Abstract: In recent years, the discharge of waste liquid in laboratories in universities and colleges has attracted much attention. Universities and colleges have issued relevant management measures. According to the Physical Chemistry Experiment Project of the Demonstration Center, a comprehensive undergraduate experiment project is designed based on the concept of environmental protection−recovery and thermogravimetric analysis of copper sulfate pentahydrate in laboratory waste liquid. Through the teaching of this comprehensive experiment project, copper sulfate pentahydrate can be recycled and students can consolidate their existing knowledge of inorganic chemistry (precipitation, washing, solid-liquid separation, concentrated crystallization) and analytical chemistry, and master knowledge of the new theory (the understanding of thermogravimetric analysis spectrum). The project can improve students’ operational skills, cultivate students’ awareness of environmental protection, exercise students’ ability to analyze and solve problems. At the same time, the comprehensive design of the experiment can be used as a material of ideological and political education to publicize the construction of national ecological civilization.