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A green approach has been used for co-crystallization of noncongruent co-crystal pair of caffeine/maleic acid using water. Ultrasound is known to affect crystallization; hence, the effect of high power ultrasound on the ternary phase diagram has been investigated in detail using a slurry co-crystallization approach. A systematic investigation was performed to understand how the accelerated conditions during ultrasound-assisted co-crystallization will affect different regions of the ternary phase diagram. Application of ultrasound showed considerable effect on the ternary phase diagram, principally on caffeine/maleic acid 2:1 (disappeared) and 1:1 co-crystal (narrowed) regions. Also, the stability regions for pure caffeine and maleic acid in water were narrowed in the presence of ultrasound, expanding the solution region. The observed effect of ultrasound on the phase diagram was correlated with solubility of caffeine and maleic acid and stability of co-crystal forms in water.

The use of near infra red spectroscopy to predict the concentration of two pharmaceutical co-crystals; 1:1 ibuprofen–nicotinamide (IBU-NIC) and 1:1 carbamazepine–nicotinamide (CBZ-NIC) has been evaluated. A partial least squares (PLS) regression model was developed for both co-crystal pairs using sets of standard samples to create calibration and validation data sets with which to build and validate the models. Parameters such as the root mean square error of calibration (RMSEC), root mean square error of prediction (RMSEP) and correlation coefficient were used to assess the accuracy and linearity of the models. Accurate PLS regression models were created for both co-crystal pairs which can be used to predict the co-crystal concentration in a powder mixture of the co-crystal and the active pharmaceutical ingredient (API). The IBU-NIC model had smaller errors than the CBZ-NIC model, possibly due to the complex CBZ-NIC spectra which could reflect the different arrangement of hydrogen bonding associated with the co-crystal compared to the IBU-NIC co-crystal. These results suggest that NIR spectroscopy can be used as a PAT tool during a variety of pharmaceutical co-crystal manufacturing methods and the presented data will facilitate future offline and in-line NIR studies involving pharmaceutical co-crystals.

highlights � This paper discusses the energy conservation of an extruder. � This describes the energy and thermal efficiencies in polymer extrusion. � This explores the correlation between energy demand and thermal stability. � This explores radial temperature fluctuations of the melt flow in extrusion. � This models the total power demand in polymer extrusion empirically. abstract Thermal stability is of major importance in polymer extrusion, where product quality is dependent upon the level of melt homogeneity achieved by the extruder screw. Extrusion is an energy intensive process and optimisation of process energy usage while maintaining melt stability is necessary in order to pro- duce good quality product at low unit cost. Optimisation of process energy usage is timely as world energy prices have increased rapidly over the last few years. In the first part of this study, a general dis- cussion was made on the efficiency of an extruder. Then, an attempt was made to explore correlations between melt thermal stability and energy demand in polymer extrusion under different process settings and screw geometries. A commodity grade of polystyrene was extruded using a highly instrumented sin- gle screw extruder, equipped with energy consumption and melt temperature field measurement. More- over, the melt viscosity of the experimental material was observed by using an off-line rheometer. Results showed that specific energy demand of the extruder (i.e. energy for processing of unit mass of polymer) decreased with increasing throughput whilst fluctuation in energy demand also reduced. How- ever, the relationship between melt temperature and extruder throughput was found to be complex, with temperature varying with radial position across the melt flow. Moreover, the melt thermal stability dete- riorated as throughput was increased, meaning that a greater efficiency was achieved at the detriment of melt consistency. Extruder screw design also had a significant effect on the relationship between energy consumption and melt consistency. Overall, the relationship between the process energy demand and thermal stability seemed to be negatively correlated and also it was shown to be highly complex in nat- ure. Moreover, the level of process understanding achieved here can help to inform selection of equip- ment and setting of operating conditions to optimise both energy and thermal efficiencies in parallel. 2014 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY license (http://

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.

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.

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.

Melt temperature is one of the key variables in polymer extrusion which determines process thermal stability and hence melt quality. Therefore, melt temperature is commonly measured in polymer processing and point/bulk melt temperature measurement methods are widely used in the present industry. Some thermal profile measurement methods have also been attempted in research. This study presents a review of melt temperature measurements in polymer extrusion in research and industry, and describes the results of an experimental evaluation carried out to explore the performance of five melt temperature measurement techniques. In addition, an investigation was carried out on the fully developed melt temperature profile of a cylindrical rod die. Moreover, the existing challenges and possible future applications for extrusion thermal monitoring are discussed. The results confirmed that melt temperature varied significantly at different radial locations within the die. Point/bulk melt temperature measurements were found to provide relatively limited information on process thermal quality close to the die wall. Hence, information provided by these sensors is less representative of actual thermal conditions as they are unable to capture thermal information from the whole melt flow cross-section. Therefore, the importance of the development of industrially compatible thermal profile measurement techniques is emphasised.

The cure of polydicyclopentadiene conducted by ring-opening metathesis polymerisation in the presence of a Grubbs catalyst was studied using non-invasive Raman spectroscopy. The spectra of the monomer precursor and polymerised product were fully characterised and all stages of polymerisation monitored. Because of the monomer's high reactivity, the cure process is adaptable to reaction injection moulding and reactive rotational moulding. The viscosity of the dicyclopentadiene undergoes a rapid change at the beginning of the polymerisation process and it is critical that the induction time of the viscosity increase is determined and controlled for successful manufacturing. The results from this work show non-invasive Raman spectroscopic monitoring to be an effective method for monitoring the degree of cure, paving the way for possible implementation of the technique as a method of real-time analysis for control and optimisation during reactive processing. Agreement is shown between Raman measurements and ultrasonic time of flight data acquired during the initial induction period of the curing process.