Arbeitsgruppe Apparatedesign

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AI in process industries
(2023-04-13) Bortz, Michael; Dadhe, Kai; Engell, Sebastian; Gepert, Vanessa; Kockmann, Norbert; Müller-Pfefferkorn, Ralph; Schindler, Thorsten; Urbas, Leon
The chemical industry is one of the key industrial sectors in Germany and at the same time one of the largest consumers of energy and raw materials. A successful energy transition and the development of a circular economy can only succeed if they are actively supported and shaped by the chemical industry – through the redesign of existing production processes and the exploration and implementation of new process routes. The challenge is to realize this transformation within a very short time and for many production processes, whereby a much larger number of process routes must be explored. Digital technologies are key to master this transformation towards more sustainability, climate, and environmental protection. The KEEN project aims to explore and leverage artificial intelligence (AI) opportunities in process industry. The newly developed AI methods are tested wherever possible in real working environments and production plants to prove the economic benefit, applicability, and reliability of the methods and technologies.
Design of module type package services for modular downstream units and process analytic technology
(2023-05-10) Bittorf, Lukas; Oeing, Jonas; Kock, Tobias; Garreis, Robert; Kockmann, Norbert
Modularization of process plants with its standardization activities is one of the current responses to react to dynamic markets, shorter product life cycles, and uncertain supply chains. Standardized solutions for intelligent process equipment assemblies with own automation promise high potential for chemical and pharmaceutical industries. Despite the standardized description of the module type package (MTP) and the corresponding service concept, the implementation of the service logic is left to the manufacturer, which often leads to finding various granular services for different process functions or assemblies. In this contribution, different service design approaches for a generic ‘separate’ service are investigated on the example of a solvent extraction and a distillation column. Additionally, a Raman spectroscope device for process analysis is implemented via MTP with an ‘analyze’ service. Pros and cons of the different service design approaches are discussed in the context of a fast and flexible process development in the laboratory.
Detecting crystals in suspensions: convolutional neural networks vs. gravity-based approach for size distribution detection
(2023-05-09) Neuendorf, Laura; Höving, Stefan; Bennemann, Lennard; Kockmann, Norbert
The majority of fine chemical and pharmaceutical processes includes some form of crystallization steps. For process optimization and control of further downstream steps, the crystal size distribution of the product is a crucial factor. To identify characteristic particle size classes from a large number of measurements, each individual probe has to be separated from the mother liquor and manually analyzed. In this contribution a deep learning-based method is presented using microscopic images as input for crystal size analysis. Additionally, a data augmentation approach was investigated to limit the data necessary for learning. A high segmentation accuracy of the crystals was achieved with 93.02 %. To evaluate the classification performed by the presented convolutional neural network (CNN), it is tested on two sets of images, containing a previously determined particle fraction. With the classifications of the CNN, a Q3 distribution is calculated. To validate the developed approach in terms of its accuracy it is compared to two other methods as well.
preHAZOP: graph‐based safety analysis for early integration into automated engineering workflows
(2023-05-08) Oeing, Jonas; Holtermann, Tim; Welscher, Wolfgang; Severins, Christian; Vogel, Marius; Kockmann, Norbert
The increasing digitalization and standardization within the process industry lead to a high availability of digital, machine-readable processes and plant descriptions. In particular, the publication of the DEXPI standard provides a digital representation of plant topologies including a complete description of all specifications. In early planning phases, this can be used as the basis for an automated safety assessment since digital availability significantly simplifies accessibility for smart search algorithms. This paper presents the preHAZOP search algorithm, which was developed to analyze P&IDs in DEXPI format and to detect safety-critical deviations regarding their risk according to a classical HAZOP analysis. The preHAZOP is of particular interest in early process development stages and can be easily integrated into modern, digital engineering workflows.
Graph learning in machine‐readable plant topology data
(2023-05-03) Oeing, Jonas; Brandt, Kevin; Wiedau, Michael; Tolksdorf, Gregor; Welscher, Wolfgang; Kockmann, Norbert
Digitalization shows that data and its exchange are indispensable for a versatile and sustainable process industry. There must be a shift from a document-oriented to a data-oriented process industry. Standards for the harmonization of data structures play an essential role in this change. In engineering, DEXPI (Data Exchange in the Process Industry) is already a well-developed, machine-readable data standard for describing piping and instrumentation diagrams (P&ID). In this publication, industry, software vendors, and research institutions have joined forces to demonstrate the current developments and potentials of machine-readable P&IDs in the DEXPI format combined with artificial intelligence. The aim is to use graph neural networks to learn patterns in machine-readable P&ID data, which results in the efficient engineering and development of new P&IDs.
AI‐based supervision for a stirred extraction column assisted with population balance-based simulation
(2023-04-25) Neuendorf, Laura; Hammal, Zakariae; Fricke, Armin; Kockmann, Norbert
Solvent extraction as environmental benign separation technique can be modeled in physical detail by population balance of the droplet size distribution. However, much information on the droplet generation and coalescence is necessary for representative results. In this contribution, we present a comparison of AI-evaluated experimental and simulated data on the behavior of a stirred solvent extraction column with an inner diameter of 32 mm. Lab experiments were performed using the standard test system with n-butyl acetate, acetone, and deionized water. A digital camera is placed in front of the middle section as well as the head of the column. Droplet size evaluation is performed using a retrained neural net (Mask R-CNN). The stirred DN32 extraction column is modeled and simulated using a 1D CFD population balance software. The simulation allows for behavior analysis, trends comparison, and validation of the hydrodynamics and mass transfer performances.
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.

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