The aims of this study, firstly, to obtain high degree of clay exfoliation in the epoxy matrix by three dispersion methods such as normal mixing, shear mixing, and high-speed mixing and, secondly, to investigate corrosion behavior of epoxy/organoclay nanocomposite, immersion test, weight change, and penetration behavior were conducted. From the three mixing methods, the high-speed mixing method showed larger clay interlayer distance, smaller clay aggregate, and more homogeneity and expectedly resulted in high anticorrosive properties. Penetration depths of these nanocomposites showed a small difference; however, the most noticeable improvements in anticorrosion performance for epoxy/organoclay nanocomposites under high-speed mixing method were found to reduce penetration and weight uptake which are described via the model of nanoparticulate-filled structure and discussed in corrosion protection mechanism against environmental liquid penetration.