Andreas Jupke

Optimal design of batch and simulated moving bed chromatographic separation processes

Preparative chromatography, especially simulated moving bed (SMB) chromatography, is a key technology for the separation of fine chemicals on a production scale. Most of the design methods for batch and SMB processes proposed in the open literature deal with the optimisation of the operating conditions for a given chromatographic unit only. Therefore, a comparison of the process economy may lead to incorrect results. In this contribution, an effective strategy for the optimal choice of all process parameters (operation and design parameters) is proposed. The main idea of this strategy is to apply a detailed and experimentally validated process model and to reduce the number of influencing parameters by introducing and optimising dimensionless process parameters. It is shown that there is an infinite choice of design and operating parameters to achieve maximum productivity or minimum separation costs and not at the maximum pressure drop only. The detailed design of the chromatographic unit and the selection of the operating conditions can be adjusted by considering the availability of columns and packing materials. As the model system, the separation of a racemic mixture (EMD53986) on Chiralpak AD was investigated. After complete optimisation of a batch and a SMB unit, a real comparison of the process economy can be achieved. Finally, the influences of two different objective functions, productivity and specific separation cost, are analysed.

Liquid/liquid extraction of biomass-derived lignin from lignocellulosic pretreatments

Despite the rapid progress in the field of biomass fractionation and lignin valorization, no industrial process for chemical utilization of lignin has yet been established. One major step in that direction has been made with the advent of biorefineries and new biomass fractionation methods that deliver a relatively clean lignin stream, allowing a more efficient recovery and utilization of this fraction. However, the transfer of lignin from the fractionation solvent to a different medium for subsequent valorization has been largely disregarded so far. In this work, we demonstrate the use of a green liquid/liquid-extraction to transfer lignin from the organic phase of the OrganoCat process into differently concentrated alkaline solutions for further utilization. We show that alkaline solutions of pH 13 and 14 are able to almost completely extract the OrganoCat lignin from the organic phase but that this extraction might be accompanied by changes in the molecular structure of lignin, here shown by a change in the apparent molecular weight distribution.

Fluid Dynamics of Microgel-Covered Drops Reveal Impact on Interfacial Conditions

Microgels are deformable polymer-networks with conspicuous properties. Their surface- activity associated with their switchability makes their application in liquid-liquid systems, such as extraction processes, particularly promising. For their application as switchable stabilizers at the interface, a detailed understanding of their impact on process relevant phenomena, such as the sedimentation behavior, is necessary. So far, the focus of research has been on microscopic-scale properties, whereby the propagation to macroscopic effects has rarely been quantified. In this study, single microgel-covered n-butyl acetate drops rising in a quiescent continuous water phase are investigated experimentally. The dependency of the microgel properties, in terms of size and cross-linking density, on the fluid dynamics are addressed. The impact of microgels is studied in detail by sedimentation velocity, drop deformation and the resulting drag coefficient. The deformation of drops is related to shape conserving interfacial properties such as the interfacial tension. Counter to our expectations, microgel-covered drops deform less than the drops of the pure system although microgels reduce the interfacial tension. Moreover, the sedimentation velocity is of special interest, since it reveals the mobility of the interface and friction conditions at the interface. Our results demonstrate the correlation between microgel properties at the interface on a microscopic scale and the macroscopic behavior of microgel-covered drops.

From beech wood to itaconic acid: case study on biorefinery process integration

Renewable raw materials in sustainable biorefinery processes pose new challenges to the manufacturing routes of platform chemicals. Beside the investigations of individual unit operations, the research on process chains, leading from plant biomass to the final products like lactic acid, succinic acid, and itaconic acid is increasing. This article presents a complete process chain from wooden biomass to the platform chemical itaconic acid. The process starts with the mechanical pretreatment of beech wood, which subsequently is subjected to chemo-catalytic biomass fractionation (OrganoCat) into three phases, which comprise cellulose pulp, aqueous hydrolyzed hemicellulose, and organic lignin solutions. Lignin is transferred to further chemical valorization. The aqueous phase containing oxalic acid as well as hemi-cellulosic sugars is treated by nanofiltration to recycle the acid catalyst back to the chemo-catalytic pretreatment and to concentrate the sugar hydrolysate. In a parallel step, the cellulose pulp is enzymatically hydrolyzed to yield glucose, which—together with the pentose-rich stream—can be used as a carbon source in the fermentation. The fermentation of the sugar fraction into itaconic acid can either be performed with the established fungi Aspergillus terreus or with Ustilago maydis. Both fermentation concepts were realized and evaluated. For purification, (in situ) filtration, (in situ) extraction, and crystallization were investigated. The presented comprehensive examination and discussion of the itaconate synthesis process—as a case study—demonstrates the impact of realistic process conditions on product yield, choice of whole cell catalyst, chemocatalysts and organic solvent system, operation mode, and, finally, the selection of a downstream concept.