This study is focused on the micronization of p-toluenesulfonamide (p-TSA) using the rapid expansion of supercritical solution (RESS) process. Taguchi’s experimental design method was applied to determine the optimum operating conditions. L₉(3⁴) orthogonal array with four control factors and three levels of each control factor was used to design nine experimental conditions. Four control factors were selected, including extraction temperature, extraction pressure, pre-expansion temperature, and post-expansion temperature. The particle size and morphology of the prepared samples were observed by scanning electron microscopy (SEM). In addition, Fourier transform infrared spectrometer (FTIR), X-ray diffraction (XRD), and differential scanning calorimetry (DSC) were employed to compare the differences between the raw and micronized p-TSA particles. The experimental and analytical results indicated that the extraction temperature was the most significant factor for the micronization of p-TSA in the RESS process, and the optimal operating conditions were at an extraction temperature of 50 °C, an extraction pressure of 220 MPa, a pre-expansion temperature of 220 °C, and a post-expansion temperature of 30 °C. The p-TSA particles were micronized from the original average size of 294.8 μm to the smallest average size of 1.1 μm at the optimal RESS process conditions. Furthermore, the physicochemical characteristics of p-TSA did not differ significantly before and after recrystallization.

Two case studies of salicylamide particle size reduction and isoniazid derivative synthesis and crystallization realized using sonocrystallization were investigated. The size, habit, structure, thermal behavior, and spectrometric properties of sonocrystallized crystals were analyzed through scanning electron microscopy (SEM), powder X-ray diffractometry (PXRD), differential scanning calorimetry (DSC), and Fourier transform infrared (FTIR) spectroscopy. The effects of the operating parameters, such as sonication intensity, sonication duration, and solution concentration, on sonocrystallization were compared. The crystal size of salicylamide was reduced from 595 μm (the original size) and was efficiently manipulated to be between 40 and 80 μm. Moreover, compared with the crystal habits of unprocessed crystals and recrystallized crystals fabricated through conventional methods, the crystal habit of salicylamide could be modified to present a regular shape. The structure, thermal behavior, and spectrometric properties of sonocrystallized salicylamide were found to be in agreement with those of an unprocessed sample. For producing isoniazid derivative crystals, N′-(propan-2-ylidene)-isonicotinohydrazide was synthesized using isoniazid in acetone at 318 K. The resulting solution was then cooled by applying power ultrasound to isolate N′-(propan-2-ylidene)-isonicotinohydrazide crystals. The solid-state properties of the synthesized N′-(propan-2-ylidene)-isonicotinohydrazide was verified through PXRD, DSC, and FTIR spectroscopy. The feasibility of particle size manipulation was then demonstrated through sonocrystallization.

In this study, a case study to produce microcellular foam of a commercial thermoplastic polyurethane (TPU) through the supercritical carbon dioxide (CO₂) foaming process is presented. To explore the feasibility of TPU in medical device and biomedical application, a soft TPU with Shore hardness value of 70A was selected as the model compound. The effects of saturation temperature and saturation pressure ranging from 90 to 140 °C and 90 to 110 bar on the expansion ratio, cell size and cell density of the TPU foam were compared and discussed. Regarding the expansion ratio, the effect of saturation temperature was considerable and an intermediate saturation temperature of 100 °C was favorable to produce TPU microcellular foam with a high expansion ratio. On the other hand, the mean pore size and cell density of TPU foam can be efficiently manipulated by adjusting the saturation pressure. A high saturation pressure was beneficial to obtain TPU foam with small mean pore size and high cell density. This case study shows that the expansion ratio of TPU microcellular foam could be designed as high as 4.4. The cell size and cell density could be controlled within 12–40 μm and 5.0 × 10⁷–1.3 × 10⁹ cells/cm³, respectively.