Abstract
New developments of synthesis routes in homogeneous catalysis often require a precise control of the reaction conditions in order to achieve optimal results. A precise control of the flow- and reactor behaviour can improve the performance of a catalytic system, e.g. by suppressing side- and consecutive reactions. The Taylor-Couette reactor (TCR) allows a precise control of the flow conditions combining the benefits of continuously stirred tank reactors (CSTR) and plug-flow reactors (PFR). A ribbed Taylor Couette reactor for the application in homogeneous catalysis was developed and tested in the continuous hydroamination of the renewable ß-myrcene in miniplant-scale. The application of the atom-efficient hydroamination to terpenes allows the continuous production of terpenyl amines based on renewable resources. Catalyst recycling of the homogeneous transition metal catalyst was achieved by means of Thermomorphic Multicomponent Solvent (TMS)-systems. TMS-systems enable the realisation of the reaction under homogeneous conditions at elevated temperatures, but also allow a biphasic phase separation after the reaction. This way the homogeneous catalyst can be separated from the product phase and used again. Yields of the desired terpenyl amines of up to 87 % could be generated in a homogeneous toluene solution on a laboratory scale.
The application of the TMS-system acetonitrile/n-heptane yielded 86 %, the TMS-system N,N-dimethylformamide/n-heptane generated 45 % of the desired hydroamination products. Both systems were then transferred into a continuously operated miniplant and realised using a Taylor-Couette reactor. The reactor performance was then validated and compared to the laboratory batch experiments. In the continuous miniplant experiments, the Taylor-Couette reactor could reproduce and even surpass the results of the batch experiments.
