This article focuses on the problems of insufficient separation of aluminum-plastic composite packaging materials, resulting in low product purity, low separation efficiency, and insufficient separation process. This paper, used environmentally friendly aluminum-plastic active media for separation technology research and the optimization of the separation process parameters. The natural solid acid citric acid solution was selected as the separation solvent for the separation of aluminum-plastic composite waste, and the influence factors such as citric acid concentration, reaction temperature, liquid-to-solid ratio, stirring speed and cutting size on the separation effect of aluminum-plastic composite materials was studied. According to the orthogonal test and range analysis, a separation process with short separation time and low aluminum loss rate was optimized. The study found that under the conditions of the citric acid concentration of 2 mol/L, temperature 100 ℃, liquid-solid ratio of 400 L/kg, stirring speed of 650 r/min, and cutting size of 0.5 cm×0.5 cm, the aluminum-plastic separation rate reached 100%, the separation time was 65 min, and the aluminum loss rate was 0.66%. Citric acid is a new type of natural separating agent, which has low corrosion rate to aluminum. It can be a reference for the recycling and reusing of aluminum-plastic composite material waste for industrial production.