Process Design for the Separation of Three Liquid Phases for a Continuous Hydroformylation Process in a Miniplant Scale

Abstract

Within the framework of the Collaborative Research Centre SFB/TR 63 InPROMPT, “Integrated chemical processes in liquid multiphase systems”, a novel process concept for the hydroformylation of long chain alkenes to aldehydes in microemulsions is investigated and developed at the Berlin Institute of Technology (Technische Universität Berlin), Germany. To start the hydroformylation reaction, a hydrophilic rhodium-ligand-complex is required. By applying a nonionic surfactant, a microemulsion system is formed and thus the hydrophilic catalyst is transported into the hydrophobic alkene phase. Next to achieve a high conversion rate in the continuously stirred tank reactor, the separation of the valuable rhodium catalyst from the product phase poses a challenge. This separation is the crucial step for the technical and economic feasibility of the overall process concept and plant design. Owing to the lack of thermodynamic data for microemulsion mixtures, the design of the phase separation unit strongly depends on experimental results. Consequently, a systematic experimental approach has been developed to identify potential operating conditions and relevant design parameters. To classify and find these, a set of experimental set-ups have been investigated to characterize impact factors on the phase separation such as type of surfactant, different concentrations of surfactant, olefin, product, and water. With the information gained through the observations the relevant composition of the investigated mixture and the separation temperature are determined for the operating conditions. Finally, necessities with regards to plant and process design are revealed.

Microemulsion Systems as Switchable Reaction Media for the Catalytic Upgrading of Long‐Chain Alkenes

“…1, consists of a feed section holding containers for the applied substances, a main reaction section holding the reactor (1.5 L), and a separation unit (decanter, 0.5 L). The mini-plant is fully automatized with SIEMENS PCS7 and meets ATEX zone 2 specifications [9]. The mini-plant is fully automatized with SIEMENS PCS7 and meets ATEX zone 2 specifications [9].…”

Recent Advances in Continuous Rhodium-Catalyzed Hydroformylation

“…Postreaction phase separation allowed the catalyst phase to be recycled back to the reactor. Based on these results, Muller and Schomäcker also constructed a miniplant for this continuous process [22].…”

Analytic Approach for Phase Equilibrium Measurements of the System Non‐Ionic Surfactant/Water/Olefine

“…Erforderlich ist die Kenntnis dieser Daten unter anderem für den Betrieb einer kontinuierlichen Miniplant, die im Rahmen des SFB/TR 63 an der TU Berlin aufgebaut wurde [12].…”

“…Die Löslichkeit kann durch den Einsatz eines Cosolvents [1], eines überkritischen Gases [4], einer ionischen Flüssigkeit [5] oder eines Tensids [2,3,6,7] [2,3,6,7]. Somit kann ein kontinuierlicher Prozess mit einem sehr geringen Katalysatorverlust entwickelt werden [12]. Grundlegende Voraussetzung für die Prozessentwicklung ist jedoch die Kenntnis des Phasenverhaltens für das System Tensid + Wasser + Olefin [13 -15].…”