The use of clays as industrial catalysts requires optimization of modification methods during their preparation. The objective of this paper was to improve the traditional method of bentonite impregnation using ultrasound. For this purpose, three series of samples with Fe3+/clay molar ratios of 0.6–11 mmol/g were prepared, which differed in terms of preparation procedure. The first batch of samples was subjected to the conventional method of impregnation, where total synthesis of catalysts took 4 h. The other two series of samples were prepared with impregnation improved by ultrasound: preparation of Fe-polycation (5 min) and then its incorporation with a clay suspension for 5 and 10 min. The effect of clay preparation method on the catalyst stability and efficiency in a heterogeneous Fenton process was studied on aqueous solutions of synthetic Reactive Blue 4 dye. The catalysts prepared by the conventional method and the improved ultrasound method achieved high efficacy (91–97%, respectively), but their stability was different in the Fenton process. The catalysts prepared using ultrasound for 10 min exhibited greatest stability in the Fenton process. The catalysts synthesized with different Fe loadings displayed an increase in specific surface area and mesoporosity. Samples prepared by the improved impregnation method are comparable in terms of their characteristics with their counterparts prepared by the conventional method. It is thus possible to reduce the time taken by traditional catalyst synthesis by using optimized exposure time to ultrasonic waves.