The layered double hydroxides (LDHs) are nano-ordered layered compounds and well known for their ability to intercalate anionic compounds. Most popular LDHs are prepared conventionally only with divalent and trivalent cations. In this study, Co-Zr LDH consisting of divalent and tetravalent cations was prepared and reacted with monocarboxylic acids at room temperature. The Co-Zr LDH and intercalated compounds have been characterized by chemical analysis (C, H, N analysis, ICP, and ESCA), X-ray powder diffraction, IR spectra, thermal analysis, and Scanning electron microscope (SEM). The insertion of cyanate and carbonate anions into LDH was confirmed by chemical analysis and IR spectra. XRD patterns of the prepared Co-Zr LDH showed that the interlayer spacing of the LDH is 0.78 nm. The spacing was similar to that of usual LDH in which chloride, carbonate, or bromide anion is the guest. SEM images showed that the aging time plays a vital role in the morphology of Co-Zr LDH. The morphology of Co-Zr LDH is plate-like structure and/or fibrous structure depending on the aging time.