Based on the scientific research concept of atomic economy and comprehensive utilization of solid waste, the production of high value-added products by “turning waste into treasure” based on the solid waste is introduced into the undergraduate’s experiment. Based on the comprehensive experiment of acidolysis of phosphorus tailings, the experiment of acidolysis and product crystallization of phosphorus tailings is designed. The comprehensive experiment includes chemical engineering process of selective tailings acid leaching decomposition, filtration and crystallization, and oriented crystal growth. Moreover, with the aid of scanning electron microscope (SEM), the micro-structure and length/diameter ratio of the whisker and the elemental content analysis are also determined. These contents can train the practical ability, experimental equipment operation skill and analytical ability of the undergraduates, and learn about the operation principle of the instruments and results analysis method, thus realizing the connection between undergraduate and postgraduate stages. Based on the experimental design, the scientific research innovation consciousness and the theoretical knowledge system of the students are highly improved, and the ideological and political theories are integrated in the teaching process, which achieve the teaching aims of comprehensive experiment.