<p>This study investigates copper/aluminum dual-layer hydroxide adsorbents with distinct morphologies as efficient cationic adsorbents for humic acid (HA) removal. The adsorbents were synthesized through the co-precipitation and hydrothermal methods. XRD analysis confirmed the high crystallinity and nanometric crystal size, while FTIR analysis validated the anion functional groups present in the adsorbents. EDX analysis further confirmed the composition of the synthesized adsorbents. BET analysis indicated a small surface area and nanometric pore size distribution of the adsorbents. Experimental results indicated the 50 mg L⁻¹ initial concentration, the adsorbent dosage of 0.02 g L⁻¹ for lamellar adsorbent and 0.05 g L⁻¹ for spherical adsorbent, pH = 4, and 25 °C temperature were optimal conditions for efficient HA removal. Isotherm studies demonstrated that the Langmuir isotherm model best fitted with experimental HA adsorption data using both lamellar and spherical adsorbents with R² &gt; 0.99 for lamellar and spherical adsorbents, respectively. Maximum adsorption capacities were determined to be 277.7 mg g⁻¹ and 285.7 mg g⁻¹ for the lamellar and spherical adsorbents, respectively. Moreover, kinetic studies revealed that the pseudo-second-order kinetic model exhibited the best fit for both adsorbents, with R² &gt; 0.99. Finally, recovery studies indicated that the lamellar and spherical adsorbents showed a 60% and 70% reduction in efficiency after 5 consecutive cycles of adsorption-regeneration, demonstrating their potential for repeated use.</p> Graphical abstract <p></p>