We deposited Fe and Cu over zeolite NaX (Fe/NaX and Cu/NaX) by adsorption from effluent industrial wastewater. We synthesized the zeolite NaX by the hydrothermal method. 5 g of NaX completely adsorbed 350 and 380 mg of Fe and Cu from the industrial wastewater, respectively, in 6 h. The distribution of Fe and Cu over the NaX was uniform and amounted at 14 and 18 mass%, respectively. Fe and Cu modify the morphology of the NaX zeolite: the particle size increased from 9 μm to 10 μm for the former and decreased to 3 μm for the latter. Fe/NaX and Cu/NaX are less crystalline than NaX. BET analysis showed that the specific surface area decreased by 30 % and 50 % compared to NaX for Fe/NaX and Cu/NaX, but the ratio between meso‐ and micropores increased by 7 and 13 times, respectively. Fe/NaX and Cu/NaX synthesized by adsorption from industrial wastewater reduced +99 % of 4‐p‐nitrophenol to 4‐aminophenol in less than 100 s, which is comparable to noble metal.