In view of the problem that 1,1,2,2,3,3,4−heptafluorocyclopentane (F7A) is difficult to separate and recover when mixed with tert−amyl alcohol (TAA) for further application, leading to high cost, we designed a reactive distillation process, and conducted experimental research on the recycle effect of F7A, aiming to recycle F7A with high purity and yield from the used compound cleaning agents, thereby greatly reducing the cost. With zinc chloride as the catalyst, the dehydration reaction of TAA was carried out and the reaction kinetics were measured. Besides, the reaction kinetic equation was obtained by the correlation of experimental data. Investigations were also conducted on the effects of catalyst amount, reaction temperature, and reflux ratio on the conversion of TAA and the recovery of F7A. Based on the reaction kinetics and process optimization, the reactive distillation process for recovery of F7A was simulated to analyze the effects of stage number, feed stage, reflux ratio, and heat duty on the reactive distillation column. Under the optimized operating conditions, F7A with purity of 99.4% and recovery of 73.1% was obtained by the reactive distillation process.