A comprehensive experimental study focusing on the preparation and application of cork-based Covalent Organic Frameworks (COFs) as composite materials for the separation of oil and water is proposed for senior students. COFs were uniformly deposited on the microchannels of cork common in daily life as the substrate, and a Cork@COFs composite with a porous structure was constructed for oil−water separation. Composite materials were prepared through the in situ growth method, and the resultant composite exhibits the capability for selective oil adsorption. Additionally, the material is both recyclable and reusable. In this lab, students will be able to practice the preparation of a novel composite and learn to analyze several characterization techniques, including powder X-ray diffraction (PXRD), scanning electron microscopy (SEM), thermogravimetric analysis (TG), Fourier transform infrared (FT-IR) spectroscopy, and the contact angle test. They will also evaluate the performance of the composite by testing its selective oil adsorption and reusability. After the completion of the experiment, students present their findings to undergraduate students with a chemistry background in their sophomore and junior years in the form of a scientific report including some experimental demonstrations. The purpose of this comprehensive experiment is (1) to understand the preparation method and significance of composite materials, (2) to deepen the understanding of chemical concepts such as surface functionality, contact angle, and hydrophobicity, (3) to realize that common materials in daily life can be well combined with cutting-edge chemical knowledge, and (4) to exercise students' experimental operation ability and scientific research expression ability. This experiment can introduce students to the synthesis of COFs, Cork@COFs composite materials, the principles for using analytical instruments, and the characterization of the hydrophobic properties of materials. The presentation allows more students to gain insights into cutting-edge chemical knowledge and inspires their thinking.