Dynamic grey-box modeling for online monitoring of extrusion viscosity

Melt viscosity is a key indicator of product quality in polymer extrusion processes. However, real time monitoring and control of viscosity is difficult to achieve. In this article, a novel “soft sensor” approach based on dynamic gray-box modeling is proposed. The soft sensor involves a nonlinear finite impulse response model with adaptable linear parameters for real-time prediction of the melt viscosity based on the process inputs; the model output is then used as an input of a model with a simple-fixed structure to predict the barrel pressure which can be measured online. Finally, the predicted pressure is compared to the measured value and the corresponding error is used as a feedback signal to correct the viscosity estimate. This novel feedback structure enables the online adaptability of the viscosity model in response to modeling errors and disturbances, hence producing a reliable viscosity estimate. The experimental results on different material/die/extruder confirm the effectiveness of the proposed “soft sensor” method based on dynamic gray-box modeling for real-time monitoring and control of polymer extrusion processes. POLYM. ENG. SCI., 2012. © 2012 Society of Plastics Engineers

Investigation of the process energy demand in polymer extrusion: a brief review and an experimental study

Extrusion is one of the fundamental production methods in the polymer processing industry and is used in the production of a large number of commodities in a diverse industrial sector. Being an energy intensive production method, process energy efficiency is one of the major concerns and the selection of the most energy efficient processing conditions is a key to reducing operating costs. Usually, extruders consume energy through the drive motor, barrel heaters, cooling fans, cooling water pumps, gear pumps, etc. Typically the drive motor is the largest energy consuming device in an extruder while barrel/die heaters are responsible for the second largest energy demand. This study is focused on investigating the total energy demand of an extrusion plant under various processing conditions while identifying ways to optimise the energy efficiency. Initially, a review was carried out on the monitoring and modelling of the energy consumption in polymer extrusion. Also, the power factor, energy demand and losses of a typical extrusion plant were discussed in detail. The mass throughput, total energy consumption and power factor of an extruder were experimentally observed over different processing conditions and the total extruder energy demand was modelled empirically and also using a commercially available extrusion simulation software. The experimental results show that extruder energy demand is heavily coupled between the machine, material and process parameters. The total power predicted by the simulation software exhibits a lagging offset compared with the experimental measurements. Empirical models are in good agreement with the experimental measurements and hence these can be used in studying process energy behaviour in detail and to identify ways to optimise the process energy efficiency.

Viscosity Control for Extrusion Processes Using Recycled Polymers

The aim of this paper is to develop a new extruder control system for recycled materials which has ability to automatically maintain constant a polymer melt viscosity of mixed recycled polymers during extrusion, regardless of variations in the Melt Flow Index (MFI) of recycled mixed grade high density polyethylene (HDPE) feedstock. A closed-loop controller is developed to automatically regulate screw speed and barrel temperature profile to achieve constant viscosity and enable consistent processing of variable grade recycled HDPE materials. The experimental results of real time viscosity measurement and control using a 38mm single screw extruder with different recycled HDPEs with widely different MFIs are reported in this work

Dynamic modelling of die melt temperature profile in polymer extrusion: Effects of process settings, screw geometry and material

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.

Investigation of the temperature homogeneity of die melt flows in polymer extrusion

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

Thermodynamically stable amorphous drug dispersions in amorphous hydrophilic polymers engineered by hot melt extrusion.

In this study thermodynamically stable dispersions of amorphous quinine, a model BCS class 2 therapeutic agent, within an amorphous polymeric platform (HPC), termed a solid-in-solid dispersion, were produced using hot melt extrusion. Characterisation of the pre-extrudates and extrudates was performed using hyper-differential scanning calorimetry (DSC), powder X-ray diffraction (PXRD) and Raman spectroscopy. Water uptake by the raw materials was determined using dynamic vapour sorption (DVS) analysis. Furthermore, the presence or absence of crystalline drug following storage at 25 °C/60% relative humidity and 40 °C/75% relative humidity in a sealed glass jar, and at 40 °C/75% relative humidity in an open glass jar for 3 months was determined using PXRD. Amorphous quinine was generated in situ during extrusion from both quinine base (5%, 10%, 20% w/w drug loading) and from quinine hydrochloride (5%, 10% w/w drug loading) and remained thermodynamically stable as a solid-in-solid dispersion within the HPC extrudates. When processed with HPC, quinine hydrochloride (20% w/w) was converted to amorphous quinine hydrochloride. Whilst stable for up to 3 months when stored under sealed conditions, this amorphous form was unstable, resulting in recrystallisation of the hydrochloride salt following storage for 1 month at 40 °C/75% relative humidity in an open glass jar. The behaviour of the amorphous quinine hydrochloride (20% w/w) HPC extrudate was related, at least in part, to the lower stability and the hygroscopic properties of this amorphous form.

Novel Supercritical Carbon Dioxide Impregnation Technique for the Production of Amorphous Solid Drug Dispersions: A Comparison to Hot Melt Extrusion

The formulation of BCS Class II drugs as amorphous solid dispersions has been shown to provide advantages with respect to improving the aqueous solubility of these compounds. While hot melt extrusion (HME) and spray drying (SD) are among the most common methods for the production of amorphous solid dispersions (ASDs), the high temperatures often required for HME can restrict the processing of thermally labile drugs, while the use of toxic organic solvents during SD can impact on end-product toxicity. In this study, we investigated the potential of supercritical fluid impregnation (SFI) using carbon dioxide as an alternative process for ASD production of a model poorly water-soluble drug, indomethacin (INM). In doing so, we produced ASDs without the use of organic solvents and at temperatures considerably lower than those required for HME. Previous studies have concentrated on the characterization of ASDs produced using HME or SFI but have not considered both processes together. Dispersions were manufactured using two different polymers, Soluplus and polyvinylpyrrolidone K15 using both SFI and HME and characterized for drug morphology, homogeneity, presence of drug-polymer interactions, glass transition temperature, amorphous stability of the drug within the formulation, and nonsink drug release to measure the ability of each formulation to create a supersaturated drug solution. Fully amorphous dispersions were successfully produced at 50% w/w drug loading using HME and 30% w/w drug loading using SFI. For both polymers, formulations containing 50% w/w INM, manufactured via SFI, contained the drug in the γ-crystalline form. Interestingly, there were lower levels of crystallinity in PVP dispersions relative to SOL. FTIR was used to probe for the presence of drug-polymer interactions within both polymer systems. For PVP systems, the nature of these interactions depended upon processing method; however, for Soluplus formulations this was not the case. The area under the dissolution curve (AUC) was used as a measure of the time during which a supersaturated concentration could be maintained, and for all systems, SFI formulations performed better than similar HME formulations.

Characterisation of Bioresorbable Composite Performance for Validation of New On-Line Process Monitoring Technology

There is an increasing interest in the biomedical field to create implantable medical devices to provide a temporary mechanical function for use inside the human body. In many of these applications bioresorbable polymer composites using PLLA with β-TCP , are increasingly being used due to their biocompatability, biodegradability and mechanical strength.1,3 These medical devices can be manufactured using conventional plastics processing methods such as injection moulding and extrusion, however there is great need to understand and control the process due to a lack of knowledge on the influence of processing on material properties. With the addition of biocompatible additives there is also a requirement to be able to predict the quality and level of dispersion within the polymer matrix. On-line UV-Vis spectroscopy has been shown to monitor the quality of fillers in polymers. This can eliminate time consuming and costly post-process evaluation of additive dispersion. The aim of this work was to identify process and performance relationships of PLLA/β-TCP composites with respect to melt-extrusion conditions. This is part of a wider study into on-line process monitoring of bioresorbable polymers as used in the medical industry.
These results show that final properties of the PLLA/ β-TCP composite are highly influenced by the particle size and loading. UV-Vis spectroscopy can be used on-line to monitor the final product and this can be utilised as a valuable tool for quality control in an application where consistent performance is of paramount importance.

The determination of optimal processing conditions for PLA and PLA/CaCO3 in twin screw extrusion using DoE and multivariate analysis

Biodegradable polymers, such as PLA (Polylactide), come from renewable resources like corn starch and if disposed of correctly, degrade and become harmless to the ecosystem making them attractive alternatives to petroleum based polymers. PLA in particular is used in a variety of applications including medical devices, food packaging and waste disposal packaging. However, the industry faces challenges in melt processing of PLA due to its poor thermal stability which is influenced by processing temperatures and shearing.
Identification and control of suitable processing conditions is extremely challenging, usually relying on trial and error, and often sensitive to batch to batch variations. Off-line assessment in a lab environment can result in high scrap rates, long lead times and lengthy and expensive process development. Scrap rates are typically in the region of 25-30% for medical grade PLA costing between €2000-€5000/kg.
Additives are used to enhance material properties such as mechanical properties and may also have a therapeutic role in the case of bioresorbable medical devices, for example the release of calcium from orthopaedic implants such as fixation screws promotes healing. Additives can also reduce the costs involved as less of the polymer resin is required.
This study investigates the scope for monitoring, modelling and optimising processing conditions for twin screw extrusion of PLA and PLA w/calcium carbonate to achieve desired material properties. A DAQ system has been constructed to gather data from a bespoke measurement die comprising melt temperature; pressure drop along the length of the die; and UV-Vis spectral data which is shown to correlate to filler dispersion. Trials were carried out under a range of processing conditions using a Design of Experiments approach and samples were tested for mechanical properties, degradation rate and the release rate of calcium. Relationships between recorded process data and material characterisation results are explored.