With regard to the widespread industrial applications of nanocomposites, a 4A zeolite based-NiCo2O4 nanocomposite was synthesized by using hydrothermal method. The 4A zeolite was synthesized from metakaolin and as comparative point of view, NiCo2O4 nano spinel precipitated by sedimentation, hydrothermal and solvothermal methods. The results showed that hydrothermal-based NiCo2O4 nano spinel has a great morphology for construction of NiCo2O4@4A nanocomposite. The comparative XRD analysis among 4A zeolite, NiCo2O4 nano spinel, and NiCo2O4@4A nanocomposite showed that the XRD pattern of NiCo2O4@4A has the highest alignment with 4A zeolite, NiCo2O4 nano spinel patterns. The spreading of 4A zeolite peaks in XRD pattern of NiCo2O4@4A reveal that NiCo2O4 nano spinel fixed on the zeolite surface. With regard to the consequences.