For the first time, the successful application of the homogeneously catalyzed reductive amination in a thermomorphic multiphase system (TMS) and the first reported scale-up of this reaction into a continuous process, which recovers and recycles the homogeneous catalyst in flow, is presented. Herein, the model substrate 1-decanal reacts with the secondary amine diethylamine to form the corresponding product N,N-diethyldecylamine. A thermomorphic multiphase system (TMS) is established as a recycling strategy to recover and reuse the catalyst for the continuous process. After screening different solvents for the TMS and optimizing the reaction conditions in batch mode, the recycling of the rhodium catalyst was realized in a fully automated miniplant. Parameters influencing the stability of the process were identified and optimized to develop the continuous process. The process was operated in a steady state over 90 h with yields >90% of the desired product and low catalyst leaching <1%/h.
Cooling crystallization processes are most often controlled by adding seed crystals within the metastable zone to induce nucleation. Seeding is a challenging task and involves the risk of contamination. Its success depends on a lot of aspects, namely, seed size and amount, time point and place of addition, and experience of the operator. Gassing to induce nucleation is an innovative technology that has shown in the past that nucleation control and product design is possible. The purpose of this Article is to show that gassing competes with seeding during a cooling crystallization process. Two different cooling process concepts with and without a holding time were considered. As model system succinic acid/water was used. Gassing as well as seeding enhances production capacity by shortening the production time by a quarter for product crystals with desired mean crystal size in comparison to a normal cooling crystallization process. Production capacity is slightly higher for seeding than for gassing, but gassing competes with seeding in many ways: it is simple and ensures constant product quality.
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