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Layered double hydroxides (abbreviated as LDHs) are one of the nanoordered layered compounds. The importance of layered compound is based on their ability to retain chemical species with electrical charges compatible to those of the layers. In this study we have reported the synthesis of nanosized layered double hydroxide (LDH) by co-precipitation method using two different surfactants as cetyl trimethyl ammonium bromide (CTAB) and octadecyl trimethyl ammonium bromide (ODTMA) having different critical micelle concentration (CMC) /chain length and its comparative results on calcined surface modified LDH (CS-LDH). The structure of surface modified layered double hydroxide (CS-LDH) synthesized is unique and has important advantages to the photocatalytic activity. LDH has significant number of application due to their structural, chemical properties etc., these compounds can be used as catalyst, adsorbents, anion exchanger. The photocatalytic activity of prepared surface modified CS-LDH was tested on degradation of the methylene blue (MB) dye in an aqueous solution. The surface characteristics of LDH and CS-LDH were examined using Energy Dispersive X-ray (EDX), Scanning Electron Microscopy (SEM), X-ray diffraction (XRD) and UV-Visible spectrophotometer for Photocatalytic activity under visible light using MB dye. It was observed that highly exfoliated and basal spacing in CS-LDH-ODTMA which enhanced photocatalytic activity (Approx. 60% degradation) than that of comparison to CS-LDH-CTAB (Approx. 32% degradation).