In view of the current research situation of antibiotic water pollution in Baiyangdian Lake and relying on the current scientific research projects, a research type experiment is designed for the adsorption of ciprofloxacin in water by the hydrothermal synthesis of composite aerogel (CMC/CoNiFe-LDH) modified with cobalt nickel iron layered hydroxide (CoNiFe-LDH) based on carboxymethyl cellulose (CMC). The morphology, phase, and functional groups of CMC/CoNiFe-LDH are characterized using SEM, XRD, FTIR, etc. The effects of pH, reaction time, and initial concentration on adsorption efficiency are analyzed. The experimental results indicated that under the optimal experimental conditions, the adsorption capacity of CMC/CoNiFe-LDH for ciprofloxacin is 298.32 mg/g. The teaching experiment involves analytical chemistry, material chemistry, instrument analysis and other curriculum knowledge, which helps stimulate students’ interest in experimental learning, cultivate innovative thinking and experimental hands-on ability, and improve the ability to use theoretical knowledge to solve practical problems.