A new mixed matrix polyvinyl chloride-based heterogeneous cation exchange membrane was prepared by incorporation of carboxy methyl cellulose-co-Fe3O4 nanoparticles through solution casting technique. The effect of simultaneous using of carboxy methyl cellulose and iron oxide nanoparticles in the casting solution on the physicochemical properties of membranes was studied. SOM images showed uniform particles distribution and uniform surfaces for the membranes relatively. The SEM images exhibited regular direction/spatial orientation for the CMC-co-Fe3O4 nanoparticles in the membrane matrix. XRD patterns showed that membrane heterogeneity was enhanced by using of Fe3O4 nanoparticles. Membrane ion exchange capacity, membrane surface hydrophilicity, membrane potential, surface charge density, transport number, selectivity, and ionic flux were increased by using CMC/Fe3O4 nanoparticles in membrane matrix. Results showed that membrane areal electrical resistance was declined up to 3.8 Ω cm2 by utilizing CMC/Fe3O4 nanoparticles in the casting solution. Also PVC/CMC-co-Fe3O4 membrane showed higher transport number, selectivity, flux, and electrical conductivity compared to PVC/CMC membrane and unmodified ones. Electrodialysis experiment in laboratory scale showed higher dialytic rate in lead ions removal for PVC/CMCco-Fe3O4 nanoparticle-mixed matrix ion exchange membrane compared to PVC/CMC membrane and pristine one.