In this work, a thin layer of manganese dioxide/zinc oxide (MnO2/ZnO) was deposited on a glass substrate using a two-stage chemical bath deposition (CBD) method to optimize the photocatalytic activities in the reduction of 2-nitrophenol. The effects of ethanol and butanol as reducing agents on the surface morphology, wettability, thermal insulation, and photocatalytic activities were investigated. At 100 kX magnification, the micrographs clearly showed the MnO2 nanoparticles embedded in the thin film for the single and two-stage CBD, with the particle agglomeration being more pronounced for the two-stage CBD. ZnO has been diffused into MnO2 for both reducing agents, albeit with lower integration. In addition, the images show that the prepared catalyst in butanol gradually granulates with increasing ZnO content compared to ethanol, affecting its particle size and the active surface. The thermal insulation test reveals that the sample with 10 % ZnO reduces the temperature by 4 °C, which improves the durability and stability of the catalyst. The exact composition of the sample demonstrates the optimum photodegradation of 2-nitrophenol with an efficiency of 94.96 % (0.0301 min−1). The measurement of the water contact angle also showed an increase in the contact angle (CA) with a value of 55.6°. Based on the findings, it was found that photocatalysts using butanol as a reducing agent demonstrate higher efficiency in reducing of 2-nitrophenol as compared to ethanol due to its homogeneous distribution and large surface area. This study brought a new direction in impact of reducing agent on void free and dense thin film of the MnO2/ZnO catalyst in reducing of persistent water pollutants under visible light irradiation.