Arbeitsgruppe Apparatedesign

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http://hdl.handle.net/2003/100

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Artificial intelligence‐based module type package‐compatible smart sensors in the process industry
(2023-08-09) Neuendorf, Laura M.; Khaydarov, Valentin; Schlander, Christiane; Kock, Tobias; Fischer, Joshua; Urbas, Leon; Kockmann, Norbert
Image analysis presents a set of powerful methods to receive additional information about multiphase processes. It enables the development of advanced applications for process monitoring and optimization or, so-called, soft sensors. However, the integration of advanced smart sensor systems based on image analysis into the process control system presents a complex task. To address this challenge, a modular automation concept offers a standardized interface to integrate modules. This paper presents an integration profile as a service specification that allows a plug-and-measure integration of smart visual sensors into modular plants. To verify the concept, we applied it to three different use cases. At the end, we discuss open challenges in the integration of complex analysis systems with multidimensional data streams into modular plants.
Development of a two-phase flow reaction system for DNA-encoded amide coupling
(2023-03-13) Dinter, Robin; Willems, Suzanne; Hachem, Mahdi; Streltsova, Yana; Brunschweiger, Andreas; Kockmann, Norbert
Synthesis platforms are of particular interest to DNA-encoded library (DEL) technologies to facilitate chemistry development, building block validation, and high-throughput library synthesis. A liquid–liquid two-phase flow reactor was designed that enables parallel conduction of reactions on DNA-coupled substrates. The dispersed phase in capillary slug flow contained the DNA reaction mixture and allowed for spatially separated batch experiments in a microchannel. A coiled flow inverter (CFI) tubular reactor with a 3D-printed internal structure on which a capillary is coiled was used for improved mixing and compact setup. An inert continuous phase was introduced, which generated slug flow and prevented backmixing of the individual reactants. In order to enable parallelized reactions, slugs containing a variety of different carboxylic acids were successfully generated to act as individual reaction compartments representing single batch experiments. As a widely used exemplary DEL reaction, the amide coupling reaction was successfully transferred to the tailored flow reaction system and DNA was recovered.
Design and characterization of a flow reaction calorimeter based on FlowPlate® Lab and Peltier elements
(2023-01-27) Frede, Timothy A.; Vom Hofe, Nils; Reuß, Rafael Jasper; Kemmerling, Niklas; Kock, Tobias; Herbstritt, Frank; Kockmann, Norbert
Continuous manufacturing and development of flow processes depend significantly on an optimized and adapted determination of thermokinetic data of chemical reactions. Reaction calorimetry represents a prominent technique to quantify the heat release of exothermic reactions. This work presents a continuous flow calorimetric measurement system based on a commercially available hastelloy C-22 microreactor. A sensor array of Peltier elements is added to the existing microreactor setup to enable the additional functionality of flow calorimetry. The calorimeter and its additional equipment are connected to open-source soft- and hardware for data acquisition and processing as well as automated reaction screening. The reaction calorimeter can be operated in both isoperibolic and isothermal operation mode. The calorimeter's performance is investigated on the basis of model reactions, where good agreement with literature was obtained for determined reaction enthalpies.
Reaction optimization of a Suzuki‐Miyaura cross‐coupling using design of experiments
(2022-03-11) Bobers, Jens; Hahn, Lisa Katharina; Averbeck, Tobias; Brunschweiger, Andreas; Kockmann, Norbert
The combination of lab automation and design of experiments for the execution of screening experiments increases productivity and reduces error-prone manual work. A self-developed software tool allows for creating fractional-factorial experimental design (FFED). Application of FFED on the screening of a Suzuki-Miyaura cross-coupling leads to a 93 % reduced design compared to full-factorial design. The resulting regression model qualitatively shows the positive effect of educt concentrations, time, and temperature and reveals the decrease in conversion at high base concentrations.
From coiled flow inverter to stirred tank reactor – bioprocess development and ontology design
(2022-03-29) Grühn, Julia; Behr, Alexander S.; Eroglu, Talha H.; Trögel, Valentin; Rosenthal, Katrin; Kockmann, Norbert
Miniaturized bioreactors, such as the coiled flow inverter (CFI), offer several benefits within process development such as lower time and cost factors. In this study, we demonstrate continuous flow experiments in a CFI and transferred them to experiments in a batch reactor by using the oxygen transfer coefficient kLa as a key parameter. In order to simplify the parameter transfer and at the same time develop a basis for future data handling according to the FAIR data principles, an equipment and process ontology was developed for these examples.
X‐ray‐based tomographic imaging for the investigation of laminar mixing in capillaries
(2022-05-06) Schuler, Julia; Herath, Jakob; Kockmann, Norbert
Micro-computed tomography is a promising non-invasive imaging technology that offers high spatial resolution without requiring optical access. This opens the opportunity to analyze concentration fields in mixing equipment in 3D. To demonstrate the potential of the methodology, laminar mixing in helically coiled capillaries is investigated by tracking the radial distribution of potassium iodide along the main flow direction. Dean flow can be observed in the helically coiled capillaries, which intensifies with Reynolds number and decreasing effect of gravity.
Reactor performance estimation in microscale flow calorimeter for rapid characterization of exothermic reactions
(2022-12-12) Frede, Timothy Aljoscha; Nikbin, Nick; Kockmann, Norbert
Continuous flow calorimeters are a promising tool in process development and safety engineering, especially for flow chemistry applications to characterize the heat release and kinetic parameters of rapid chemical reactions. In this study, the digital accompaniment of an isoperibolic flow calorimeter for characterization of exothermic reactions is presented. To support experimental planning and evaluation, computational fluid dynamic simulations are carried out for single-phase flow in the microreactor. The residence time distribution is obtained and used for estimation of conversion and temperature profiles along the microreactor channel. This leads to an integration of CFD simulations into the calorimeter’s software-guided workflow reducing the experimental effort regarding the determination of thermokinetic data. The approach is tested for a highly exothermic test reaction, which provides further hints for future investigations.
Small-scale solids production plant with cooling crystallization, washing, and drying in a modular, continuous plant
(2023-08-15) Höving, Stefan; Schmidt, Thomas; Peters, Maximilian; Lapainis, Hendrik; Kockmann, Norbert
Small-scale continuous apparatuses for solid product manufacturing are receiving increasing interest due to the demand for the fast market availability of specialty chemical products manufactured in integrated and modular processing plants. Relevant unit operations span from crystallization over solid–liquid separation and filter cake washing to drying. For this purpose, the quasi-continuous filter belt crystallizer (QCFBC) was developed and is presented here. The newly integrated unit operations with positive pressure filtration (Δ𝑝max = 0.8 bar), filter cake washing (𝑉˙wash = 55 mL·min−1), and convection drying (𝑇dry = 60 °C) have been individually characterized and integrated into the filter apparatus that has been modified for continuous operation. They were synchronized with the flexible cooling crystallization, enabling for a seamless production process. Sucrose in water was used as model substance system. Long-term operations of up to 14 h were successfully performed with dry product filter cakes (22.64 g ± 1.64 g·h−1) of constant quality attributes (𝑥50,3 = 216.095 ± 14.766, 𝑠𝑝𝑎𝑛 = 0.347 ± 0.109, 𝑌rel. = 69.9% ± 5%, 𝑋RM = 1.64 mg·g−1 ± 1.38 mg·g−1).
Experimental investigation of the pre–Darcy regime
(2022-02-02) Boettcher, Konrad E. R.; Fischer, Michael-David; Neumann, Tim; Ehrhard, Peter
The validity of Darcy’s law at very low Reynolds numbers is discussed controversially in literature, as some authors propose a pre–Darcy flow regime below some critical Reynolds number. The scope of this work is to investigate this problem experimentally. Therefore, a packing of glass spheres is perfused by different glycerin–water solutions. A linear behaviour between the flow velocity and the pressure drop through the packed spheres is found in the complete investigated range of Reynolds number Red′, based on the mean-pore diameter d′ and mean-pore velocity v′ with 10−9≤Red′≤10−1. This contradicts the results of different authors like Fand et al. (1987) or Kececioglu and Jiang (1994), postulating a pre–Darcy regime for Red′≤2.8⋅10−6 or Red′≤0.13, respectively.
Open-source multi-purpose sensor for measurements in continuous capillary flow
(2021-12-09) Höving, Stefan; Bobers, Jens; Bobers, Jens
Limited applicability and scarce availability of analytical equipment for micro- and millifluidic applications, which are of high interest in research and development, complicate process development, control, and monitoring. The low-cost sensor presented in this work is a modular, fast, non-invasive, multi-purpose, and easy to apply solution for detecting phase changes and concentrations of optically absorbing substances in single and multi-phase capillary flow. It aims at generating deeper insight into existing processes in fields of (bio-)chemical and reaction engineering. The scope of this work includes the application of the sensor to residence time measurements in a heat exchanger, a tubular reactor for concentration measurements, a tubular crystallizer for suspension detection, and a pipetting robot for flow automation purposes. In all presented applications either the level of automation has been increased or more information on the investigated system has been gained. Further applications are explained to be realized in the near future.
Gas-liquid mass transfer intensification for bubble generation and breakup in micronozzles
(2021-06-14) Reichmann, Felix; Herath, Jakob; Mensing, Lena; Kockmann, Norbert
The local gas-liquid mass transfer was characterized during bubble generation in T-contactors and in an adjacent micronozzle. A colorimetric technique with the oxygen sensitive dye resazurin was investigated to visualize gas-liquid mass transfer during slug flow, bubble deformation, as well as laminar and turbulent bubble breakup in the wake of a micronozzle. Two optimized nozzle geometries from previous studies were evaluated concerning volumetric mass transfer coefficients for low pressure loss, narrow residence time distribution, or high dispersion rates. Highest values in kla up to 60 s−1 were found for turbulent bubble breakup and an optimized micronozzle design in respect to pressure drop and dispersion rate. The achieved mass transfer coefficients were correlated with the energy dissipation rate within the micronozzles and with the inverse Kolmogorov time scale in vortex dissipation in good agreement for laminar and turbulent breakup regimes.
Application of polyimide-based microfluidic devices on acid-catalyzed hydrolysis of dimethoxypropane
(2021-02-18) Bobers, Jens; Forys, Elisabeth; Oldach, Bastian; Kockmann, Norbert
Microfluidic devices intensify transport phenomena and can improve chemical processes. New manufacturing processes and materials are perpetually developed due to constantly growing interest in process intensification. In this contribution, the authors present the design and application of polyimide-foil-based microfluidic mixing devices manufactured by reactive ion etching. As appropriate model reaction system, acid-catalyzed 2,2-dimethoxypropane (DMP) hydrolysis was chosen and investigated in three different mixing structure with varying flow rate. Energy dissipation rates were calculated to estimate mixing performances. The results show good mixing quality for Reynolds numbers between 10 and 100 and similar mixing times scales for all investigated microstructured mixers.
Software-guided microfluidic reaction calorimeter based on thermoelectric modules
(2021-03-10) Frede, Timothy Aljoscha; Burke, Inga; Kockmann, Norbert
A software-guided, continuous reaction calorimeter based on thermoelectric modules for direct heat flux measurements is presented. Sensors and actuators of the calorimeter's setup are implemented within a lab automation system, which enables the automated calibration of the heat flux sensors and investigations of chemical reactions through sequential function charts. Functionality of the calibration is shown by heat transfer experiments. Additionally, the calorimeter's performance is demonstrated by good agreement of conducted neutralization experiments with literature data.
Digital image processing of gas-liquid reactions in coiled capillaries
(2021-03-15) Grühn, Julia; Vogel, Marius; Kockmann, Norbert
In the course of the investigation of biocatalytic gas-liquid reactions with color change in straight and coiled capillaries, a non-invasive evaluation method is needed to determine reaction progress and selectivity. Correlations between hydrodynamics, mass transfer phenomena, and reaction kinetics are in the focus of our work. For this purpose, it is necessary to investigate the flow and evaluate the reaction progress without disturbing the flow. Digital image processing (DIP) is presented as a suitable optical evaluation method for reactions with color change in capillary reactor designs. The developed DIP program is independent from the capillary reactor design, applicable to differently colored systems, and can analyze up to three different species simultaneously.
3D investigations of microscale mixing in helically coiled capillaries
(2021-04-20) Schuler, Julia; Herath, Jakob; Kockmann, Norbert
In capillary reactors, improving radial mixing and narrowing the residence time distribution is of great importance for high selectivity and reaction performance. A well-known approach is inducing secondary flow patterns by coiling the capillary around a cylinder. To increase understanding of transport phenomena in helically coiled capillaries non-invasive 3D imaging approaches are required. In this perspective paper, we introduce X-ray-based micro-computed tomography for the investigation of dispersion of iodide in a helically coiled tube. The methodology presented here allows for the direct evaluation of radial concentration fields. By varying Dean number Dn and modified torsion parameter T∗, the effect of torsion and curvature on the radial concentration profile can be identified. Detailed knowledge of local radial mixing in helically coiled capillaries will help the precise prediction of reaction progress and selectivity.
Characterization of an automated spinning-band column as a module for laboratory distillation
(2021-07-13) Bittorf, Lukas; Böttger, Nils; Neumann, Daniel; Winter, Alina; Kockmann, Norbert
Modularization is a promising technology to respond to short product life cycles. Not only in production but also in the laboratory, the concept of modularization can help to quickly explore new products or processes. A modular continuously operated spinning-band distillation column for small product amounts is presented and characterized regarding operating window and separation efficiency. The column can be used either for first product amounts within a small-scale production or as feasibility studies for distillation in a scale-up context with small amounts of resources, energy, and time. By introducing the modular automation concept and a certain degree of automation structures, this column can be operated almost fully automatically and integrated quickly to higher automation structures such as a process orchestration layer.
Machine learning based suggestions of separation units for process synthesis in process simulation
(2021-09-15) Oeing, Jonas; Henke, Fabian; Kockmann, Norbert
As part of Industry 4.0, workflows in the process industry are becoming increasingly digitalized. In this context, artificial intelligence (AI) methods are also finding their way into the process development. In this communication, machine learning (ML) algorithms are used to suggest suitable separation units based on simulated process streams. Simulations that have been performed earlier are used as training data and the information is learned by machine learning models implemented in Python. The trained models show good, reliable results and are connected to a process simulator using a .NET framework. For further optimization, a concept for the implementation of user feedback will be assigned. The results will provide the fundamental basis for future AI-based recommendation systems.
Flooding prevention in distillation and extraction columns with aid of machine learning approaches
(2021-10-13) Oeing, Jonas; Neuendorf, Laura Maria; Bittorf, Lukas; Krieger, Waldemar; Kockmann, Norbert
Flooding of separation columns is a severe limitation in the operation of distillation and liquid-liquid extraction columns. To observe operation conditions, machine learning algorithms are implemented to recognize the flooding behavior of separation columns on laboratory scale. Besides this, the investigated columns already provided the modular automation interface Module Type Package (MTP), which is used for data access of necessary sensor data. Hence, artificial intelligence (AI) tools with deep learning offer high potential for the process industry and allow to capture operating states that are otherwise difficult to detect or model. However, the advanced methods are only hesitantly applied in practice due to complex combination of operational sensing, data analysis, and active control of the equipment. This article provides an overview on how AI-based algorithms can be implemented in existing laboratory plants. Process sensor data as well as image data are used to model the flooding behavior of distillation and extraction columns for stable and robust operational conditions.
Towards a systematic data harmonization to enable AI application in the process industry
(2021-11-15) Wiedau, Michael; Tolksdorf, Gregor; Oeing, Jonas; Kockmann, Norbert
Current methods of artificial intelligence may often proof ineffective in the process industry, usually because of insufficient data availability. In this contribution, we investigate how data standards can contribute to fulfill the data availability requirements of machine learning methods. We give an overview of AI use cases relevant in the process industry, name related requirements and discuss known standards in the context of implicit vs. explicit data. We conclude with a roadmap sketching how to bring the results of this contribution into practical application.
Investigations on selectivity of gas-liquid reactions in capillaries
(2020-02-06) Grühn, Julia; Burke, Inga; Neuhaus, Nadine; Kockmann, Norbert
Biocatalysis offers a broad spectrum of possible ecological and economic advantages over conventional chemical catalysis processes, e.g., lower energy consumption and high enantio selectivity. The focus of this work is on gas-liquid reactions. These are of great importance in the chemical and biochemical industry and subject of current research since they are often limited by mass transfer or show low selectivity. Different suitable biocatalytically gas-liquid reaction systems were tested in capillary reactor designs in order to obtain information about the interaction between reaction and fluid mechanics. Furthermore, an optical measuring method was established. The experiments were performed in batch mode in a glass beaker with a flow cuvette for UV/Vis measurement of product concentration.

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