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This research incorporates iron-loaded crosslinked chitosan (CS) polymeric structure into the interlayer lattice space of Montmorillonite clay (MT) to enhance the phosphate adsorption capacity of MT. The synthesized Fe-loaded crosslinked chitosan montmorillonite composite (Fe-CS-MT) is evaluated effectively for phosphate removal from aqueous media. Batch adsorption experiments optimized the influence of adsorption parameters, i.e., contact time (50 min), solution pH (3), and adsorbent dosage (2 g L−1) for phosphate removal. The experimental results of equilibrium and kinetic studies indicated that phosphate adsorption on Fe-CS-MT follows Pseudo-second-order kinetic and Freundlich isotherm models with a high degree of accuracy. A series of analytical tools used to profile the investigated material's surface features involves CHNS Analyser, SEM-EDX, FTIR, XRD, XRF, UV-Visible Spectrophotometer, TGA, DSC, and surface analysis. The calculations of the thermodynamic study confirmed the endothermic and spontaneous nature of the phosphate adsorption process. This study presents an eco-friendly adsorbent tested in natural conditions to assess the feasibility of removing phosphate from an aqueous phase.