No / Extrusion is one of the major methods for processing polymeric materials and the thermal homogeneity of the process output is a major concern for manufacture of high quality extruded products. Therefore, accurate process thermal monitoring and control are important for product quality control. However, most industrial extruders use single point thermocouples for the temperature monitoring/control although their measurements are highly affected by the barrel metal wall temperature. Currently, no industrially established thermal profile measurement technique is available. Furthermore, it has been shown that the melt temperature changes considerably with the die radial position and hence point/bulk measurements are not sufficient for monitoring and control of the temperature across the melt flow. The majority of process thermal control methods are based on linear models which are not capable of dealing with process nonlinearities. In this work, the die melt temperature profile of a single screw extruder was monitored by a thermocouple mesh technique. The data obtained was used to develop a novel approach of modelling the extruder die melt temperature profile under dynamic conditions (i.e. for predicting the die melt temperature profile in real-time). These newly proposed models were in good agreement with the measured unseen data. They were then used to explore the effects of process settings, material and screw geometry on the die melt temperature profile. The results showed that the process thermal homogeneity was affected in a complex manner by changing the process settings, screw geometry and material. (C) 2013 Elsevier Inc. All rights reserved.

Yes / Polymer extrusion, in which a polymer is melted and conveyed to a mould or die, forms the basis of most polymer processing techniques. Extruders frequently run at non-optimised conditions and can account for 15-20% of overall process energy losses. In times of increasing energy efficiency such losses are a major concern for the industry. Product quality, which depends on the homogeneity and stability of the melt flow which in turn depends on melt temperature and screw speed, is also an issue of concern of processors. Gear pumps can be used to improve the stability of the production line, but the cost is usually high. Likewise it is possible to introduce energy meters but they also add to the capital cost of the machine. Advanced control incorporating soft sensing capabilities offers opportunities to this industry to improve both quality and energy efficiency. Due to strong correlations between the critical variables, such as the melt temperature and melt pressure, traditional decentralized PID (Proportional-Integral-Derivative) control is incapable of handling such processes if stricter product specifications are imposed or the material is changed from one batch to another. In this paper, new real-time energy monitoring methods have been introduced without the need to install power meters or develop data-driven models. The effects of process settings on energy efficiency and melt quality are then studied based on developed monitoring methods. Process variables include barrel heating temperature, water cooling temperature, and screw speed. Finally, a fuzzy logic controller is developed for a single screw extruder to achieve high melt quality. The resultant performance of the developed controller has shown it to be a satisfactory alternative to the expensive gear pump. Energy efficiency of the extruder can further be achieved by optimising the temperature settings. Experimental results from open-loop control and fuzzy control on a Killion 25 mm single screw extruder are presented to confirm the efficacy of the proposed approach. (C) 2013 Elsevier Ltd. All rights reserved.

Blends of poly butylene terephthalate (PBT) and polycarbonate (PC) form a very important class of commercial blends in numerous applications requiring materials with good chemical resistance, impact resistance even at low temperatures, and aesthetic and flow characteristics. PC and PBT are usually blended in a twin screw extruder (TSE). Product melt volume flow rate (MVR) is a property used to monitor product quality while blending the PC/PBT in a twin screw extruder. It is usually measured off line in a quality control laboratory using extrusion plastometer on samples collected discretely during the compounding operation. Typically a target value representing the desired value of the quality characteristics for an in-control process, along with upper and lower control limits are specified. As long as the MVR measurement is within the control limits, the sample is approved and the whole compounded blend is assumed to meet the specification. Otherwise, the blend is rejected. Because of infrequent discrete sampling, corrective actions are usually applied with delay, thus resulting in wasted material. It is important that the produced PC/PBT blend pellets have consistent properties. Variability and fault usually arise from three sources: human errors, feed material variability, and machine operation (i.e. steady state variation). Among these, the latter two are the major ones affecting product quality. The resulting variation in resin properties contributes to increased waste products, larger production cost and dissatisfied customers. Motivated by this, the objective of this project was to study the compounding operation of PC/PBT blend in a twin screw extruder and to develop a feasible methodology that can be applied on-line for monitoring properties of blends on industrial compounding operations employing available extruder input and output variables such as screw speed, material flow rate, die pressure and torque. To achieve this objective, a physics-based model for a twin screw extruder along with a MVR model were developed, examined and adapted for this study, and verified through designed experiments. This dynamic model for a TSE captures the important dynamics, and relates measurable process variables (screw speed, torque, feed rates, pressure etc.) to ones that are not being measured (material holdups and compositions at the partially and filled section along a TSE barrel). This model also provides product quality sensors or inferential estimation techniques for prediction of viscosity and accordingly MVR. The usefulness of the model for inferential MVR sensing and fault diagnosis was demonstrated on experiments performed on a 58 mm co-rotating twin-screw extruder for an industrial compounding operation at a SABIC Innovative Plastics plant involving polycarbonate – poly butylene terephthalate blends. The results showed that the model has the capability of identifying faults (i.e., process deviation from the nominal conditions) in polymer compounding operations with the twin screw extruder. For instance, the die pressure exhibited a change as a function of changes in raw materials and feed composition of PC and PBT. In the presence of deviations from nominal conditions, the die pressure parameters are updated. These die pressure model parameters were identified and updated using the recursive parameter estimation method. The recursive identification of the die pressure parameters was able to capture very well the effects of changes in raw material and/or composition on the die pressure. In addition, the developed MVR model showed a good ability in monitoring product MVR on-line and inferentially from output process variables such as die pressure which enables quick quality control to maintain products within specification limits and to minimize waste production.

In this work, the compounding of polycarbonate (PC) / poly-butylene terephthalate (PBT) blends was studied for the purpose of improving quality of products with reduced wastage and finally to satisfaction of end users. The effect of material rheological characteristics and processing conditions on compounding of PC /PBT was investigated through statistical experiments carried out on a 58 mm twin-screw extruder at SABIC Innovative Plastics Limited (formerly GE Plastics Limited) in Cobourg, Ontario. Melt Volume-Flow Rate (MVR) is the most commonly used property to monitor the quality of products of PC/PBT blends. The MVR was studied with different sampling times and correlations between product properties (melt flow) and processing conditions (screw speed, flow rates) were discussed. The rheological behavior of PC/PBT blends was investigated by dynamic and capillary rheometers. The effects of processing conditions (screw speed, feed rate) on viscosity were measured and it was found that the Cox-Merz rule is not valid for PC/PBT blends. The change of morphology of PC/PBT blends was observed under a scanning electron microscope (SEM) by using different types of samples. Those samples were (i) PC/PBT blends pellets, (ii) PC/PBT blend samples, but collected after completing the rheological tests in the parallel plate rheometer, and (iii) PC/PBT blend samples, but collected after completing the rheological tests in the capillary rheometer. There was evidence that the samples collected after completing the tests in the parallel and capillary rheometer might be degraded due to temperature and time.

Blends of poly butylene terephthalate (PBT) and polycarbonate (PC) form a very important class of commercial blends in numerous applications requiring materials with good chemical resistance, impact resistance even at low temperatures, and aesthetic and flow characteristics. PC and PBT are usually blended in a twin screw extruder (TSE). Product melt volume flow rate (MVR) is a property used to monitor product quality while blending the PC/PBT in a twin screw extruder. It is usually measured off line in a quality control laboratory using extrusion plastometer on samples collected discretely during the compounding operation. Typically a target value representing the desired value of the quality characteristics for an in-control process, along with upper and lower control limits are specified. As long as the MVR measurement is within the control limits, the sample is approved and the whole compounded blend is assumed to meet the specification. Otherwise, the blend is rejected. Because of infrequent discrete sampling, corrective actions are usually applied with delay, thus resulting in wasted material. It is important that the produced PC/PBT blend pellets have consistent properties. Variability and fault usually arise from three sources: human errors, feed material variability, and machine operation (i.e. steady state variation). Among these, the latter two are the major ones affecting product quality. The resulting variation in resin properties contributes to increased waste products, larger production cost and dissatisfied customers. Motivated by this, the objective of this project was to study the compounding operation of PC/PBT blend in a twin screw extruder and to develop a feasible methodology that can be applied on-line for monitoring properties of blends on industrial compounding operations employing available extruder input and output variables such as screw speed, material flow rate, die pressure and torque. To achieve this objective, a physics-based model for a twin screw extruder along with a MVR model were developed, examined and adapted for this study, and verified through designed experiments. This dynamic model for a TSE captures the important dynamics, and relates measurable process variables (screw speed, torque, feed rates, pressure etc.) to ones that are not being measured (material holdups and compositions at the partially and filled section along a TSE barrel). This model also provides product quality sensors or inferential estimation techniques for prediction of viscosity and accordingly MVR. The usefulness of the model for inferential MVR sensing and fault diagnosis was demonstrated on experiments performed on a 58 mm co-rotating twin-screw extruder for an industrial compounding operation at a SABIC Innovative Plastics plant involving polycarbonate – poly butylene terephthalate blends. The results showed that the model has the capability of identifying faults (i.e., process deviation from the nominal conditions) in polymer compounding operations with the twin screw extruder. For instance, the die pressure exhibited a change as a function of changes in raw materials and feed composition of PC and PBT. In the presence of deviations from nominal conditions, the die pressure parameters are updated. These die pressure model parameters were identified and updated using the recursive parameter estimation method. The recursive identification of the die pressure parameters was able to capture very well the effects of changes in raw material and/or composition on the die pressure. In addition, the developed MVR model showed a good ability in monitoring product MVR on-line and inferentially from output process variables such as die pressure which enables quick quality control to maintain products within specification limits and to minimize waste production.

In this work, the compounding of polycarbonate (PC) / poly-butylene terephthalate (PBT) blends was studied for the purpose of improving quality of products with reduced wastage and finally to satisfaction of end users. The effect of material rheological characteristics and processing conditions on compounding of PC /PBT was investigated through statistical experiments carried out on a 58 mm twin-screw extruder at SABIC Innovative Plastics Limited (formerly GE Plastics Limited) in Cobourg, Ontario. Melt Volume-Flow Rate (MVR) is the most commonly used property to monitor the quality of products of PC/PBT blends. The MVR was studied with different sampling times and correlations between product properties (melt flow) and processing conditions (screw speed, flow rates) were discussed. The rheological behavior of PC/PBT blends was investigated by dynamic and capillary rheometers. The effects of processing conditions (screw speed, feed rate) on viscosity were measured and it was found that the Cox-Merz rule is not valid for PC/PBT blends. The change of morphology of PC/PBT blends was observed under a scanning electron microscope (SEM) by using different types of samples. Those samples were (i) PC/PBT blends pellets, (ii) PC/PBT blend samples, but collected after completing the rheological tests in the parallel plate rheometer, and (iii) PC/PBT blend samples, but collected after completing the rheological tests in the capillary rheometer. There was evidence that the samples collected after completing the tests in the parallel and capillary rheometer might be degraded due to temperature and time.

Das Ziel dieser Arbeit bestand in der Erarbeitung von Verfahrenskonzepten zur stofflichen Nutzung von Fichtenrinde und im Nachweis deren technischer Realisierbarkeit. Dabei wurden drei Verfahrensvarianten zur Herstellung eines festen Rindenwerkstoffes mit guter Dämmwirkung, einem schüttfähigen Dämmstoff in Form von Pellets und Granulaten und einem Werkstoff mit hoher Festigkeit und Oberflächengüte erarbeitet. Zu Beginn der Arbeit wurden Qualitätsziele der Produktkennwerte formuliert, die für Rindenprodukte bisher nicht erreichbar waren. Diese sollten trotz der Maßgabe, auf synthetische Bindemittel zu verzichten, erreicht werden. Die konsequente Anwendung verfahrenstechnischer Grundoperationen mit bewährten Apparaten, erweitert durch ein neues System aus Heizung und Kühlung während der Pressverdichtung, ermöglichten das Erreichen und zum Teil Übertreffen der geforderten Qualitätsziele. Die technische, aber auch wirtschaftliche Umsetzung ist möglich.

Le mélange de polymères est une méthode répandue pour élaborer des matériaux polymères. Cependant, la plupart des polymères sont thermodynamiquement immiscibles entre eux, engendrant une séparation de phase des mélanges et une détérioration de leurs propriétés. Afin de palier ces problèmes, la méthode dite compatibilisation réactive est souvent employée. Elle est basée sur la formation in-situ de copolymères à bloc ou greffés par l’intermédiaire de réactions interfaciales entre polymères réactifs. Cette thèse a pour objet de développer un concept dit agent compatibilisant-traceur réactif qui permettra d’utiliser de faibles quantités d’agents compatibilisants réactifs pour évaluer leurs efficacités de compatibilisation directement sur des extrudeuses bi-vis industrielles, d’une part ; et de caractériser la performance du mélange d’une extrudeuse bi-vis en fonction des conditions opératoires et/ou du profil de vis employé. Ses principales contributions se résument ci-après. L’anthracène de 9-méthylaminométhyle (MAMA), une molécule fluorescente, est incorporée dans un copolymère statistique de styrène (St) et d’isocyanate de 3-isopropenyle-?, ?’-diméthylebenzène (TMI), noté PS-TMI, pour former un agent compatibilisant-traceur réactif, noté PS-TMI-MAMA. Ce dernier sert à la fois comme agent compatibilisant réactif grâce aux groupements isocyanate et traceur grâce aux groupements fluorescents. Il est utilisé pour les mélanges à base de polystyrène (PS) et de polyamide 6 (PA6) afin d’évaluer son efficacité de compatibilisation. Les mélanges PS/PA6 sont élaborés dans un mélangeur discontinu et une extrudeuse bi-vis, respectivement. Dans le cas du mélangeur discontinu, la quantité du copolymère greffé formé in-situ, noté PS-g-PA6-MAMA, augmente alors que le diamètre des domaines de la phase dispersée (DDD) diminue considérablement au début du mélange. Lorsque le mélange se poursuit, le nombre de greffons en PA6 du PS-g-PA6-MAMA augmente, engendrant une composition très asymétrique du PS-g-PA6-MAMA qui est thermodynamiquement instable aux interfaces. De ce fait, il peut être arraché des interfaces vers la phase PA6 et peut y former des micelles. Lorsqu’il est arraché des interfaces, il perdra son efficacité de compatibilisation et le DDD augmentera. L’action du mélange a un double effet sur le procédé de compatibilisation réactive. Il promeut la réaction interfaciale entre le PS-TMI-MAMA et le PA6, d’une part ; et aggrave l’arrachage du PS-g-PA6-MAMA de l’interface, d’autre part. L’utilisation de faibles quantités de l’agent compatibilisant-traceur réactif permet de mesurer les évolutions de la teneur en agent compatibilisant-traceur réactif, du DDD et de la teneur en agent compatibilisant-traceur réactif ayant réagi en fonction du temps de séjour dans une extrudeuse bi-vis. Pour une masse molaire donnée, l’efficacité de compatibilisation d’un agent compatibilisant-traceur réactif augmente avec l’augmentation de la teneur en TMI dans une certaine limite. Pour une teneur en TMI donnée, la réaction interfaciale est plus rapide avec la diminution de la masse molaire dans une certaine limite et le DDD devient plus petit en un temps plus court. L’influence du taux de remplissage de la vis est plus significative que celle du temps de séjour. Lorsque le taux de remplissage de la vis augmente, le taux de la réaction interfaciale augmente et le DDD diminue. Lorsque l’angle d’un élément de mélange augmente, les efficacités du mélange distributif et du mélange dispersif augmentent, ce qui se traduit par une augmentation de la quantité du PS-g-PA6-MAMA formée et une diminution du DDD par rapport à la même quantité de PS-g-PA6-MAMA produite. Lorsque la largeur d’un élément de mélange augmente, l’efficacité du mélange distributive augmente alors que celle du mélange dispersif demeure inchangée. La substitution d’éléments de mélange par des éléments inverses améliore l’efficacité du mélange distributif et celle du mélange dispersif / Polymer blending is a common method to prepare high-performance polymer materials. However, most polymer pairs are thermodynamically immiscible, leading to phase separation and deterioration in material properties. To overcome such problems, the most common method is reactive compatibilization which is based on the in-situ formation of a graft or block copolymer by interfacial reaction between reactive polymers. This thesis aims at developing a concept of reactive compatibilizer-tracer which will allow using small amounts of reactive compatibilizers to evaluate their compatibilizing efficiency in industrial scale twin screw extruders, on the one hand; and to characterize the mixing performance of a twin screw extruder as a function of process conditions and/or screw profile. Its main contributions are summarized below. 9-(methylaminomethyl) anthracene (MAMA), a fluorescent molecule, is incorporated into a random copolymer of styrene (St) and 3-isopropenyl-?, ?’-dimethylbenzene isocyanate (TMI), denoted as PS-TMI, to form a reactive compatibilizer-tracer, denoted as PS- TMI-MAMA. The latter serves both as a reactive compatibilizer due to its isocyanate moieties and a tracer due to its fluorescent moieites. It is used for polystyrene (PS)/polyamide 6 (PA6) blends to evaluate its compatibilizing efficiency. Compatibilized PS/PA6 blends are processed in a batch mixer and in a twin screw extruder, respectively. In the case of the batch mixer, the amount of the in-situ formed graft copolymer denoted as PS-g-PA6-MAMA increases and the dispersed phase domain diameter (DDD) decreases drastically in the initial period of mixing. As the mixing further proceeds, the number of PA6 grafts of the PS-g-PA6-MAMA increases, resulting in a highly asymmetrical composition of the PS-g-PA6-MAMA which causes thermodynamic instablility at the interface. As a result, it could be pulled out of the interface to the PA6 phase and form micelles. Once it is pulled out of the interface, it will lose its compatibilizing efficiency and the dispersed phase domain diameter increases sharply. Mixing has a dual effect on the reactive compatibilization process. On the one hand, it promotes the interfacial reaction between the PS-TMI-MAMA and PA6. On the other hand, it aggravates the pull out of the resulting PS-g-PA6-MAMA from the interface. The use of small amounts of the reactive compatibilizer-tracer together with transient experiments for RTD allows assessing the evolutions of the reactive compatibilizer-tracer content (CC), the dispersed phase domain diameter (DDD), and the reacted reactive compatibilizer-tracer content (RCC) as a function of residence time in a twin-screw extruder. Based on the above results, the emulsification curve (DDD vs. CC), the RCC vs. CC curve and effective emulsification curve (DDD vs. RCC) are obtained. When the molar mass of the reactive compatibilizer-tracer is fixed, its compatibilizing efficiency increases with increasing TMI content within an appropriate range. When its TMI content is fixed, the interfacial reaction goes faster as the molar mass of the reactive compatibilizer-tracer decreases within a certain range, and the DDD becomes smaller in a shorter time. The effect of degree of fill fixed by the throughput Q/screw speed N ratio is more dominant than that of residence time. As the degree of fill increases, the interfacial reaction increases and the DDD decreases. As the angle of adjacent the kneading block increases, its distributive and dispersive mixing efficiencies increase, resulting in an increase in interfacial area generation and a decrease in DDD on the basis of the same amount of PS-g-PA6-MAMA. On the other hand, as the width of the kneading block increases, the distributive mixing efficiency increases and the dispersive mixing efficiency remains unchanged. Substitution of kneading blocks by reverse ones increase both the distributive and dispersive mixing efficiencies

Les apiaceae peuvent être définies en tant qu' Aroma-Tincto-Oleo-Crop (ATOC), plantes qui contiennent à la fois une huile végétale et une huile essentielle. Appliquer le concept d'agroraffinage aux ATOC revient à proposer un procédé séquentiel alliant une co-extraction huile végétale et huile essentielle à une valorisation des résidus en tant que source de molécules biosourcées et de susbtrat pour la formulation d'agromatériaux . Les objectifs de cette thèse seront donc d'étudier la faisabilité biologique et technologique d'application du concept d'ATOC-raffinage à la coriandre (Coriandrum sativum L.). Le chapitre I présente l'état de l'art bibliographique sur l'extraction et l'analyse des huiles végétales et huiles essentielles de coriandre tandis que dans le chapitre II sont décrits les matériels et méthodes mis en oeuvre au cours de la thèse tant au niveau échantillonnage, extraction, analyse que traitement des données. Le chapitre III est centré sur l'étude des différents paramètres biologiques pouvant influencer la bioaccumulation des huiles végétales et huiles essentielles dans la coriandre (différentes variétés, différents organes de la plante, différents stades de développement biologique) et leur impact sur l'activité anti-oxydante des extraits obtenus à partir des résidus d'extraction. Dans le chapitre IV, la technologie d'extrusion (mono-vis et bi-vis) a été appliquée aux graines de coriandre dans le but d’évaluer la faisabilité du pressage mécanique du fruit de la coriandre pour l’extraction d'une huile végétale aromatisée. L’influence des conditions expérimentales sur le rendement d'extraction en huile végétale (diamètre de buse et distance buse-vis (extrudeur mono-vis) ou configuration de vis, coefficient de remplissage et température de pressage (extrudeur bi-vis)) a été étudiée tandis que la faisabilité de la valorisation du résidu solide d'extraction en agromatériaux (thermo-pressage) a été montrée. / Apiaceae could be defined as Aroma Tincto Oleo Crops (ATOC), e.g. plants containing both vegetable oil and essential oil. Applying agroreffinery concept to ATOC led to propose a sequential fractionation process coupling co-extraction of vegetal oil and essential oil to a valorization of by-product residues as biosourced active molecules and substrates for designing agromaterials. The aim of this thesis is to determine the biological and technological feasability of application of the ATOC-refinery concept to coriander (Coriandrum sativum L.) Chapter I reports a bibliographic state of the art study on extraction and characterisation of coriander vegetal oil and essential oil while chapter II describes materials and methods setting up during the thesis for sampling, extraction, analysis and data processing. Chapter III focus on the study of major various biological parameters influencing bioaccumulation of vegetal oil and essential oil in coriander (different plant varieties, different plant organs, different biological stages) and their impact on anti-oxidant activity of extracts obtained from extraction residues. In chapter IV, coriander fruits are processed by extrusion technology (mono screw and twin-screw extruder) in order to evaluate the feasability of mechanical pressing for extracting a flavored vegetal oil. Influence of operating parameters on vegetal oil extraction yields (nozzle diameter and nozzle/screw distance (single-screw extruder) or screw configuration, device’s filling coefficient and pressing temperature (twin-screw extruder)) is studied while the feasability of valorization of extraction cake as agromaterial (thermopressing) was stated.

Thesis is dealing with the creation of robotic worplace and its periphery. The paper is discrabing the robotic function and kinematics. The practical part of the paper shows several types of suggested robotic workplaces followed by solution processing of one selected type, where technical documentation and the calculation of production is made. The end of the paper shows economical and technological evaluation of the selected type of workplace including the price returns.