This paper reported the preparation of styrene sulfonate intercalated layered double hydroxides (LDHs) material, SS-LDHs by coprecipitation method, followed by in-situ polymerization of the monomers in the interlayer space of LDHs. The polymerization reaction was monitored by UV and NMR. It is confirmed that when the reaction occurred at 100℃ for 24 h, part of monomers did not react .When the reaction was carried out at 150℃, the polymeriza tion of the intercalated monomers is complete to afford the polymer intercalated product PSS-LDHs. During the polymerization process, the layered structure remains well. At thesame time the gallery height increases with the lengthening of reaction time. This is preliminarily because that the PSS becomes more swelling with the amount of water it absorbs due to its hygroscopicity property.