence of significant co-polymer formation during processing. Small decreases in molecular weight were attributed to mechanical degradation. Blending increased the crystallization and melting temperatures, as well as blend crystallinity. No practically significant difference in melting temperatures was observed between the different processing conditions. Analysis of glass transitions indicated that the blend components were partially miscible. The amorphous phase compositions were unaffected by blend composition or processing; however, the weight fraction PC-rich-phase present in the blend was strongly influenced by the screw speed. The phase structure of as-extruded blends could not be resolved using the SEM. Therefore, the blends were annealed to coarsen the phases. After annealing, a continuous PC-rich-phase and a discrete PBT-rich-phase were observed. The PBT phase size increased with increasing PBT content. No other statistically significant effects on phase size were observed but this is not conclusive due to the large scatter in the measurements. MVR was primarily influenced by blend composition and specific energy consumption, with the effects of composition being dominant. Further study using higher imaging resolution is required if the phase structures of as received blend pellets are to be characterized. Contrary to current practice, it is recommended that the Utracki-Jukes equation be used rather than the Fox equation for determining amorphous phase composition from glass transition data in PC/PBT blends.

Submitted by Ronildo Prado (ronisp@ufscar.br) on 2017-08-23T13:47:40Z No. of bitstreams: 1 DissRB.pdf: 6420019 bytes, checksum: 9a9303246e3fd99e5635cc0d40d684d5 (MD5) / Approved for entry into archive by Ronildo Prado (ronisp@ufscar.br) on 2017-08-23T13:47:48Z (GMT) No. of bitstreams: 1 DissRB.pdf: 6420019 bytes, checksum: 9a9303246e3fd99e5635cc0d40d684d5 (MD5) / Approved for entry into archive by Ronildo Prado (ronisp@ufscar.br) on 2017-08-23T13:47:53Z (GMT) No. of bitstreams: 1 DissRB.pdf: 6420019 bytes, checksum: 9a9303246e3fd99e5635cc0d40d684d5 (MD5) / Made available in DSpace on 2017-08-23T13:48:00Z (GMT). No. of bitstreams: 1 DissRB.pdf: 6420019 bytes, checksum: 9a9303246e3fd99e5635cc0d40d684d5 (MD5) Previous issue date: 2017-03-08 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES) / The present study investigated the utilization efficiency of an intermeshing co-rotating twin-screw extruder (ICTSE) in the devulcanization of natural rubber compounds (NR), evaluating the physical, chemical and mechanical characteristics of these materials in each project step. Three accelerated compounds with different sulfur concentrations were submitted to torque rheometry and vulcanized according these results aiming the achievement of elastomers with different crosslinks densities. The influences on the characteristics of the devulcanized material caused by the variation of the extruder barrel temperature, screw rotation, thermoplastics addition and material stiffness were evaluated. Thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), infrared spectroscopy (FTIR), soluble fraction extraction and crosslink density were performed, evaluating the devulcanized compound. Horikx's theory was also used as an indicator of selective crosslink cleavage, defining the compounds to be revulcanized for comparison with the virgin pure material. The revulcanization was carried out with the mixture of the devulcanized compound with the pure, in the proportions of 30/70 w/w, respectively, and in the devulcanized compound singularly, with addition of complementary vulcanization system in both cases. The mechanical, dynamic-mechanical and crosslink density properties of the revulcanized compounds were characterized and evaluated in relation to the properties of the pure compounds. The increase in the concentration of uncrosslinked BN chains and the concentration of sulfur compounds in the extruded samples was observed by thermal tests and spectrocopy, together with the verification of a high level of devulcanization percentage, according to Flory-Rehner, evidencing the regeneration of the natural rubber existent. Also, satisfactory mechanical properties were found in the revulcanized compounds, especially when using auxiliary thermoplastics, revealing the great potential of ERDCI processing for the reuse of discarded BN compounds. / O presente estudo avaliou a eficiência de utilização de uma extrusora com rosca dupla co-rotacional e interpenetrante (ERDCI) na desvulcanização de compostos de borracha natural (BN), avaliando as características físicas, químicas e mecânicas destes materiais em cada fase do projeto. Três compostos acelerados com diferentes concentrações de enxofre foram submetidos a reometria de torque, e vulcanizados de acordo com a curva reométrica, para obtenção de elastômeros com diferentes densidades de ligações cruzadas. Foram avaliadas as influências nas características do material desvulcanizado, causadas pela variação da temperatura do barril da extrusora, velocidade de rotação das roscas, adição de termoplásticos e módulo elástico do material. Análises de termogravimetria (TGA), calorimetria exploratória diferencial (DSC), espectroscopia no infravermelho (FTIR), fração solúvel (FS) e densidade de ligações cruzadas foram realizadas, avaliandose o composto desvulcanizado. A teoria de Horikx também foi utilizada como indicativa da seletividade de ruptura de ligações cruzadas, definindo os compostos a serem revulcanizados para comparação com o material virgem. A revulcanização foi realizada com a mistura de 30 %(m/m) do composto desvulcanizado e 70 %(m/m) do puro, e também com 100 % do composto desvulcanizado, e adição de sistema de vulcanização complementar. Caracterizou-se os compostos revulcanizados quanto às suas propriedades mecânicas, dinâmico-mecânicas e densidade de ligações cruzadas. Através dos ensaios TGA, DSC, FTIR e a verificação de alto nível de percentual de desvulcanização pela teoria de Flory- Rehner, foi observado o aumento da concentração de cadeias de BN não reticuladas e da concentração de compostos de enxofre nas amostras extrudadas, evidenciando a regeneração da BN presente nos compostos. Também foram encontradas propriedades mecânicas satisfatórias nos compostos revulcanizados, principalmente quando utilizados termoplásticos auxiliares, revelando o grande potencial do processamento por ERDCI para a reutilização de compostos de BN descartados.

Les procédés de transformation de biomasse lignocellulosique en bioéthanol de seconde génération sont actuellement des sujets de recherche très répandus mais ne sont toujours pas compétitifs avec ceux de la première génération. Les facteurs clés limitants sont : l’efficacité et les coûts du prétraitement, les rendements de l’hydrolyse enzymatique, et la co-fermentation C5-C6. Un procédé continu de déconstruction de la matière végétale, compactant un prétraitement thermo-mécano-chimique utilisant un agent alcalin avec une introduction d’enzymes en extrusion bi-vis, appelé bioextrusion, est développé dans cette étude. Il permet de préparer la matière cellulosique à un haut taux de matière sèche (>20%), à une saccharification et une fermentation pouvant être simultanées (SSF). Le traitement continu peut extraire une grande part des hémicelluloses (jusqu’à 97%) et des lignines (>50%) et améliorer l’accessibilité de la cellulose tout en initiant sa dépolymérisation par des cocktails enzymatiques pendant la bioextrusion. Plusieurs matières premières (Résidu de maïs doux, Bagasse d’agave bleue, Résidu d’huilerie de palme, Paille d’orge, Résidu d’Eucalyptus, Sarments de vigne et Bagasse de canne à sucre) ont été caractérisées et leurs comportements vis-à-vis du procédé ont été comparés. L’évolution de la composition de ces matières à travers le procédé et leur hydrolysabilité ont été étudiées. Suite au traitement, une augmentation du rendement de saccharification dans un réacteur (24h de temps de réaction à 20% de consistance) a été obtenue pour ces matières (jusqu’à 85% des C6 théoriques et 70% des C5-C6 théoriques). Les rendements de fermentation non optimisés atteignent un maximum de 85% théorique des sucres C6 convertis, 65% théorique des C5-C6 convertis, et une concentration d’éthanol de 15g/100g extrudat sec. Le procédé de production d’éthanol dans son ensemble (avec addition de l’énergie de la valorisation des coproduits) atteint un ratio « énergie consommée/produite » de 0.5-0.6. Le nouveau procédé présente ainsi les avantages de minimiser la consommation d’énergie par l’application de faibles températures, de minimiser la consommation d’eau par l’utilisation de faibles ratios liquide/solide, de ne pas produire d’inhibiteurs de fermentation et d’être rapide, compact, continu et adaptable sur différentes biomasses. / Lignocellulosic biomass transformation processes in order to produce second generation bioethanol are actually widely studied all around the world but still not yet competitive compare to the first generation. The limiting key factors of the different processes are: the pre-treatment efficiency and costs, the enzymatic hydrolysis yields, and the co-fermentation C5-C6. A continuous plant matter deconstruction process, compacting a thermo-mechanico-chemical pre-treatment using alkali solution with an enzymes injection in twin-screw extruder, called bioextrusion, is developed in this study. It allows preparing the cellulosic material at a high dry matter content (>20%), to a possible simultaneous saccharification and fermentation (SSF). This continuous treatment may extract a big part of hemicelluloses (until 97%) and lignin (>50%) and configures cellulose to a better accessibility and a start of its depolymerisation by enzymes cocktail during the bioextrusion. Several raw matters (Sweet Corn Cob and Spathe, Blue Agave Bagass, Oil Palm Empty Fruit Bunch, Barley Straw, Eucalyptus Residue, Grape Pruning Residue and Sugarcane Bagass) have been characterized and theirs behaviours toward to the process were compared. Evolutions of these matters compositions throughout the process and their hydrolysability have been studied. Further to the treatment, an improvement of the saccharification yields in reactor (24h reaction time at 20% consistency) has been obtained on these matters (until 85% of theoretical C6 and 70% of theoretical C5-C6). The not optimized fermentation yields reach a maximum of 85% of theoretical converted C6 sugars, 65% of theoretical converted C5-C6 sugars, and an ethanol concentration of 15g/100g dry matter extrudate. The whole ethanol production process (with addition of energy from the recovery of the by-products) is achieved with a “consumed/produced energy” ratio of 0.5-0.6. The new process presents the advantages to minimize the energy consumption by operating low temperatures, to minimize water consumption by working at low liquid/solid ratio, to not produce fermentation ‘s inhibitors and to be quick, compact, continuous and adaptable to different biomasses.

L’incorporation de fibres végétales, différentes par leur origine, leur nature chimique et leur forme, a été effectuée dans deux matrices thermoplastiques : le poly(acide lactique) et la farine de blé thermoplastifiée. Ces deux matrices biodégradables et biosourcées ont elles aussi des natures chimiques et des propriétés thermo-mécaniques différentes. Des incorporations de fibres jusqu’à 40 % en poids ont permis de modifier considérablement les propriétés de base des matrices et d’améliorer certaines de leurs faiblesses (stabilité thermique, manque de rigidité…). Les fibres de miscanthus ont été sélectionnées comme étant les plus performantes pour l’amélioration des propriétés des deux matrices. Les propriétés des matériaux composites ont été ajustées par un travail sur la formulation du mélange (ajout de plastifiants) et l’optimisation du procédé complet, jusqu’au moulage par injection. L’incorporation des fibres dans un mélange compatibilisé des deux matrices a également été testée et réalisée en une seule étape d’extrusion, comprenant la plastification de la farine, le mélange des polymères et la dispersion des fibres. / Incorporation of vegetal fibres, differing by their source, their chemical composition and their shape, have been performed by twin screw extrusion in two thermoplastic matrices: the poly(lactic acid) and the thermoplastified wheat flour. These two biobased and biodegradable matrices have also different chemical character and thermo-mechanical properties. Fibre incorporation up to 40 % in weight considerably modified both matrix properties and improved several weaknesses (thermal stability, lack of stiffness…). Miscanthus fibres have been selected as best improvers for properties of both matrices. Materials properties were adjusted with a formulating work (addition of plasticizers) and whole process optimization, until injection-molding. Fibre incorporation in a compatibilized blend of the two matrices was also tested and performed in a one step extrusion process, including flour thermoplasticization, polymer blending and fibre dispersion.