Evaluation of the printability of agar and hydroxypropyl methylcellulose gels as gummy formulations: Insights from rheological properties.

The trial-and-error method currently used to create formulations with excellent printability demands considerable time and resources, primarily due to the increasing number of variables involved. Rheology serves as a relatively rapid and highly beneficial method for assessing materials and evaluating their effectiveness as 3D constructs. However, the data obtained can be overwhelming, especially for users lacking experience in this field. This study examined the rheological properties of formulations of agar, hydroxypropyl methylcellulose, and the model drug caffeine, alongside exploring their printability as gummy formulations. The gels' rheological properties were characterized using oscillatory and rotational experiments. The correlation between these gels' rheological properties and their printability was established, and three clusters were formed based on the rheological properties and printability of the samples using principal component analysis. Furthermore, the printability was predicted using the sample's rheological property that correlated most with printability, the phase angle δ, and the regression models resulted in an accuracy of over 80%. Although these relationships merit confirmation in later studies, this study suggests a quantitative definition of the relationship between printability and one rheological property and can be used for the development of formulations destined for extrusion 3D printing.

Polymer Supercritical CO2 Foaming under Peculiar Conditions: Laser and Ultrasound Implementation.

The two-step batch foaming process of solid-state assisted by supercritical CO2 is a versatile technique for the foaming of polymers. In this work, it was assisted by an out-of-autoclave technology: either using lasers or ultrasound (US). Laser-aided foaming was only tested in the preliminary experiments; most of the work involved US. Foaming was carried out on bulk thick samples (PMMA). The effect of ultrasound on the cellular morphology was a function of the foaming temperature. Thanks to US, cell size was slightly decreased, cell density was increased, and interestingly, thermal conductivity was shown to decrease. The effect on the porosity was more remarkable at high temperatures. Both techniques provided micro porosity. This first investigation of these two potential methods for the assistance of supercritical CO2 batch foaming opens the door to new investigations. The different properties of the ultrasound method and its effects will be studied in an upcoming publication.

Foaming of PLA Composites by Supercritical Fluid-Assisted Processes: A Review.

Polylactic acid (PLA) is a well-known and commercially available biopolymer that can be produced from different sources. Its different characteristics generated a great deal of interest in various industrial fields. Besides, its use as a polymer matrix for foam production has increased in recent years. With the rise of technologies that seek to reduce the negative environmental impact of processes, chemical foaming agents are being substituted by physical agents, primarily supercritical fluids (SCFs). Currently, the mass production of low-density PLA foams with a uniform cell morphology using SCFs as blowing agents is a challenge. This is mainly due to the low melt strength of PLA and its slow crystallization kinetics. Among the different options to improve the PLA characteristics, compounding it with different types of fillers has great potential. This strategy does not only have foaming advantages, but can also improve the performances of the final composites, regardless of the implemented foaming process, i.e., batch, injection molding, and extrusion. In addition, the operating conditions and the characteristics of the fillers, such as their size, shape factor, and surface chemistry, play an important role in the final foam morphology. This article proposes a critical review on the different SCF-assisted processes and effects of operating conditions and fillers on foaming of PLA composites.

Modelling of the rheological behavior of mechanically dewatered sewage sludge in uniaxial cyclic compression.

The rheological behavior of mechanically dewatered sewage sludges is complex but essential as it affects almost all treatment, utilization and disposal operations, such as storage, pumping, land-spreading, or drying. In this work, a specific methodology coupling experiments and modelling is developed to characterize the rheological and textural properties of highly concentrated sludge. The experimental part based on a uniaxial compression method has been presented in a previous paper (Liang et al., 2017). This article is dedicated to the modelling part, which includes the behavior identification and the parameters optimization. Previous and additional mechanical tests allow the identification of a visco-elasto-plastic behavior. This behavior is then modelled with a Burgers-Ludwik model, with 7 rheological parameters. This model is able to simulate the viscoelastic behavior of sludge under the yield stress, and the visco-elasto-plastic hardening behavior over the yield stress. The optimization of model parameters is carried out in two steps and relies on the calculation of basins of attraction and confidence intervals with initial conditions estimated from the mechanical tests. Finally, the entire characterization methodology, from experimental mechanical tests to model parameter optimization, is applied to sludge samples at different operating conditions and structural states. The determination of the rheological properties of sludge is achieved with excellent matching between simulation and experimental results. Being able to take into account these impact factors, the rheological model can be used to predict the sludge behavior in various operating conditions.

A uniaxial cyclic compression method for characterizing the rheological and textural behaviors of mechanically dewatered sewage sludge.

The mechanically dewatered sewage sludge with total solid content around 20% on a weight basis is very similar to yield stress fluid, its complex transition between solid and fluid states is not perfectly reversible and especially challenging in terms of pumping, land spreading and drying. To characterize the rheological and textural properties of highly concentrated sludge, a specific methodology based on uniaxial single and cyclic compression tests is developed. Three types of sludge samples (fresh original, fresh premixed and aged original ones) are extruded into cylinders and pressed between two parallel plates using a material testing machine. In single compression, the bioyield point beyond which the sludge fractures is around 7.3 kPa with true strain equal to 0.21. The cyclic compression tests reveal that the sludge behaves as a viscoelastic body when the true strain is smaller than 0.05 and as a visco-elasto-plastic once exceeding the yield stress. The elastic module is around 78 kPa; the viscosity is deduced, in the order of magnitude 104-105 Pa·s and the yield stress is estimated about 4 kPa. In the unloading phase, the sludge behaves again as a viscoelastic body with clear hysteresis. With the increase of compression speed, the viscosity declines, which confirms that the sludge is a shear-thinning material. The yield stress and the bioyield increase with compression speed, but it does not induce extra internal damage in the samples since the resilience and the cohesiveness are unaltered. The reliability and sensitivity of the method is justified by highlighting the changes of sludge behavior due to aging and premixing effects: both decrease the strain energy density, but do aggravate the adhesiveness of the sludge; the aging makes the sludge less cohesive, while the premixing does not modify its cohesiveness. In spite of changes in test conditions, the elastic module of sludge samples remains unchanged.

A new methodology for measurement of sludge residence time distribution in a paddle dryer using X-ray fluorescence analysis.

Drying is a necessary step before sewage sludge energetic valorization. Paddle dryers allow working with such a complex material. However, little is known about sludge flow in this kind of processes. This study intends to set up an original methodology for sludge residence time distribution (RTD) measurement in a continuous paddle dryer, based on the detection of mineral tracers by X-ray fluorescence. This accurate analytical technique offers a linear response to tracer concentration in dry sludge; the protocol leads to a good repeatability of RTD measurements. Its equivalence to RTD measurement by NaCl conductivity in sludge leachates is assessed. Moreover, it is shown that tracer solubility has no influence on RTD: liquid and solid phases have the same flow pattern. The application of this technique on sludge with different storage duration at 4 °C emphasizes the influence of this parameter on sludge RTD, and thus on paddle dryer performances: the mean residence time in a paddle dryer is almost doubled between 24 and 48 h of storage for identical operating conditions.

A three step supercritical process to improve the dissolution rate of eflucimibe.

The aim of this study is to improve the dissolution properties of a poorly-soluble active substance, Eflucimibe by associating it with gamma-cyclodextrin. To achieve this objective, a new three-step process based on supercritical fluid technology has been proposed. First, Eflucimibe and cyclodextrin are co-crystallized using an anti-solvent process, dimethylsulfoxide being the solvent and supercritical carbon dioxide being the anti-solvent. Second, the co-crystallized powder is held in a static mode under supercritical conditions for several hours. This is the maturing step. Third, in a final stripping step, supercritical CO(2) is flowed through the matured powder to extract the residual solvent. The coupling of the first two steps brings about a significant synergistic effect to improve the dissolution rate of the drug. The nature of the entity obtained at the end of each step is discussed and some suggestions are made as to what happens in these operations. It is shown the co-crystallization ensures a good dispersion of both compounds and is rather insensitive to the operating parameters tested. The maturing step allows some dissolution-recrystallization to occur thus intensifying the intimate contact between the two compounds. Addition of water is necessary to make maturing effective as this is governed by the transfer properties of the medium. The stripping step allows extraction of the residual solvent but also removes some of the Eflucimibe which is the main drawback of this final stage.