A novel polyvinyl alcohol/alginate/zeolite nanohybrid adsorbent for the adsorption of Ni(II) and Co(II) metal ions was prepared by the casting method. The prepared adsorbent was characterized by Fourier transform infrared spectroscopy, scanning electron microscopy as well as Barrett-Joyner-Halenda and Brunauer-Emmett-Teller analyses. The optimum adsorption conditions in terms of content of zeolite nanoparticles, adsorbent dosage, and initial pH were determined. The kinetic data for both ions were well described by the double-exponential kinetic model. The obtained Langmuir maximum adsorption capacities of Ni(II) and Co(II) metal ions were 81.51 and 79.58 mg g(-1), respectively. The adsorption/desorption experiments showed a good performance after 5 cycles of adsorption.