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Furfural (FF), levulinska kislina (LA) in hidroksimetilfurfural (HMF), predstavljajo ključne intermediate različnih kemijskih spojin, pomembnih za razvoj zelenega gospodarstva kot tudi zdravilnih učinkovin v farmacevtski industriji. Pridobljene so iz sladkorjev biomase kot so celuloza, glukoza, heksoza, v primeru HMF/LA in hemiceluloze, ksiloze in pentoze v primeru FF. Način pridobivanja je tako pogosto hidroloza sladkorjev, v nadaljevanju pa tudi hidrogenacija in oksidacija. Kljub pomembnosti molekul sta njihova detekcija s procesno-analiznimi tehnologijami in temperaturna odvisnost topnosti slabo raziskani. Zato bomo v nalogi poročali o topnosti posameznih spojin (FF, HMF, LA) v izbranih topilih pri različnih temperaturah : n-heksan, cikloheksan, benzen, toluen, 1,4-dioksan, dietileter, diklorometan, tetrahidrofuran, etilacetat, aceton, dimetilformamid, acetonitril, dimetilsulfoksid, mravljična kislina, n-butanol, n- propanol, etanol, metanol in voda. Pridobljeni podatki so izjemnega pomena za sintezo, čiščenje in kasnejše kemijske reakcije molekul. Uporabljena PAT (Process Analytical Technology) metoda, ATR-FTIR (Attenuated Total Reflectance Fourier-Transform Infrared Spectroscopy) nam omogoča izračun termodinamičnih podatkov topnosti, ki nam kasneje v pomagajo pri načrtovanju kristalizacije kot procesa čiščenja in izolacije molekul levulinske kisline in hidroksimetilfurfurala. Pri nadzorovanju procesa nam je v pomoč FBRM (Focused Beam Reflectance Measurement) metoda, s katero lahko določimo ključne podatke, kot porazdelitev in velikost delcev ter začetno oz. »onset« temperaturo kristalizacije. Furfural (FF), levulinic acid (LA) and hydroxymethylfurfural (HMF), represent key intermediates for various chemical compounds important in both green economy development and API (active pharmaceutical ingredient) synthesis in pharmaceutical industry. Obtained from biomass derived sugars i.e. either cellulose, glucose, hexoses, etc. (HMF/LA), or hemicellulose, xylose and pentose (FF). Conversion of sugars is mainly done by hydrolysis which later on continues with hydrogenation or oxidation. Despite the great importance of these molecules are PAT (Process Analytical Technology) detection and temperature dependence of solubility poorly researched. Thus, the temperature dependence solubility data for solutions of all molecules in selected spectrum of solvents: n- hexane, cyclohexane, benzene, toluene, 1,4-dioxane, diethyl ether, dichloromethane, tetrahydrofuran, ethyl acetate, acetone, dimethylformamide, acetonitrile, dimethyl sulfoxide, formic acid, n-butanol, n-propanol, ethanol, methanol and water are collected and reported in this thesis. The obtained data are of extreme importance for synthesis, purification and subsequent chemical reactions. The PAT (Process Analytical Technology) method, ATR-FTIR (Attenuated Total Reflectance Fourier-Transform Infrared Spectroscopy) allowed us, to collect the data used for temperature dependence of solubility calculations. Obtained information helped us with the design of crystallization process, as potential method for purification and isolation of levulinic acid and hydroxymethylfurfural molecules. Crystallization process was monitored by FBRM (Focused Beam Reflectance Measurement) method, enabling determination of all key data particle size and distribution and onset crystallization temperature. |
