Synthesis of metal catalyst with wet impregnation method

Namen diplomskega dela je bil sintetizirati kovinske kislinske katalizatorje z metodo mokre impregnacije aktivnih soli AlCl3, Al(NO3)3 in Al-izopropoksida na nosilec γ–Al2O3. Za karakterizacijo sintetiziranih katalizatorjev smo uporabili različne metode, kot so FTIR (Fourier-transform infrared spectroscopy), BET (Brunauer-Emmett-Teller surface area analysis), DSC (differential scanning calorimetry), TGA (thermogravimetric analysis) in NH3 fizisorpcija. Aktivnost sintetiziranih katalizatorjev smo preizkusili na reakciji esterifikacije miristinske kisline z metanolom. Vzorce smo analizirali s HPLC povezanim z UV-VIS detektorjem. Iz umeritvene krivulje standardnih raztopin miristinske kisline in metil miristata smo določili koncentracije in nadalje presnovo miristinske kisline. Izkazalo se je, da so katalizatorji, ki imajo impregnirano aktivno sol v večjih masnih deležih, bolj učinkoviti pri reakciji esterifikacije, kot pa katalizatorji z manjšim masnim deležem soli. Dobljene eksperimentalne podatke smo opisali z Langmuir-Hinshelwood-Hougen-Watson-ovim modelom. Določili smo konstante proizvodnosti pri različnih temperaturah (50, 55, 60 in 64,5) °C in različnih masah dodanega katalizatorja (0,2, 0,15, 0,1 in 0,05) g.The purpose of this bachelor’s thesis was to synthesize metal acid catalysts with the method of wet impregnation of the active salt AlCl3, Al(NO3)3 and Al-isopropoxide on γ – Al2O3 support. Various methods such as FTIR (Fourier-transform infrared spectroscopy), BET (Brunauer-Emmett-Teller surface area analysis), DSC (differential scanning calorimetry), TGA (thermogravimetric analysis) and NH3 physisorption were used to characterize the synthesized catalysts. The activity of the synthesized catalysts was tested on the esterification reaction of myristic acid with methanol. Samples were analyzed by HPLC, coupled with a UV-VIS detector. From the calibration curve of standard solutions of myristic acid and methyl myristate, the concentrations and conversion rates of myristic acid were determined. Catalysts having an impregnated active salt in higher mass fractions have been shown to be more effective in the esterification reaction than catalysts with a lower mass fraction. The obtained experimental data were described by the Langmuir-Hinshelwood-Hougen-Watson model. Productivity constants were determined at different temperatures (50, 55, 60 and 64.5) ° C and different masses of added catalyst (0.2, 0.15, 0.1 and 0.05) g