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 / Grinding solid reagents under solvent-free or low-solvent conditions (mechanochemistry) is emerging as a general synthetic technique which is an alternative to conventional solvent-intensive methods. However, it is essential to find ways to scale-up this type of synthesis if its promise of cleaner manufacturing is to be realised. Here, we demonstrate the use of twin screw and single screw extruders for the continuous synthesis of various metal complexes, including Ni(salen), Ni(NCS)2(PPh3)2 as well as the commercially important metal organic frameworks (MOFs) Cu3(BTC)2 (HKUST-1), Zn(2-methylimidazolate)2 (ZIF-8, MAF-4) and Al(fumarate)(OH). Notably, Al(fumarate)(OH) has not previously been synthesised mechanochemically. Quantitative conversions occur to give products at kg h−1 rates which, after activation, exhibit surface areas and pore volumes equivalent to those of materials produced by conventional solvent-based methods. Some reactions can be performed either under completely solvent-free conditions whereas others require the addition of small amounts of solvent (typically 3–4 mol equivalents). Continuous neat melt phase synthesis is also successfully demonstrated by both twin screw and single screw extrusion for ZIF-8. The latter technique provided ZIF-8 at 4 kg h−1. The space time yields (STYs) for these methods of up to 144 × 103 kg per m3 per day are orders of magnitude greater than STYs for other methods of making MOFs. Extrusion methods clearly enable scaling of mechanochemical and melt phase synthesis under solvent-free or low-solvent conditions, and may also be applied in synthesis more generally. / EPSRC (EP/L019655/1)

No / The development and validation of a sensor for extrusion melt temperature field measurement is described. A grid of opposing thermocouple wires was constructed and held in position by a supporting frame. Wires were joined together at crossing points to form thermocouple junctions, which were computer monitored. The mesh was used to monitor melt temperature fields during single screw extrusion at the die entrance. Design and construction of the mesh is described in addition to experimental optimization of wire diameter and junction forming. Calibration of the sensor and potential measurement errors including shear heating effects are discussed. Initial results from single screw extrusion are presented for a commercial grade of low density polyethylene using five- and seven-junction thermocouple meshes. The dependence of melt temperature profile on screw speed is illustrated. At low screw speeds melt temperature profiles were flat in shape and higher than set wall temperatures. At higher screw speeds the profiles became more pointed in shape. Use of higher resolution sensors exposed more complex temperature profiles with shoulder regions.

No / Polymer extrusion is fundamental to the processing of polymeric materials and melt flow temperature homogeneity is a major factor which influences product quality. Undesirable thermal conditions can cause problems such as melt degradation, dimensional instability, weaknesses in mechanical/optical/geometrical properties, and so forth. It has been revealed that melt temperature varies with time and with radial position across the die. However, the majority of polymer processes use only single-point techniques whose thermal measurements are limited to the single point at which they are fixed. Therefore, it is impossible for such techniques to determine thermal homogeneity across the melt flow. In this work, an extensive investigation was carried out into melt flow thermal behavior of the output of a single extruder with different polymers and screw geometries over a wide range of processing conditions. Melt temperature profiles of the process output were observed using a thermocouple mesh placed in the flow and results confirmed that the melt flow thermal behavior is different at different radial positions. The uniformity of temperature across the melt flow deteriorated considerably with increase in screw rotational speed while it was also shown to be dependent on process settings, screw geometry, and material properties. Moreover, it appears that the effects of the material, machine, and process settings on the quantity and quality of the process output are heavily coupled with each other and this may cause the process to be difficult to predict and variable in nature. (C) 2013 Society of Plastics Engineers

No / Polymer extrusion is an energy intensive process, which is often run at less than optimal conditions. The extrusion process consists of gradual melting of solid polymer by thermal conduction and viscous shearing between a rotating screw and a barrel; as such it is highly dependent upon the frictional, thermal and rheological properties of the polymer. Extruder screw geometry and extrusion variables should ideally be tailored to suit the properties of individual polymers, but in practice this is rarely achieved due to the lack of understanding of the process. Here, in-process monitoring techniques have been used to characterise the thermal dynamics of the extrusion process. Novel thermocouple grid sensors have been used to measure melt temperature fields within flowing polymer melts at the entrance to an extruder die in conjunction with infra-red thermometers and real-time quantification of energy consumption. A commercial grade of polyethylene has been examined using three extruder screw geometries at different extrusion operating conditions to understand the process efficiency. Extruder screw geometry, screw rotation speed and set temperature were found to have a significant effect on the thermal homogeneity of the melt and process energy consumed. (C) 2012 Elsevier Ltd. All rights reserved.

This research investigates formulation, compounding and thin-wall injection moulding of Polypropylene/clay nanocomposites (PPCNs) prepared using conventional melt-state processes. An independent study on single screw extrusion dynamics using Design of Experiments (DoE) was performed first. Then the optimum formulation of PPCNs and compounding conditions were determined using this strategy. The outcomes from the DoE study were then applied to produce PPCN compounds for the subsequent study of thin-wall injection moulding, for which a novel four-cavity injection moulding system was designed using CAD software and a new moulding tool was constructed based upon this design. Subsequently, the effects of moulding conditions, nanoclay concentration and wall thickness on the injection moulded PPCN parts were investigated. Moreover, simulation of the injection moulding process was carried out to compare the predicted performance with that obtained in practice by measurement of real-time data using an in-cavity pressure sensor. For the selected materials, the optimum formulation is 4 wt% organoclay (DK4), 4 wt% compatibiliser (Polybond 3200, PPgMA) and 1.5 wt% co-intercalant (erucamide), as the maximum interlayer spacing of clay can be achieved in the selected experimental range. Furthermore, DoE investigations determined that a screw speed of 159 rpm and a feed rate of 5.4 kg/h are the optimum compounding conditions for the twin screw extruder used to obtain the highest tensile modulus and yield strength from the PPCN compounds. The optimised formulation of PPCNs and compounding conditions were adopted to manufacture PPCN materials for the study of thin-wall injection moulding. In the selected processing window, tensile modulus and yield strength increase significantly with decreasing injection speed, due to shear-induced orientation effects, exemplified by a significantly increased frozen layer thickness observed by optical microscopy (OM) and Moldflow® simulation. Furthermore, the TEM images indicate a strong orientation of clay particles in the flow direction, so the PPCN test pieces cut parallel to the flow direction have 36.4% higher tensile modulus and 13.6 % higher yield strength than those cut perpendicular to the flow direction, demonstrating the effects of shear induced orientation on the tensile properties of thin-wall injection moulded PPCN parts. In comparison to injection speed, mould temperature has very limited effects in the selected range investigated (25-55 °C), in this study. The changes in moulding conditions show no distinctive effects on PP crystallinity and intercalation behaviour of clay. Impact toughness of thin wall injection moulded PPCN parts is not significantly affected by either the changes in moulding conditions or clay concentration (1-5 %). The SEM images show no clear difference between the fracture surfaces of PPCN samples with different clay concentrations. TEM and XRD results suggest that higher intercalation but lower exfoliation is achieved in PPCN parts with higher clay content. The composites in the thin sections (at the end of flow) have 34 % higher tensile modulus and 11 % higher yield strength than in the thicker sections, although the thin sections show reduced d001 values. This is attributed to the significantly enhanced shear-induced particle/molecular orientation and more highly oriented frozen layer, according to TEM, OM and process simulation results. In terms of the reduced d001 values in the thin sections, it is proposed that the extreme shear conditions in the thin sections stretch the PP chains in the clay galleries to a much higher level, compaction of clay stacks occurs as less interspacing is needed to accommodate the stretched chains, but rapid cooling allows no time for the chains to relax and expand the galleries back. Overall, data obtained from both actual moulding and simulation indicate that injection speed is of utmost importance to the thin-wall injection moulding process, development of microstructure, and thus the resulting properties of the moulded PPCN parts, in the selected experimental ranges of this research.