Impact of simultanes application of mechanical stirring and ultrasound irradiation on the growth rate dynamics of borax crystals : diploma thesis

Glavni cilj ovoga rada bio je ispitati istovremeno djelovanje mehaničkog miješanja i ultrazvuka na dinamiku rasta kristala boraksa. Sonokristalizacija hlađenjem izvršena je u staklenom kristalizatoru, pri čemu je volumen kapljevine iznosio 2,65 dm 3 , a brzina hlađenja 6 °C h -1 . Brzine miješanja SBT miješala odgovarale su onima potrebnima za postizanje stanja potpune suspenzije (N JS ) po Zwieteringovom kriteriju, a amplitude ultrazvučnog djelovanja (A) iznosile su redom 0, 20, 25 i 30 %. Određena je promjena koncentracije matične otopine potenciometrijski, kao i promjena apsolutne prezasićenosti pri navedenim ultrazvučnim amplitudama pri čemu dobiveni rezultati pokazuju da ultrazvuk utječe na promjenu apsolutne prezasićenosti, a samim time i na promjenu veličine kristala. Prikazana je i promjena veličine kristala s vremenom koja pokazuje prosječno sitnije kristalne produkte s povećanjem amplitude ultrazvuka. Također, određeno je i vrijeme dostizanja konačne veličine kristala te utjecaji ultrazvuka i miješanja na brzinu rasta kristala i njihovu veličinsku raspodjelu metodom laserske difrakcije gdje je uočljivo da se vrijeme potrebno za nastajanje kristala konačne veličine povećava s povećanjem amplitude ultrazvuka, ali i da se raspodjela veličina kristala sužava. Određena je i snaga potrebna za izvođenje eksperimenta. Dobivene vrijednosti ukazuju na to da je utrošak snage izražen po jediničnoj masi otopine boraksa čak do 10 puta veći kod ultrazvučnog djelovanja nego kod mehaničkog miješanja. S obzirom na rezultate eksperimenta, više amplitude ultrazvuka ne čine proces sonokristalizacije učinkovitijim te se amplituda ultrazvuka od 20% čini optimalnom zbog toga što ima najkraće vrijeme dostizanja konačne veličine kristala i energetski je manje zahtjevna od onih pri 25 i 30 %. The primary goal of this thesis was to examine the effect of simultaneous application of mechanical stirring and ultrasound irradiation on borax crystals growth rate dynamics. The cooling sonocrystallization has been conducted in a glass crystallizer with the liquid volume being 2.65 dm 3 and the cooling rate of 6 °C h -1 . Stirring speeds of the SBT stirrer matched the ones required for achieving the state of a complete suspension (N JS ) by Zwietering's criterion, while amplitudes of the ultrasound were as follows: 0, 20, 25 and 30 %.The change of the mother liquor's concentration was determined potentiometrically as well as the change of the absolute supersaturation during above-mentioned amplitudes. According to results, ultrasound irradiation affects absolute supersaturation as well as the change of crystal size during the process. Given the measured sizes of crystals, change in crystal size over time was shown and it is noticeable that continuous sonocrystallization yields averagely smaller crystals. Also, the time required for crystals to attain their final size, effects of both stirring and ultrasound irradiation on the growth rate and the crystal distribution determined by laser diffraction were presented for each amplitude. In general, the time required for attaining the crystalline product of final size extends with an increase of ultrasound amplitude. At the same time, crystal size distribution narrows. Power needed to perform the experiment was also determined. Results suggest that power consumed per unit mass of borax solution by stirring is up to 10 times lower than that of ultrasound irradiation. Considering all obtained results, it can be said that higher ultrasound amplitudes do not imply a more effective sonocrystallization process and therefore, the amplitude of 20 % seems like the optimal one with reasons being that it ensures the shortest time needed for attaining the final size of the crystal as well as not being as costly in terms of energetics as the amplitudes of 25 i 30 %.