A series of experiments was performed on groups of samples made from materials currently used to manufacture tooling for extruders to determine if the ASTM G65 dry sand rubber wheel abrasion test could be used as an accelerated test to evaluate candidate materials. Samples were tested in the heat treated condition and after surface modification by plasma ion nitriding. The range of materials tested included medium and high alloy steels and steel bonded carbide composites. The abrasives used were AFS 50/70 test sand and Dresser Glasgrain crushed fused silica. Evaluation of test wear scars and wear debris from the tests using AFS 50/70 showed that delamination was the primary wear mechanism for the composite materials, with some ploughing and microcutting, while ploughing and microcutting were the primary mechanisms in the wear of the steels. Evaluation of parts made from a composite material which were removed from service indicated that matrix erosion was the primary wear mechanism. Tests with Glasgrain fused silica as the abrasive yielded wear scars with the same morphology as the parts returned from service, but the very poor flow characteristics of this material caused inconsistency in the supply of this abrasive to the contact region. Interrupted tests showed that the wear rate was constant for the steels in the non-nitrided condition. After nitriding, the wear rate increased with test duration. The nitriding was found to act as a barrier coating providing an initial period of very low wear until the nitride layer is broached. The wear rate then increases to approximate the wear rate of the non-nitrided samples. It was found that the friction force alters the location of the maximum normal force, shifting the point of greatest contact force toward the entry end of the wear scar. / Master of Science

Yes / Recycling of polymers is a necessity in our intensively consuming polymer world but the nature of polymers is such that they are prone to thermal degradation when re-extruded and this poses technical challenges to recycling. This article describes research that seeks to rebuild the structure of degraded PA6. We present data from controlled experiments with pristine pPA6 extruded to form a base recycle rPA6 to which we added two chain extenders, separately: one with anhydride multifunctionality (ANHY), highly reactive with amide groups and one with epoxy multifunctionality (EPOX), less reactive. We found from rheological data carried out in the linear viscoelastic region (so as to study structural changes) a striking difference in the ability of the chain extenders to rebuild structure: 306% increase in the complex viscosity of rPA6/ANHY compared to 25% in that of rPA6/EPOX of the base rPA6. Mechanical and thermal (DSC and TGA) tests confirmed the superior efficacy of the multifunctional anhydride chain extender. Beside the practical benefit that ensues from this research, it also provides a strategic platform to develop chain extenders for other degrading polymers on the basis of understanding the degradation chemical reaction and targeting the most reactive end group of the split chains.

No / The aims of the present work were to pelletize talc by extrusion-spheronization technique using microcrystalline cellulose (MCC) as a pelletization aid and to study its performance as a neutral substrate for coating. A 32 factorial design was used to study the effect of independent variables (X1, amount of talc, and X2, MCC) on pellet properties.

No / Mechanochemical synthesis, i.e., reactions conducted by grinding solid reactants together with no or minimal solvent, has been demonstrated as an excellent technique for the formation of both organic and inorganic compounds. Mechanochemistry is viewed as an alternative approach to chemical synthesis and is not always considered when developing manufacturing processes of fine chemicals. Here, recent advances are highlighted regarding mechanochemical synthesis, by utilizing a well‐developed continuous technique – extrusion, and the advantages it offers to further support its use in the manufacturing of these chemicals. To put this work into context, it is shown how extrusion plays a vital role for manufacturing in the food, polymer, and pharmaceutical industries, and how the research carried out by these respective industrialists provides great insight and understanding of the technique, with the results being applicable in the chemical industry. The synthesis of metal–organic frameworks (MOFs) is highlighted herein as an excellent example showcasing the advantages that extrusion provides to the manufacture of these materials, one advantage being the exceptional space time yields (STYs) reported for these processes, at three orders of magnitude greater than conventional (solvothermal) synthesis. / EPSRC. Grant Number: EP/L019655/1

No / An infrared temperature sensor has been used to provide real time quantification of the thermal homogeneity of polymer extrusion. The non-intrusive sensor was located in the barrel of a single screw extruder, positioned such that it provided a measurement of melt temperature in the channel of the metering section of the extruder screw. The rapid response of the technique enabled melt temperature within the extruder screw channel to be monitored in real time, allowing quantification of the thermal stability of the extrusion process. Two polyethylenes were used in experiments with three extruder screw geometries at a range of screw speeds. Data generated by the infrared sensor was found to be highly sensitive to thermal fluctuations relating to the melting performance of the extruder screw. Comparisons made with an intrusive thermocouple grid sensor located in the extruder die suggested that the infrared technique was able to provide a similar level of information without disturbing the process flow. This application on infrared thermometry could prove highly useful for industrial extrusion process monitoring and optimization.

Yes / In this work, a highly instrumented single screw extruder has been used to study the effect of polymer rheology on the thermal efficiency of the extrusion process. Three different molecular weight grades of high density polyethylene (HDPE) were extruded at a range of conditions. Three geometries of extruder screws were used at several set temperatures and screw rotation speeds. The extruder was equipped with real-time quantification of energy consumption; thermal dynamics of the process were examined using thermocouple grid sensors at the entrance to the die. Results showed that polymer rheology had a significant effect on process energy consumption and thermal homogeneity of the melt. Highest specific energy consumption and poorest homogeneity was observed for the highest viscosity grade of HDPE. Extruder screw geometry, set extrusion temperature and screw rotation speed were also found to have a direct effect on energy consumption and melt consistency. In particular, specific energy consumption was lower using a barrier flighted screw compared to single flighted screws at the same set conditions. These results highlight the complex nature of extrusion thermal dynamics and provide evidence that rheological properties of the polymer can significantly influence the thermal efficiency of the process. (C) 2014 The Authors. Published by Elsevier B.V. All rights reserved.

Yes / Hot melt extrusion has been used to produce a solid dispersion of the thermolabile drug artemisinin. Formulation and process conditions were optimised prior to evaluation of dissolution and biopharmaceutical performance. Soluplus®, a low Tg amphiphilic polymer especially designed for solid dispersions enabled melt extrusion at 110ºC although some drug-polymer incompatibility was observed. Addition of 5% citric acid as a pH modifier was found to suppress the degradation. The area under plasma concentration time curve (AUC0-24hr) and peak plasma concentration (Cmax) were four times higher for the modified solid dispersion compared to that of pure artemisinin. / EPSRC grant no (EP/J003360/1) and UKIERI: UK-India Education and Research Initiative (TPR 26).

Avec les émissions de gaz à effet de serre contribuant aux changements climatiques, les technologies de capture du CO₂ commencent à gagner en intérêt. Les contacteurs à membranes sont une alternative prometteuse aux contacteurs conventionnels pour l'absorption gaz-liquide du CO₂, permettant d'éviter les complications liées à la dispersion des phases tout en bénéficiant d'une modularité, d'un contrôle indépendant des débits de liquide et de gaz et d'une surface de contact plus élevée. Les deux inconvénients majeurs des contacteurs à membranes incluent l'usage de solvants coûteux et toxiques lors de la fabrication des membranes, ainsi que le potentiel de mouillage qui interfère avec l'absorption en augmentant la résistance au transfert de matière. Afin de remédier à ces deux obstacles, une méthode d'extrusion par fusion avec lessivage de sel a été développée dans notre groupe de recherche pour la fabrication de membranes à fibres creuses microporeuses hydrophobes, n'utilisant que du sel et de l'eau pour la formation des pores tout en générant une surface rugueuse et hydrophobe. L'objectif principal de ce projet est d'investiguer l'application de ce procédé d'extrusion par fusion avec lessivage de sel pour la fabrication de membranes planes. Les membranes ont été extrudées sous différentes conditions, en variant le type de polymère, la teneur en sel à l'alimentation, la méthode de d'alimentation, la méthode de figeage, la vitesse de rotation des vis et la vitesse de tirage à la sortie de l'extrudeuse. Lors de la fabrication des membranes, le contrôle de la structure poreuse est un défi important car le sel peut être sujet à des agglomérations. Toutefois, le cisaillement par la rotation des vis lors de l'extrusion et la désagglomération du sel par broyage peuvent aider à limiter les irrégularités dans la structure poreuse. Due à l'ajustabilité limitée de la filière utilisée pour l'extrusion, l'épaisseur des membranes a dû être ajustée en étirant les membranes à la sortie de l'extrudeuse, ce qui a comme effet secondaire d'altérer les propriétés de surface, menant à des angles de contact(105 à 115°) et des rugosités moyennes (20 à 150 nm) plus faibles que prévu. Par conséquent, l'usage d'une filière adaptée pour l'extrusion à des épaisseurs inférieures à 0,2 mm est recommandé pour la suite des travaux afin d'obtenir des membranes plates aux épaisseurs voulues et sans détériorer les propriétés de surfaces.

Cette thèse vise à la production de poudre de polymère par un procédé continu, en une seule étape et supprimant l'utilisation des solvants organiques en faveur de celle du CO2 supercritique. Avant de développer le procédé, une caractérisation du mélange CO2/polymère a été effectuée. Des mesures de solubilité, de gonflement et de coefficient de diffusion du CO2 ont été réalisées et représentées par différents modèles. De plus, une technique de rhéologie capillaire en ligne a été développée, permettant la mesure de viscosité du polymère, seul ou en mélange, avec le CO2 dans les conditions du procédé. Un montage batch a ensuite permis de tester l'influence des paramètres opératoires sur de faibles quantités. Parallèlement, le procédé continu a été étudié sur une extrudeuse équipée d'outils de mélange du CO2 dans le polymère fondu. L'efficacité et l'homogénéité du mélange ont été étudiées à travers la fabrication de mousses de polymères et la réalisation de distributions de temps de séjour par spectroscopie Raman en ligne. L'ajout d'un dispositif de pulvérisation spécifique a conduit à l'obtention de poudres d'aspect fibreux avec deux populations de tailles. / Polymer powders are widely used in industry and are traditionally manufactured by processes using organic solvent or by grinding low molecular weight polymers with a post-polymerization step. This thesis aimss at the generation of polymer powders with a single-step continuous process, based on the use of supercritical CO2, hence without organic solvent. Before developing this process, the characterization of the mixture CO2/polymer was done. Solubility measurements were carried out and fitted with the Sanchez-Lacombe equation of state. Moreover, a capillary rheometry technique was implemented on-line, allowing the measurement of the viscosity of the polymer alone or in mixture with CO2, under process conditions. The modeling of swelling as a function of time led to the evaluation of the diffusion coefficient of CO2 into the polymer. Afterwards, two experimental devices were designed. A batch process with a pressurized autoclave was used to determine the influence of experimental parameters on powder production, with small amounts of material. Formation of small fibrous particles was obtained. In parallel, the continuous process was studied on an extruder adapted to CO2 introduction and equipped with mixing devices. This study, which led to foam manufacture, was used to evaluate efficiency and homogeneity of the mixing. Residence time distributions were determined by Raman spectroscopy on the die in order to evaluate the flowing in the extruder under different conditions. The equipment was also fitted with a specific nozzle allowing co-injection of hot air. Production of fibrous particles with two different size ranges was obtained.

L'objectif de ce travail est d'étudier la faisabilité d'ajout de sel nylon à un polyamide (PA) par un procédé d’extrusion réactive. Dans ce cadre, l'ajout de sel 6T comprenant des motifs aromatiques à du PA 66 est réalisé dans le but de synthétiser du PA 66/6T. En effet, ce dernier répond à la demande actuelle en polymères à haute résistance thermique. Le taux d'avancement de la réaction et le taux de motifs 6T insérés doivent dès lors être maximisés.Le travail comprend les synthèses et les analyses du sel 6T, du PA 6T et du PA 66/6T. Le sel 6T est produit puisqu'il n'est pas commercialisé. Le PA 6T est synthétisé pour permettre l’identification des hydrogènes aromatiques du PA 66/6T. Le travail sur ce dernier nécessite la mise au point et l'étude du procédé d'extrusion. Pour ce faire, les influences d'un certain nombre de paramètres opératoires sont étudiées comme, par exemple, le niveau de vide sur les évents de l'extrudeuse.Les meilleures conditions opératoires du procédé permettent d’obtenir un taux d'avancement de 93 mol% et un taux d'insertion de motifs 6T de 15,3 mol%. Néanmoins, le PA 66/6T produit présente un fort excès de fonctions terminales acides / The aim of this work is to study the feasibility of addition of nylon salt to polyamide (PA) by a reactive extrusion process. As example, the addition of 6T salt, which includes aromatic monomers, to PA 66 is performed in order to synthesize PA 66/6T. This latter replies to demand of high resistance temperature polymer. Consequently, the progress rate of the reaction and the rate of 6T motifs insertion have to be maximized.This work includes the synthesis and the analysis of 6T salt, PA 6T and PA 66/6T. 6T salt synthesis is performed since it is not commercialised. PA 6T is synthesized in order to identify aromatic hydrogen in PA 66/6T molecule. About this latter, it is necessary to adjust and to study the extrusion process. So, the influences of few process parameters are studied as, for example, pressure level on vent gas of the extruder.With the best process parameters, the progress rate is 93 mol% and the rate of 6T motifs insertion is 15,3 mol%. Yet, PA 66/6T presents a significant excess of acidic end group