Batik industryiswell known intheEast Coast of Malaysia, particularly in Terengganu and Kelantan. This industry consumes a lot of waterforthe batik making processwhich contributes tohigh dischargeof wastewater containingexcess dye pollutants. Hence,in this study, ananionic clayofnickel/aluminium-layered double hydroxide (NiAL) was investigatedas a potential adsorbent for the removal of anionic dyeof Eriochrome Black T (EBT). The NiAL was synthesized via self-assemblymethod and characterization of NiALwas carried outusing powder X-ray diffraction (PXRD) and Fourier transform infrared spectrophotometer (FTIR). The composition and morphology of NiAL was further analyzed using carbon, hydrogen, nitrogen, sulphur elemental analyzer (CHNS), thermogravimetric analyzer (TGA) and scanning electron microscope (SEM).The potential of NiAL as an adsorbent for the removal ofEBT in aqueous solution was tested at different dosages of NiAL. Theadsorptionabilitywasanalyzedby using two common adsorption isotherms, which were Langmuir and Freundlich models. The adsorption of EBT onto NiAL was governedby Freundlich isotherm model indicating that the adsorption occurs in heterogeneous system.