ABSTRACT
This study synthesized UiO-66, a typical Zr-Metal Organic Framework (MOF), by using an ultrasound-assisted synthesis method to reduce the synthesis time. This method was short-time ultrasound irradiation at the initial stage of the reaction. As compared with average particle size of conventional solvothermal method (=192 nm), averaged particle size by the ultrasound-assisted synthesis method showed particle sizes that were smaller on average, ranging from 56 to 155 nm. In order to compare the relative reaction rates of the solvothermal method and the ultrasound-assisted synthesis method, the cloudiness of the reaction solution in the reactor was observed with a video camera, and the luminance was calculated from the images obtained by the video camera. It was found that the ultrasound-assisted synthesis method showed a faster increase in luminance and shorter induction time than the solvothermal method. The slope of the luminance increase during the transient period was also found to become increase with the addition of ultrasound, which also affects the growth of particles. Observation of the aliquoted reaction solution confirmed that particle growth was faster in the ultrasound-assisted synthesis method than in the solvothermal method. Numerical simulations were also performed using MATLAB ver. 5.5 to analyze the unique reaction field generated by ultrasound. Bubble radius and temperature inside a cavitation bubble was obtained using the Keller-Miksis equation, which reproduces the motion of a single bubble. The bubble radius expanded and contracted repeatedly according to the ultrasound sound pressure, and eventually collapsed. The temperature at the time of collapse was extremely high, exceeding 17,000 K. It was confirmed that the high-temperature reaction field generated by ultrasound irradiation promoted nucleation, leading to a reduction in particle size and induction time.
ABSTRACT
This study investigated the position of ultrasonic irradiation source and reactor geometry on fragmentation rate of a layered compound, α-zirconium phosphate (α-ZrP). By numerically solving the acoustic pressure distribution using COMSOL Multiphysics®, it is clarified the mechanism whereby the operating factors influenced the α-ZrP dispersion to make a suggestion of guideline of the process design method. Two vessels made of glass with a flat-bottom and a spherical-bottom, respectively, were used. Although the flat-bottom vessel at lower horn position showed the best performance of fragmentation, the region of high acoustic pressure field in the flat bottom vessel sharply narrowed and the transmittance became prominently low. On the other hand, no significant difference of the transmittance value in the spherical bottom vessel between the cases of low and high horn positions could be observed and the spherical bottom vessel was robust for the horn position. These results suggest that not only the magnitude of acoustic pressure but also the size of high acoustic pressure region is also an important factor and a spherical bottom vessel is one of suitable shape which gives large size of high acoustic pressure region regardless of the horn position.
