As a preliminary work for the preparation of nylon 6/clay nanocomposites by reactive extrusion, nylon 6/clay nanocomposites were prepared by anionic polymerization in a flask. In order to investigate the effect of the intercalation of clay layers, the clay feeding times, such as in pre-mixing where the clay was fed before initiation of polymerization and in after-mixing method where the clay was fed after initiation of polymerization, were changed. The appearance of the WAXD peak of nanocomposites prepared by the pre-mixing method was obvious and the tensile strength was decreased compared with that of pure nylon 6, which indicates that the clay layers were not dispersed and distributed. During the preparation of the nanocomposites by the after-mixing method, disordering of the clay layers was observed with increasing clay addition time and was suspected to result from the rapid polymerization of nylon 6 within the clay layers.