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In this research work, tri-metallic layered double hydroxides (NiZnAl-LDH) nano-sheets were efficiently synthesized by hydrothermal technique and applied for the decontamination of rhodamine B (Rh-B) and methyl orange (MO). Material characterizations confirm the formation of tri-metallic NiZnAl-LDH nano-sheets of continuous macrostructure skeleton with interconnected macropores. Several adsorption factors like initial concentration, pH of dyes solution, contact time and adsorbent dosage were investigated. Results exposed that synthesized NiZnAl-LDH perform best in basic medium for the removal of Rh-B and in mild acidic for that of MO. Also with 210 min contact time NiZnAl-LDH showed adsorption efficiency of 38.03 mg/g for Rh-B and 32.67 mg/g for that of MO. The Langmuir model perfectly defined the adsorption process on to the surface of NiZnAl-LDH as monolayer with relatively higher R² value (R² = 0 …