This article contains the experimental and statistical data related to decolourization of Amido Black 10B using photocatalytic process. Box-Behnken experimental design (BBD) has been used to study the influence of operational parameters on photocatalytic oxidation of Amido Black 10B by using zinc oxide (ZnO) as a catalyst. This data set presents a concise description of experimental conditions for variable factors such as initial dye concentration of 100 ppm, oxidant dosage 20 mMol/L and catalyst dose 1g/L at natural pH for 4 hr of reaction time in presence of 12W intensity ultra-violet radiation were optimized for over a response parameter, decolorization efficiency of Amido Black 10B. The effects of decolorization on process variables were investigated by developing a mathematical model, results indicated that ZnO can be used as an efficient catalyst for the decolorization of Amido Black 10B. Analysis of variance (ANOVA) showed a high coefficient of statistical measure value (R
2
= 0.9915) and prediction of the driven regression model was found to be satisfactory.