Removing the pollutants from various wastewater is crucial to the environment, ecology, and humans. However, the pollutants are generally removed by chemical decomposition, which not only consumes a lot of energy but also produces carbon emissions. Electrochemical flocculation is effective to extract pollutant molecules and heavy ions from wastewater. To solidify the theoretical knowledge of electrochemical flocculation including electrochemistry and environmental science with industrial application, we propose a hands-on experimental design of extracting Rhodamine B (RhB) from wastewater via the waste iron oxidation reaction-assisted electrochemical flocculation for undergraduates. The laboratory can be conducted in a general lab with basic facilities and nontoxic chemicals. The experimental design combines the traditional chemical and electrochemical theory with highly efficient chemical processes for the extraction of RhB from wastewater, concurrently producing hydrogen. Therefore, an energy and environmental protection coupled system has been developed to enable students to appreciate the significance of energy and the environment in achieving global carbon neutrality.