A novel shadowgraphic inline probe to measure crystal size distributions (CSD), based on acquired greyscale images, is evaluated in terms of elevated temperatures and fragile crystals, and compared to well-established, alternative online and offline measurement techniques, i.e., sieving analysis and online microscopy. Additionally, the operation limits, with respect to temperature, supersaturation, suspension, and optical density, are investigated. Two different substance systems, potassium dihydrogen phosphate (prisms) and thiamine hydrochloride (needles), are crystallized for this purpose at 25 L scale. Crystal phases of the well-known KH₂PO₄/H₂O system are measured continuously by the inline probe and in a bypass by the online microscope during cooling crystallizations. Both measurement techniques show similar results with respect to the crystal size distribution, except for higher temperatures, where the bypass variant tends to fail due to blockage. Thiamine hydrochloride, a substance forming long and fragile needles in aqueous solutions, is solidified with an anti-solvent crystallization with ethanol. The novel inline probe could identify a new field of application for image-based crystal size distribution measurements, with respect to difficult particle shapes (needles) and elevated temperatures, which cannot be evaluated with common techniques.

A recently developed continuous enantioseparation process utilizing two coupled fluidized bed crystallizers is systematically investigated to identify essential correlations between different operation parameters and the corresponding process performance on the example of asparagine monohydrate. Based on liquid phase composition and product crystal size distribution data, it is proven that steady state operation is achieved reproducibly in a relatively short time. The process outputs at steady state are compared for different feed flow rates, supersaturations, and crystallization temperatures. It is shown that purities >97% are achieved with productivities up to 40 g/L/h. The size distribution, which depends almost exclusively on the liquid flow rate, can be easily adjusted between 260 and 330 µm (mean size) with an almost constant standard deviation of ±55 µm.

In this study, a comprehensive investigation of PET glycolysis has been performed. The research included the development of analytical techniques, experiments with different reactor systems, and the development of mathematical models to understand the kinetics of the process. Quantitative HPLC analysis was adopted and optimized for the detection of BHET, while the size-exclusion chromatography method was developed to determine the molecular weight distribution of solid PET residues. Over 33 experiments were performed with magnetically coupled shaft-stirred Amar reactors, resulting in more than 300 experimentally determined BHET concentration points at various reaction times, temperatures, catalyst concentrations, and ethylene glycol-to-PET ratios. Afterwards, a kinetic model was developed to describe the observed phenomena with a validation step.

In recent years, sustainability and the concept of a circular economy have grown in importance within almost all industrial sectors. Especially in the chemical industry, recycling of polymer waste streams has become an important pathway to avoid plastic waste being landfilled or incinerated. Additionally, traditional carbon sources, such as fossil fuels, can be substituted with streams of recycled polymer. For example, polyethylene terephthalate (PET), which is utilized in plastic bottles and textiles, may be recycled via glycolysis. This depolymerization yields the monomer bis(2-hydroxyethyl) terephthalate (BHET). This study focuses on the thermal behavior and stability of BHET, both in pure form as well as in the presence of ethylene glycol (EG), as it results from PET glycolysis. For this, differential scanning calorimetry (DSC), Fourier transform infrared spectroscopy (FTIR), high-performance liquid chromatography (HPLC), powder X-ray diffraction (PXRD), and thermogravimetry (TG) were utilized. The results exhibited pure BHET polymerizing to PET at temperatures above 120 °C, while further increasing temperatures increased the reaction kinetics. Additionally, no reaction was observed in BHET/EG mixtures at any temperature investigated, which can be attributed to the presence of EG shifting the equilibrium of the reaction towards the BHET, thus inhibiting polymerization. Based on these results and the determined BHET/EG (solubility) phase diagram, potential purification strategies based on crystallization are proposed.