The nano-photocatalyst of Cu-Al-Layered Double [email protected] Carbon Nitride ([email protected] NPC) was synthesized via a fast and cheap method, characterized, and applied for photocatalytic degradation of tetracycline (TC) antibiotic, as a model of main concern contaminant degradation under visible ray illumination and different conditions of initial TC concentration, irradiation time, photocatalyst dose and pH. The experimentally obtained results were modelled using the approaches of central composite design (CCD) and artificial neural network (ANN) to achieve a more accurate description of the process behaviour. Free radical trapping experiments verify that the holes and superoxide anion radicals were the main active species. Therefore, the high decomposition efficiency (96 %) where the parameters were 30 mgL−1, 7.18, 90 min, and 0.018 g of the mentioned variables, respectively, is attributed to the boosted in production of oxidants species through Z-scheme electron transfer heterojunction. The LC-Mass technique was also used to detect the intermediates and offer the proper pathway for photodegradation of TC. The favourable performance of this photocatalyst may be a promising step forward for prosperous large scale photodegradation of persistent organic pollutants in wastewater treatment plants. Evaluation of the developed models’ performance using several statistics showed a higher predictive capability of the ANN model. Comparison of photocatalytic performance of [email protected] NPC with other recently developed counterparts highlighted its potential to be regarded as an alternative in the remediation of these categories of pollutants in water bodies.