In this study, NiAl-LDH was modified with hydrochar using the NiAl-Hydrochar composite coprecipitation method. Materials were characterized by XRD and FT-IR analysis. XRD diffractogram and FT-IR spectra show that the NiAl-Hydrochar composite material has the characteristics of the precursors. NiAl- Hydrochar composite materials have a large adsorption capacity to adsorb cationic dyes. The adsorption follows the Langmuir adsorption isotherm model with the maximum capacity (Qmax) of the NiAl-Hydrochar composite material reaching 256.410 mg/g for malachite green and the adsorption process takes place spontaneously and endothermically. The regeneration process of NiAl-Hydrochar composites was more stable and the decrease was not significant (>70%). The selectivity of the dye mixture showed that the adsorbent was more selective for malachite green dye compared to methylene blue and rhodamine-B.