The aim of this work was to study the stability and morphological properties of polystyrene latex containing kaolinite as a filler during the process of synthesis of nanocomposites viaemulsion polymerization. Nanocomposites with 1, 3, and 5 wt% of kaolinite were prepared. Latexes with 1 to 3 wt% of kaolinite were stable during the polymerization reaction. Hydrodynamic diameters of 93.68 and 82.11 nm were found for latexes with 1 and 3 wt% of kaolinite, respectively. The quantities of 1 to 3 wt% of kaolinite added during the reaction did not influence the reaction conversion curves or the number of particles. X-ray diffraction (XRD) and unconventional techniques of scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HRTEM) showed the presence of exfoliated and intercalated structures of the kaolinite.