The invention discloses a preparation method of a p-CuO/n-CdS/ZnS composite semiconductor photochemical catalyst, which comprises the steps of: firstly, with an ammonium salt, a zinc salt, a cadmium salt, thiocarbamide and deionized water as raw materials, sequentially carrying out treatments such as microwave reaction, ultrasonic dispersion, heating reaction, washing, ultrasonic dispersion, filtering, drying, roasting, grinding and the like to obtain CdS/ZnS solid powder; and secondly, with the CdS/ZnS solid powder, a copper salt, alkali and deionized water as raw materials, sequentially carrying out treatments such as reaction, ultrasonic dispersion, decompression distillation, thermal treatment, washing, ultrasonic dispersion, filtering, drying, roasting, grinding and the like to obtain the p-CuO/n-CdS/ZnS composite semiconductor photochemical catalyst. Through compounding a p-type semiconductor CuO with n-type semiconductor CdS and ZnS, oxidization of holes to the CdS can be effectively reduced, the light corrosion rate of the CdS is decreased; and photoproduced electronics are effectively separated from the holes, thus the service life of the CdS is prolonged, and the photochemical catalysis efficiency of the p-CuO/n-CdS/ZnS composite semiconductor photochemical catalyst is increased. The method is simple, convenient and practical, and is beneficial to popularization.