This research deals with the preparation of heterogeneous cation exchange membranes by solution-casting techniques using S-polyvinylchloride (S-PVC) and polycarbonate (PC) as binders, cation exchange resin powder as functional groups agent, and tetrahydrofuran as solvent. The effects of polymer binder type and resin ratio loading on morphological, electrochemical, and mechanical properties of prepared membranes were studied and evaluated. Scanning electron microscopy and scanning optical microscopy were used for the membranes structure investigation. Images showed that increase of resin loading in casting solution resulted in a highly uniform phase forming. Moreover resin particles were distributed more uniformly in polycarbonate membranes compared to the polyvinylchloride ones. The water content, surface hydrophilicity, ion exchange capacity, ion concentration, permselectivity, membrane potential, surface charge density, transport number, ionic permeability, flux of ions, and current efficiency were enhanced for the prepared membranes by increase in resin ratio loading. Moreover, the increase of resin ratio in casting solution reduced the mechanical strength of the prepared membranes. The mechanical strength of S-PVC membrane was higher than the PC ones. Furthermore, the increment of resin content caused some decreases in areal electrical resistance and oxidative stability of the prepared membranes. Home-made membranes exhibited appropriate electrochemical properties in comparison with a tested commercial heterogeneous cation exchange membrane in the same experimental conditions. Swelling of the prepared membranes was also negligible compared to the commercial type.