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Large-scale distillation is a challenge in many respects. Particularly difficult is the purification by distillation of a compound with limited thermal stability. This article describes various aspects of these difficulties with some possible solutions. Special emphasis is placed on the collaboration of different disciplines to find pragmatic solutions to these challenges. The purification of diketene in quantities of several 1000 ta–1 is an excellent example to illustrate the different requirements. Although the distillation of diketene has been carried out by several companies for many years, there are still some aspects that deserve special attention.