Advanced automotive fleet repair facility wastewater treatment was investigated with Zero-Valent Iron/Hydrogen Peroxide (Air/ZVI/H2O2) process for different process parameters: ZVI and H2O2 doses, time, pH. The highest Chemical Oxygen Demand (COD) removal efficiency, 76%, was achieved for ZVI/H2O2 doses 4000/1900 mg/L, 120 min process time, pH 3.0. COD decreased from 933 to 227 mg/L. In optimal process conditions odor and color were also completely removed. COD removal efficiency was increasing with ZVI dose. Change pH value below and over 3.0 causes a rapid decrease in the treatment effectiveness. The Air/ZVI/H2O2 process kinetics can be described as d[COD]/dt = −a [COD]tm, where ‘t’ corresponds with time and ‘a’ and ‘m’ are constants that depend on the initial reagent concentrations. H2O2 influence on process effect was assessed. COD removal could be up to 40% (560 mg/L) for Air/ZVI process. The FeCl3 coagulation effect was also evaluated. The best coagulation results were obtained for 700 mg/L Fe3+ dose, that was slightly higher than dissolved Fe used in ZVI/H2O2 process. COD was decreased to 509 mg/L.