Dicofol is an Organochlorine pesticide. Dicofol is used for variety of fruit, vegetable and field crops. It is moderately toxic to humans and highly toxic to aquatic animals. The (Ni, Zn) dually doped multiwalled carbon nanotubes (Ni/Zn-MWCNTs) were used as catalyst adsorbent (nanocatalyst) for the degradation of dicofol. Nanomaterials have been the subject of wide research with interesting properties like size and shape depending optical and electrical properties. There are so many preparation techniques have accounted for the synthesis of nanorods and multiwalled carbon nanotubes including chemical reduction, laser treatment, co-precipitation, thermal hydrolysis, hydrolysis, hydrothermal, chemical vapour deposition, photochemical methods and biologically related synthetic methods, electro mechanical. In present study nanostructured samples of Ni doped ZnO nanorods were synthesized by Co-precipitation method. Multiwalled carbon nanotubes were synthesized by chemical vapour deposition method. The synthesis of (Ni, Zn) dually doped multiwalled carbon nanotubes using Co-precipitation method. The high yield and high product purity advantages of the coprecipitaion method. As a part of research the size of (Ni, Zn) dually doped Multiwalled carbon nanotubes were analyzed using various analyzing instruments like the Scanning electron microscope (SEM), Fourier transform infrared spectroscopy (FTIR), X-Ray Diffraction. With the help of the analyzing methods the nanotubes size was characterized and the properties were studied. The maximum percentage degradation of dicofol was obtained by varying different parameters like time (84.96), Dosage (89.44), pH (94.52), rpm (96.47), initial concentration (97.47) and at Temperature of 318 K. The final %degradation of dicofol obtained under the optimum conditions is 99.2%. Further, the adsorption kinetics (pseudo-first order, pseudo-second order, Elovich), isotherms (Langmuir, Freundlich, Temkin) and thermodynamic studies are also discussed.