Abstract: Sodium tripolyphosphate is widely recognized as one of the best chemical additives. It serves as a water-retaining agent and pH regulator in the food industry, and as a bleaching agent, dyeing assistant, and more in the textile industry. This paper introduces a comprehensive experiment tailored for the top-tier talent cultivation program in chemistry, using the high-temperature solid-state condensation method to synthesize sodium tripolyphosphate. The experiment is designed for 6+2 class hours, encompassing both inorganic synthesis operations and the utilization of large-scale research instruments. It cultivates students’ comprehension of fundamental inorganic synthesis knowledge and practical application skills, while training them to apply inorganic synthesis methods to practical problems. Furthermore, it broadens their understanding of the development of the inorganic chemical industry, enhances their innovative thinking and industrial perspectives, and comprehensively promotes their professional development. Ultimately, this experiment provides effective support for cultivating top-tier talents in the field of chemistry.