This work is devoted to the synthesis of a new type of adsorbent based on maleic anhydride styrene copolymer (MAST) and N,N`-diphenylguanidine (S) and its modification with 4,4'-(ethane-1,2-diylbis(azanylylidene))bis(pentane-2-one) (S+R). Adsorption study of Fe (III) ions with this adsorbent has been carried out. Effects of the pH value, contact time, ionic strength and the initial concentration of metal ions on the adsorption capacity of the product have been studied. In the course of research, several adsorption isotherms and kinetic models have been studied and the equilibrium data has been found to agree well with the pseudo-second-order model, and the pseudo-second-order model can describe the adsorption process. The results best fit the Langmuir adsorption isotherm model. The studies have shown that compared to the initial product (S), for which the adsorption capacity was 404.88 mg/g, the reagent-modified adsorbent (S+R) shows higher adsorption capacity over Fe(III) ions which is equal to 890.68 mg/g. Synthesized adsorbent was characterized by the Scanning Electron Microscopy (SEM) with Energy Dispersive X-ray Spectroscopy (EDS) and Ultraviolet-visible Spectroscopy (Uv/Vis). Temperature stability of adsorbent has been studied by thermal analysis methods (TG, DTA, DDTA)