Poly(vinyl acetate-co-methyl methacrylate)/Cloisite 30B, P(VAc-co-MMA)/C30B nanocomposite have been prepared via emulsion polymerization method. In the nanocomposite latex preparation sodium lauryl sulfate, ammonium persulfate, and poly(vinyl alcohol) were as anionic emulsifier, conventional anionic initiator, and stabilizer, respectively. The resulting P(VAc-co-MMA)/C30B nanocomposites with various filler contents were characterized using elemental analysis, Fourier transform infrared spectroscopy, X-ray diffraction (XRD), scanning electron microscopy, transmission electron microscopy (TEM), and atomic force microscopy. The effects of various C30B contents on the polymerization rate and monomer conversion of P(VAc-co-MMA)/C30B were studied. Thermal properties of the nanocomposite were studied by dynamic mechanical thermal analysis. The XRD and TEM results demonstrated that the synthesized polymer chains were aggregated into the C30B interlayer regions and consequently complete exfoliation was produced.