To create new nanosized catalysts for oxidative transformations of sulfur compounds of thiophene series, monometallic catalysts based on carbon nanotubes M/CNTs (M = Ce, Cu, Mo) were prepared with a variation of the synthesis method. The incipient wetness impregnation method, adsorption, and precipitation methods were applied for active component introduction onto CNTs. The effect of preparation mode on textural and structural characteristics of M/CNTs was investigated using a set of physicochemical methods (optical emission spectrometry with inductively coupled plasma, low-temperature nitrogen adsorption, X-ray phase analysis, Raman spectroscopy, and scanning electron microscopy). It was shown that precipitation and impregnation methods provide appropriate metal content in catalyst composition while adsorption is suitable for synthesizing samples with a low active component concentration. The kinds of active component species are similar (CeO2, Cu2O/Cu or MoO3/MoO2) but their distribution behavior and dispersion are controlled by the preparation mode. The using precipitation method for M/CNTs synthesis provides uniform distribution of the nanosized metal-containing particles on the carbon matrix surface.