This study focuses on the production and purification of multi-walled carbon nanotubes (P-CNTs) via a catalytic chemical vapor deposition method and subsequent functionalization with amino polyethylene glycol (NH2-PEG) and its mixture with polyhydroxybutyrate (PHB) through a multi-step purification process to produce NH2-PEG-CNTs and NH2-PEG-PHB-CNTs, respectively. The developed nanoadsorbents were used to treat electroplating wastewater via batch adsorption to sorb potentially toxic metals and emerging pollutants. The nanoadsorbents were characterized before and after treatment with wastewater after thermal regeneration analyzed using HRSEM/EDS/SAED, DLS Nanozetasizer, BET, TGA/DTG, and FTIR. The nanoadsorbents showed a homogeneous distribution of clean and smooth crystalline interwoven tubular/cylindrical shapes and sizes, with broad polydispersed/high aspect ratio, large surface area, mesopores, and functional groups. The batch adsorption study showed simultaneous multi-capturing of toxic metals from industrial electroplating wastewater with a directly proportional relationship between contact time, adsorbent dosage andtemperature, and electrostatic activities via the positive surface charge of the nanoadsorbents (pH > pHzpc). The highest removal of Fe (15.86 %), Ni (79.82 %), Pb (79.82 %), and Cu (84.97 %) were obtained using NH2-PEG-PHB-CNTs. In addition, the ANOVA results show that the adsorption process depends on other parameters such as the concentration of toxic metals in the wastewater, its hydration energy, electronegativity, ionic mobility in the electrostatic activities, pH of the nanoadsorbents, water holding capacity of the polymer-functionalized nanoadsorbents, and synergistic effects of the bi-polymer. Moreover, the nanoadsorbents have a stable morphology after thermal regeneration for reusability purposes, and treated wastewater can be safely reused in the electroplating industry or for other purposes, such as agriculture.