In this work, the peroxide-initiated degradation of polypropylene (PP) in co-rotating intermeshing twin-screw extruders (COITSEs) is analyzed by means of numerical simulations. This reactive extrusion (REX) operation is simulated by implementing (i) a one-dimensional and (ii) a three-dimensional (3D) modeling approach. In the case of the 1D modeling, a REX mathematical model previously developed and implemented as a computer code is used for the evaluation of two scale-up rules for COITSEs of various sizes. The first scale-up rule which is proposed in this work is based on the concept of thermal time introduced by Nauman (1977), and the second one is based on specific energy consumption (SEC) requirements. The processing parameters used in testing the previously referred to scale-up approaches are the mass throughput, the screw rotating speed, and the peroxide concentration, whereas the extruder screw configuration and the barrel temperature profiles are kept constant. The results for the simulated operating conditions show that when the REX operation is scaled-up under constant thermal time, very good agreement is obtained between the weight-average molecular weight (Mw) and poly-dispersity index (PDI) from the larger extruders and the values of these parameters corresponding to the reference extruder. For the constant SEC approach, on the other hand, more significant variations are observed for both of the aforementioned parameters. In the case of the implemented constant thermal time procedure, a further analysis of the effect of the mass throughput and screw speed of the reference device on the scaled-up operation is performed. It is observed that when the lower mass throughput is implemented for the smaller extruder keeping a constant screw speed, the predicted residence times of extrusion for the larger extruders are lower, in general terms, than those corresponding to the reference device, and a converse situation occurs for the higher implemented value of the mass throughput. Also, in general terms, the higher increase of the reaction temperature on the scaled-up operation corresponds to the lower mass throughputs and higher screw speeds specified for the reference extruder. For the 3D modeling approach, two different case studies are analyzed by means of a commercial FEM software package. The REX simulations are performed under the assumption of steady-state conditions using the concept of a moving relative system (MRS). To complement the information obtained from the MRS calculations, simulations for selected conditions (for non-reactive cases) are performed considering the more realistic transient-state (TS) flow conditions. The TS flow conditions are associated to the time periodicity of the flow field inside the conveying elements of COITSEs. In the first case study, the peroxide-initiated degradation of PP is simulated in fully-filled screw elements of two different size COITSEs in order to evaluate scale-up implications of the REX operation. In the second case, the reacting flow is simulated for a conventional conveying screw element and a conveying screw element having a special design and corresponding to the same extruder size. For both of the analyzed cases, the effects of the initial peroxide concentration and mass throughput on the final Mw and PDI of the degraded resin are studied. The effect of the processing conditions is discussed in terms of the residence time distribution (RTD), the temperature of reaction, and the distributive mixing capabilities of the REX system. When analyzing the scale-up case, it is found that for the implemented processing conditions, the final Mws and PDIs are very close to each other in both of the analyzed flow geometries when the specified flow is close to that corresponding to the maximum conveying capabilities of the screw elements. For more restrictive flow conditions, the final Mws and PDIs are lower in the case of the screw element of the larger extruder. It is found that the distributive mixing ability of the reactive flow is mainly related to the specified mass throughput and almost independent of the specified peroxide concentration for a particular extruder size. For the analyzed screw elements, the conveying element corresponding to the small size extruder shows a slightly better distributive mixing performance. For this same case study, a further evaluation of the proposed scale-up criterion under constant thermal time confirms the trend of the results observed for the 1D simulations. In the second case study, the special type of screw element consists of screws rotating at different speeds which have different cross sections. In this case, the outer and inner diameters of both the special and the conventional type of screw elements are specified to be the same. As in the previous case study, the distributive mixing capabilities appear to be independent of the specified peroxide concentrations but dependent on the mass flow rate. It is speculated from the simulation results, from both the transient- as well as the steady-state flow conditions, that the screw element with the special design would yield lower final values of the PDI and Mw. Also, this screw element appears to have improved distributive mixing capabilities as well as a wider RTD.

In this work, the peroxide-initiated degradation of polypropylene (PP) in co-rotating intermeshing twin-screw extruders (COITSEs) is analyzed by means of numerical simulations. This reactive extrusion (REX) operation is simulated by implementing (i) a one-dimensional and (ii) a three-dimensional (3D) modeling approach. In the case of the 1D modeling, a REX mathematical model previously developed and implemented as a computer code is used for the evaluation of two scale-up rules for COITSEs of various sizes. The first scale-up rule which is proposed in this work is based on the concept of thermal time introduced by Nauman (1977), and the second one is based on specific energy consumption (SEC) requirements. The processing parameters used in testing the previously referred to scale-up approaches are the mass throughput, the screw rotating speed, and the peroxide concentration, whereas the extruder screw configuration and the barrel temperature profiles are kept constant. The results for the simulated operating conditions show that when the REX operation is scaled-up under constant thermal time, very good agreement is obtained between the weight-average molecular weight (Mw) and poly-dispersity index (PDI) from the larger extruders and the values of these parameters corresponding to the reference extruder. For the constant SEC approach, on the other hand, more significant variations are observed for both of the aforementioned parameters. In the case of the implemented constant thermal time procedure, a further analysis of the effect of the mass throughput and screw speed of the reference device on the scaled-up operation is performed. It is observed that when the lower mass throughput is implemented for the smaller extruder keeping a constant screw speed, the predicted residence times of extrusion for the larger extruders are lower, in general terms, than those corresponding to the reference device, and a converse situation occurs for the higher implemented value of the mass throughput. Also, in general terms, the higher increase of the reaction temperature on the scaled-up operation corresponds to the lower mass throughputs and higher screw speeds specified for the reference extruder. For the 3D modeling approach, two different case studies are analyzed by means of a commercial FEM software package. The REX simulations are performed under the assumption of steady-state conditions using the concept of a moving relative system (MRS). To complement the information obtained from the MRS calculations, simulations for selected conditions (for non-reactive cases) are performed considering the more realistic transient-state (TS) flow conditions. The TS flow conditions are associated to the time periodicity of the flow field inside the conveying elements of COITSEs. In the first case study, the peroxide-initiated degradation of PP is simulated in fully-filled screw elements of two different size COITSEs in order to evaluate scale-up implications of the REX operation. In the second case, the reacting flow is simulated for a conventional conveying screw element and a conveying screw element having a special design and corresponding to the same extruder size. For both of the analyzed cases, the effects of the initial peroxide concentration and mass throughput on the final Mw and PDI of the degraded resin are studied. The effect of the processing conditions is discussed in terms of the residence time distribution (RTD), the temperature of reaction, and the distributive mixing capabilities of the REX system. When analyzing the scale-up case, it is found that for the implemented processing conditions, the final Mws and PDIs are very close to each other in both of the analyzed flow geometries when the specified flow is close to that corresponding to the maximum conveying capabilities of the screw elements. For more restrictive flow conditions, the final Mws and PDIs are lower in the case of the screw element of the larger extruder. It is found that the distributive mixing ability of the reactive flow is mainly related to the specified mass throughput and almost independent of the specified peroxide concentration for a particular extruder size. For the analyzed screw elements, the conveying element corresponding to the small size extruder shows a slightly better distributive mixing performance. For this same case study, a further evaluation of the proposed scale-up criterion under constant thermal time confirms the trend of the results observed for the 1D simulations. In the second case study, the special type of screw element consists of screws rotating at different speeds which have different cross sections. In this case, the outer and inner diameters of both the special and the conventional type of screw elements are specified to be the same. As in the previous case study, the distributive mixing capabilities appear to be independent of the specified peroxide concentrations but dependent on the mass flow rate. It is speculated from the simulation results, from both the transient- as well as the steady-state flow conditions, that the screw element with the special design would yield lower final values of the PDI and Mw. Also, this screw element appears to have improved distributive mixing capabilities as well as a wider RTD.

Yes / When compounding polymers with additives to develop materials at specifications (colouring plastics is the simplest example), the difficulties is in getting the formulation right the first time. Also, when developing completely new materials such as in nanotechnology applications, there is a need to do the initial trials safely and with as small quantities as possible to enable a wide range of experimentation. Wiith traditional applications, often the initial compounding formulation is done using small single or twin screw extruders but with machines that have a fair output to instruct the large scale operation. This step is costly in material wastage and time but more importantly it often does not provide the right formulation which in turn results in bigger wastage cost at the industrial scale before the right formulation is eventually obtained. With the very new material formulations, any reduction in cost of development is always essential. With these aims in mind, we have developed a new minimixer capable of handling tiny quantities of order 10-100g but the minimixer is capable of reproducing the very high mixing conditions experienced in large machines. This invention provides a new opportunity to develop new products quickly, safely and cheaply. The application is not restricted to polymers and can be extended to other soft materials. It has also other spin-offs as a research tool for studying mixing and developing new, more efficient, mixing flows. In this paper we explain the principle of operation we have engineered to produce such intense mixing. Basically, the device is based on combining two opposing flows: a single screw extruder circulation flow with a twin screw extruder mixing flow. The mixing is carried out as a batch but on its completion, the single screw extruder flow is reversed and becomes co-current with the twin extruder flow to enable the discharging of the batch through a die. In the paper we present mixing data obtained with various polymer-additive combinations tested in the minimixer under various conditions of screw speeds, mixing times and temperatures and at the larger scale to underpin the operation of this novel mixer. The quality of mixing of the extrudate was measured using a variety of methods depending on applications: using image analysis of microtome sections of the extrudate or of blown film samples produced from the formulations or measuring electrical properties.

No description available.

No description available.

Parmi les différents procédés d’élaboration de minigranules, le procédé d’extrusion-sphéronisation présente de nombreux avantages, puisqu’il permet notamment d’élaborer des minigranules fortement chargées en principe actif et d’éviter l’emploi de solvants organiques. Ce travail a pour objectif de comparer les performances de plusieurs systèmes d’extrusion à vis, de l’échelle du laboratoire jusqu’à la transposition à l’échelle industrielle. Pour cela, des plans d’expériences ont été construits afin d’identifier les variables critiques et de sélectionner l’extrudeur le plus favorable selon différentes approches spécifiques à cette étude. En effet, le système d’extrusion idéal est défini dans ce travail comme celui donnant les meilleurs résultats en termes de productivité et de caractéristiques des minigranules (« qualité »), entraînant le moins d’impact sur le produit après transposition d’échelle (« transposabilité »), montrant le moins d’influence sur le produit lorsque la formule utilisée change (« robustesse »), et permettant d’ajuster ou d’améliorer la qualité des minigranules lorsque les conditions opératoires varient (« flexibilité »). Quelle que soit l’approche étudiée, les résultats ont permis de mettre en évidence l’influence de paramètres critiques et de leurs interactions sur les différentes réponses et ont montré des différences entre les différents systèmes d’extrusion. L’étude à l’échelle du laboratoire a permis de comparer les extrudeurs radial, dôme et frontal et a mis en évidence l’intérêt des systèmes frontal et dôme en termes de qualité des minigranules, et du système radial en termes de robustesse et de flexibilité du procédé. L’étude à l’échelle industrielle a permis de comparer les extrudeurs radial et frontal, et a permis d’identifier l’extrudeur frontal comme étant le plus favorable en termes de qualité des minigranules, de robustesse, de flexibilité et de transposabilité. Les conclusions observées à l’échelle industrielle sont donc différentes de celles considérées à l’échelle du laboratoire, pour l’étude comparative des différents systèmes. Cela confirme l’importance de tester les systèmes à échelle industrielle avant l’acquisition d’un équipement. / Among the various methods of developing minigranules, extrusion-spheronization has many advantages, particularly since it allows to develop minigranules highly charged with active pharmaceutical ingredient and to avoid the use of organic solvents. This work aims to compare the performance of several extrusion screws systems, from the lab to the scale-up at industrial scale. Designs of experiments were built to identify critical variables and compare the extruder in terms of different approaches specific to this study. As a matter of fact, the ideal extrusion system is defined in this work as the one which gives the best results in terms of productivity and pellets characteristics (“quality”), the one which shows less impact on the product after scaling-up (“scalability”), the one which shows the less influence on these same properties when the formula used changes (“robustness”), and the one which allows the possibility to adjust or improve pellets properties with operating variables (“flexibility”). Whatever the approach studied, the results allowed to highlight the influence of critical parameters and their interactions on the different responses and showed differences between the different extrusion systems. The study at lab scale compared radial, dome and axial extruders and underlined the interest of axial and dome systems in terms of pellets quality, and radial system in terms of process robustness and flexibility. The study at industrial scale compared radial and axial systems, and identified the axial system as the most favorable in terms of pellets quality , robustness, flexibility and scalability. The conclusions observed at industrial scale are different from those observed at lab scale for the different systems comparative study. This confirms the importance to test systems at industrial scale before investing in one equipment.