As emerging organic agricultural pollutants, carbamate pesticides can react with other contaminants in aquatic environments

to produce new toxic compounds threatening aquatic life and ecosystems. This study introduces a novel, nonhazardous, and

greener method to synthesize a cross-linked ZnO/αFe 2 O 3 nano-photocatalyst to treat carbamate pesticides via ball milling.

ZnO/αFe 2 O 3 was characterized through various methods, including XRD, EDX, XRF, DRS, BET, FE-SEM, PL, and FTIR

analyses. Using the Response Surface Methodology (RSM), the ability of ZnO/αFe 2 O 3 nano-photocatalyst to remove carbamate

from synthesized wastewater was assessed. The BET result indicated a decrease in the diameter of the nanocomposite

size after the synthesis. At the same time, the BET surface area and total pores increased from 4.9871 m 2 .g −1 and 0.02806

cm 3 .g −1 to 6.8524 m 2 .g −1 and 0.069497 cm 3 .g −1 , respectively. In addition, the band-gap energy decreased from 3.179 eV for

ZnO to 1.907 eV for ZnO/αFe 2 O 3 and eventually reached 1.878 eV for heat-treated ZnO/αFe 2 O 3 nanocomposite. The catalyst

concentrations used in the experiments were 0.5, 1, and 1.5 g/L. The solution pH was set to 5, 8, and 11, and three diff erent

residence times of 1, 2, and 3 h were used. The model’s results indicated a strong agreement between the experimental and

predicted data (R 2 = 0.99). When the nanocomposite’s concentration, pH, and retention time were set at 1 g/L ZnO/αFe 2 O 3 ,

8.51, and 3 h respectively, the optimized conditions predicted a removal effi ciency of 89%. In addition, the cost of COD

removal was reduced by 50% using ball milling and heat-treatment synthesis. The photocatalyst’s reusability was tested in

three stages, and the outcomes demonstrated its stability throughout these three stages.