Evaluation of Different Thermoanalytical Methods for the Analysis of the Stability of Naproxen-Loaded Amorphous Solid Dispersions.

The aim of this research was to investigate three thermoanalytical techniques from the glass transition temperature (Tg) determination point of view. In addition, the examination of the correlation between the measured Tg values and the stability of the amorphous solid dispersions (ASDs) was also an important part of the work. The results showed that a similar tendency of the Tg can be observed in the case of the applied methods. However, Tg values measured by thermally stimulated depolarization currents showed higher deviation from the theoretical calculations than the values measured by modulated differential scanning calorimetry, referring better to the drug-polymer interactions. Indeed, the investigations after the stress stability tests revealed that micro-thermal analysis can indicate the most sensitive changes in the Tg values, better indicating the instability of the samples. In addition to confirming that the active pharmaceutical ingredient content is a crucial factor in the stability of ASDs containing naproxen and poly(vinylpyrrolidone-co-vinyl acetate), it is worthwhile applying orthogonal techniques to better understand the behavior of ASDs. The development of stable ASDs can be facilitated via mapping the molecular mobilities with suitable thermoanalytical methods.

Development of Bioepoxy Resin Microencapsulated Ammonium-Polyphosphate for Flame Retardancy of Polylactic Acid.

Ammonium-polyphosphate (APP) was modified by microencapsulation with a bio-based sorbitol polyglycidyl ether (SPE)-type epoxy resin and used as a flame retardant additive in polylactic acid (PLA) matrix. The bioresin-encapsulated APP (MCAPP) particles were characterized using Fourier transform infrared (FTIR) spectroscopy and Raman mapping, particle size distribution was determined by processing of scanning electron microscopic (SEM) images. Interaction between the APP core and the bioresin shell was revealed by combined thermogravimetric analysis (TGA)­FTIR spectroscopy. The APP to SPE mass ratio of 10 to 2 was found to be optimal in terms of thermal, flammability, and mechanical properties of 15 wt% additive containing biocomposites. The bioresin shell effectively promotes the charring of the APP-loaded PLA composites, as found using TGA and cone calorimetry, and eliminates the flammable dripping of the specimens during the UL-94 vertical burning tests. Thus, the V-0 rating, the increased limiting oxygen index, and the 20% reduced peak of the heat release rate was reached compared to the effects of neat APP. Furthermore, better interfacial interaction of the MCAPP with PLA was indicated by differential scanning calorimetry and SEM observation. The stiff interphase resulted in increased modulus of these composites. Besides, microencapsulation provided improved water resistance to the flame retardant biopolymer system.

Application of Melt-Blown Poly(lactic acid) Fibres in Self-Reinforced Composites.

The aim of our research was to produce poly(lactic acid) (PLA) fibres with diameters in the micrometer size range, serving as the reinforcing phase in self-reinforced (SR) PLA composites. Nonwoven PLA mats were manufactured by solvent-free melt-blowing technology. Three types of PLA differing in d-lactide content were processed with a productivity as high as 36 g/h. The crystallinity of the PLA microfibres was enhanced by thermal annealing. A 2⁻3-fold increase in the degree of crystallinity was obtained, as measured by differential scanning calorimetry (DSC). Fibre diameters between 2⁻14 µm were revealed by scanning electron microscopy (SEM). Static tensile tests were performed on the nonwoven mats, showing the reduced moduli of the annealed fibres due the amorphous relaxation. The PLA mats were processed via the hot compaction technique and formed into SR⁻PLA composites. The morphological and mechanical properties of the obtained microstructural composites were comprehensively studied. Composites prepared from annealed, thermally more stable PLA nonwoven mats showed superior mechanical properties; the tensile strength improved by 47% due to the higher residual fibre content.