20.500.12556/DKUM-90436 Impregnacija grafen oksida za uporabo pri kataliziranih reakcijah magistrsko delo Impregnation of graphene oxide for use in catalyzed reactions Industrijski proizvodni postopki pogosto ustvarjajo škodljive stranske proizvode, ki ogrožajo zdravje in okolje. V okviru eksperimentalnega dela smo preučevali možnost zmanjšanja teh škodljivih produktov z razvojem učinkovitejših katalizatorjev, sintetiziranjem grafen oksida in vezavo soli AlCl3. Pripravili smo štiri katalizatorje z različnimi koncentracijami impregnirane soli. Sintetizirane katalizatorje smo testirali s naslednjimi metodami: infrardečo spektroskopijo s Fourier-jevo transformacijo, metodo za merjenje adsorpcije plina, vrstično elektronsko mikroskopijo, dinamično sipanje svetlobe, diferenčno dinamično kalorimetrijo, termogravimetrično kalorimetrijo, temperaturno programirano desorpcijo , ter na koncu izvedli reakcijo esterifikacije, kjer smo koncentracijo nastalega produkta določili z uporabo plinskega kromatografa. Z metodo infrardeče spektroskopije smo potrdili uspešno sintezo grafen oksida po Hummer-jevi metodi. Glede na rezultate diferenčne dinamične kalorimetrije smo ugotovili, da so vzorci brez nečistoč, razen prisotnosti vezane vode. S temperaturno programirano desorpcijo smo razkrili, da ima katalizator kGO – 20 mg AlCl3 največ aktivnih kislinskih mest. Z uporabo metode dinamičnega sipanja svetlobe smo ugotovili, da so vzorci homogeni, z največjo velikostjo delcev pri katalizatorju kGO – 20 mg AlCl3 (169,7 nm). Iz rezultatov analize vrstične elektronske mikroskopije je razvidno, da so delci kalciniranih in nekalciniranih vzorcev različnih velikosti. S termogravimetrično kalorimetrijo smo ugotovili, da se masa vzorcev linearno zmanjšuje z višanjem temperature. Glede na rezultate metode za merjenje adsorpcije plina smo razbrali, da so vzorci mezoporozni, pri čemer je kGO – 20 mg AlCl3 imel najboljšo specifično površino in volumen por. Pri reakciji esterifikacije miristinske kisline z metanolom se je izkazalo, da s katalizatorjem GO – 10 mg AlCl3 dosežemo 100 % presnovo že po eni uri, medtem ko smo z uporabo katalizatorja kGO – 20 mg AlCl3 dosegli najslabšo presnovo (36 %). Povzamemo lahko, da kombinacija nosilca grafen oksida in impregnirane soli AlCl3 predstavlja potencial za razvoj učinkovitih katalizatorjev. Industrial production processes often generate harmful by-products that endanger health and the environment. Experimental work has investigated the possibility of reducing these harmful products by developing more efficient catalysts, synthesising graphene oxide and fixing AlCl3 salts. Four catalysts were prepared with different concentrations of impregnated salt. The synthesised catalysts were tested by the following methods: Fourier transform infrared spectroscopy, gas adsorption method, in-line electron microscopy, dynamic light scattering, differential dynamic scanning calorimetry, thermogravimetric calorimetry, temperature-programmed desorption, and finally an esterification reaction was carried out, where the concentration of the resulting product was determined using a gas chromatograph. The successful synthesis of graphene oxide by the Hummer method was confirmed by infrared spectroscopy. According to the results of differential dynamic calorimetry, the samples were found to be free from impurities, except for the presence of bound water. Temperature-programmed desorption revealed that the kGO-20 mg AlCl3 catalyst has the highest number of active acid sites. Using the dynamic light scattering method, the samples were found to be homogeneous, with the largest particle size for the kGO-20 mg AlCl3 catalyst (169,7 nm). From the results of the in-line electron microscopy analysis, it is evident that the particles of the calcined and the non-calcined samples are of different sizes. Thermogravimetric calorimetry showed that the mass of the samples decreased linearly with increasing temperature. According to the results of the gas adsorption method, the samples were found to be mesoporous, with kGO - 20 mg AlCl3 having the best specific surface area and pore volume. In the esterification reaction of myristic acid with methanol, it was found that the catalyst GO - 10 mg AlCl3 achieved 100% digestion after only one hour, while the catalyst kGO - 20 mg AlCl3 achieved the worst digestion (36%). In conclusion, the combination of a graphene oxide support and an impregnated salt of AlCl3 represents a potential for the development of efficient catalysts. mokra impregnacija katalizator grafen oksid esterifikacija Hummer-jeva metoda plinska kromatografija wet impregnation catalyst graphene oxide esterification Hummer method gas chromatography true true false [T. Cmager] Slovenski jezik Angleški jezik Magistrsko delo/naloga 2024-09-03 17:10:22 2024-09-10 13:49:06 2024-11-30 03:13:18 0000-00-00 00:00:00 2024 0 Maribor 0 Maribor 1 spletni vir (1 datoteka PDF (VIII, 38 f.)) 0000-00-00 NiDoloceno NiDoloceno NiDoloceno 0000-00-00 0000-00-00 0000-00-00 66.097.3:661.666(043.2) 217029123 MAG_Cmager_Tjasa_2024.pdf MAG_Cmager_Tjasa_2024.pdf 1 32A58DA37A5C9F82ABA544571D7EBCAC fc2f7a6a7b77013291e93721ea6b3bd7f45e1dd6bf5b53f730f3a6ac9e260239 1cb52d53-6eae-11ef-a573-00155d000105 https://dk.um.si/Dokument.php?lang=slv&id=184719 Fakulteta za kemijo in kemijsko tehnologijo 0 0 0