The organoclay was prepared by alkylammonium ions and silane coupling agent modifying Na-Clay through Solid State Method and two kinds of silane coupling agents, KH-560 and KH-550, were comparatively studied. The X-ray diffraction patterns and the transmission electron microscopy photographs show that Polyvinyl Chloride (PVC)/organoclay nanocomposites were prepared by melt intercalation. The PVC/Org-560 nanocomposites, which were modified by silane coupling agent KH-560, possess intercalated structure and the PVC/Org-550 nanocomposites, which were modified by silane coupling agent KH-550, are mainly exfoliated structure. The mechanical properties of the PVC/Org-550 nanocomposite are much better than those of PVC/Org-560 nanocomposite.