Norbert Kockmann

• TU Dortmund University

The exact measurement of the temperature in laboratory continuous flow processes is of high importance for many investigations e.g. of heat transfer or reaction kinetics. In particular, miniaturization poses high challenges on temperature measurement due to increased heat transfer. Despite the high relevance of this topic, there are only few public...

The rapid advancement of AI algorithms presents new opportunities for sensing technologies based on image recognition, such as real-time crystallization monitoring. This work investigates the use of computer vision to detect and size crystals in a lab scale draft tube baffle crystallizer (DTBC). A specially developed analytical bypass was implement...

Since the emergence of microfluidic devices, subtractive manufacturing techniques have dominated their production. Although the conventional manufacturing processes are well established, they come along with some disadvantages that limit the accessibility and hinder the further development of microfluidics. With the rise of additive manufacturing,...

The bacterium Zymomonas mobilis is investigated as a model organism for the cultivation and separation of ethanol as a product by in situ extraction in continuous flow microreactors. The considered microreactor is the Coiled Flow Inverter (CFI), which consists of a capillary coiled onto a support structure. Like other microreactors, the CFI benefit...

Miniaturization promotes the efficiency and exploration domain in scientific fields such as computer science, engineering, medicine, and biotechnology. In particular, the field of microfluidics is a flourishing technology, which deals with the manipulation of small volumes of liquid. Dispersed droplets or bubbles in a second immiscible liquid are o...

In industry, reliable process supervision is essential to ensure efficient, safe, and high-quality production. The droplet size distribution represents a critical quality attribute for emulsification processes and should be monitored. For emulsion characterization, image-based analysis methods are well-known but are often performed offline, leading...

For reliable supervision in multiphase processes, the droplet size represents a critical quality attribute and needs to be monitored. A promising approach is the use of smart image flow sensors since optical measurement is the most commonly used technique for droplet size distribution determination. For this, two different AI-based object detection...

Droplet-based microfluidics exhibit numerous benefits leading to relevant innovations and many applications in various fields. The precise handling of droplets in capillaries, including droplet formation, manipulation, and separation, is essential for successful operation. Only a few reports are known concerning the separation of segmented flows, p...

Maximizing the use of digitally captured data is a key requirement for many of the late adopters of digital infrastructure. One of the newcomers is the chemical industry in the area of digitized laboratories. Here, tools and services that satisfy individual needs still need to be developed and distributed within the community. This work explores th...

Due to the miniaturization of equipment for flow chemistry and microprocess engineering, low-cost sensors and analytical devices are becoming increasingly important for automated inline process control and monitoring. The combination of 3D printing technology and open-source lab automation facilitates the creation of a microfluidic toolbox containi...

Layered double hydroxides (LDHs) are a vital tool in many different areas, such as drug delivery, catalysis, anion exchange (materials), polymer processing, etc. Conventionally, LDHs are synthesized in a batch process that consists of particle generation and ripening, where product properties are manipulated for stability and the optimal uptake of...

Emulsification processes are often found in the process industry and their evaluation is crucial for product quality and safety. Numerous methods exist to analyze critical quality attributes (CQA) such as the droplet sizes and droplet size distribution (DSD) of an emulsification process. During the emulsification process, the optical process access...

Due to the miniaturization of equipment for flow chemistry and microprocess engineering, low-cost sensors and analytical devices are becoming increasingly important for automated inline process control and monitoring. The combination of 3D printing technology and open-source lab automation facilitates the creation of a microfluidic toolbox containi...

As scientific digitization advances it is imperative ensuring data is Findable, Accessible, Interoperable, and Reusable (FAIR) for machine-processable data. Ontologies play a vital role in enhancing data FAIRness by explicitly representing knowledge in a machine-understandable format. Research data in catalysis research often exhibits complexity an...

“Lab on Chip” is no longer a thing of the future. Microfluidic devices grow in popularity not only in research and development but also in industrial applications. The precise controllability and characteristic phenomena of microfluidic devices are systematically used. Education institutions support these trends and offer courses covering physical...

Current lecture methods at educational institutions are still performed analogously and mostly try to query knowledge from the students. Moreover, the field of digital skills, which is uncared of, gets increasingly crucial for today’s work life. Practical laboratory courses were introduced to counteract the analog-fashioned and theoretical lecture...

Structured research data management in catalysis is crucial, especially for large amounts of data, and should be guided by FAIR principles for easy access and compatibility of data. Ontologies help...

As scientific digitization advances it is imperative ensuring data is Findable, Accessible, Interoperable, and Reusable (FAIR) for machine-processable data. Ontologies play a vital role in enhancing data FAIRness by explicitly representing knowledge in a machine-understandable format. Research data in catalysis research often exhibits complexity an...

An automated flow chemistry platform for DNA-encoded library (DEL) technologies requires the integration of a purification process for DNA-tagged substrates. It facilitates the development of further DEL reactions, building block rehearsal, and library synthesis. Therefore, a recently developed, manual affinity-based batch purification process for...

This work provides a survey of ontologies for catalysis research to improve the findability, accessibility, interoperability, and reusability (FAIRness) of research data. Applying tools that are commonly used by lab scientists, ontologies relevant to catalysis research are classified in a simple, well formatted spreadsheet template (Excel). This en...

The presented work explores the use of ontologies and standardized enzymatic data to set up enzymatic reactions in process simulators, such as DWSIM. Setting up an automated workflow to start a process simulation based on enzymatic data obtained from the laboratory can help save costs and time during the development phase. Standardized conditions a...

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 dr...

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 pre...

The transfer from batch to flow chemistry is often based on commercial microfluidic equipment, such as costly complete reactor systems, which cannot be easily tailored to specific requirements of technologies such as DNA-encoded library technology (DELT), in particular for increasingly important photochemical reactions. Customized photoreactor conc...

Ontologies store semantic knowledge in a machine-readable way and represent domain knowledge in controlled vocabulary. In this work, a workflow is set up to derive classes from a text dataset using natural language processing (NLP) methods. Furthermore, ontologies and thesauri are browsed for those classes and corresponding existing textual definit...

Implementation of data-based key performance indicators (KPIs) within existing plants usually requires a thorough manual analysis of the plant topology to define which sensors could provide reliable information for calculating the KPIs. In this publication, we propose an assistance system that automates this process. First the automatic linkage bet...

The rise of artificial intelligence (AI)-based image analysis has led to novel application possibilities in the field of solvent analytics. Using convolutional neural networks (CNNs), better and more automated analysis of optically visible phenomena becomes feasible, broadening the spectrum of non-invasive measurements. These so-called smart sensor...

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...

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...

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...

This is an open access article under the terms of the Creative Commons Attribution License, which permits use, distribution and reproduction in any medium, provided the original work is properly cited. Solvent extraction as environmental benign separation technique can be modeled in physical detail by population balance of the droplet size distribu...

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...

Fast time‐to‐market, increased efficiency, and flexibility of production processes are major motivators for the development of integrated, continuous apparatuses with short changeover times. Following this trend, the modular belt crystallizer was developed and characterized in lab scale with the model system sucrose‐water. Based on the promising re...

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...

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...

The knowledge of product particle size distribution (PSD) in crystallization processes is of high interest for the pharmaceutical and fine chemical industries, as well as in research and development. Not only can the efficiency of crystallization/production processes and product quality be increased but also new equipment can be qualitatively chara...

An imine synthesis was investigated in a nearly isothermal oscillating segmented flow microreactor at different temperatures using non-invasive Raman spectroscopy. Multivariate curve resolution provided a calibration-free approach for obtaining kinetic parameters. The two different multivariate curve resolution approaches, soft and hard modeling, w...

Unifying research data collection methods and capturing data streams in an organized and standardized manner are becoming increasingly important in laboratories as digital processes and automation progressively shape the laboratory workflows. In this context, the Internet of Things (IoT) not only offers the opportunity to minimize time-consuming an...

The characterization of new process equipment often includes tedious experiments, particularly for (cooling) crystallization. This can be cost-intensive and time-consuming when the actual equipment has to be continuously operated to gain new insights. For multi-purpose plants that frequently change the process substance system, this can be especial...

Liquid‐liquid extraction is performed in most cases at moderate temperatures to utilize its energy‐efficient advantages. This contribution shows a new concept of a process‐intensified extraction device for liquid‐liquid systems at increased temperature and pressure. The design of the extraction device with its new subsystems, such as stirrer and pu...

Ontologies store semantic knowledge in a machine-readable way and represent domain knowledge in controlled vocabulary. In this work, a workflow is set up to derive classes from a text dataset using natural language processing (NLP) methods. Furthermore, ontologies and thesauri are browsed for those classes and corresponding existing textual definit...

The paper presents a machine-learning based approach to text-to-ontology mapping. We explore a possibility of matching texts to the relevant ontologies using a combination of artificial neural networks and classifiers. Ontologies are formal specifications of the shared conceptualizations of application domains. While describing the same domain, dif...

A chemometrics-based approach for process optimisation of a chemical reaction in an automated microreactor flow setup and performing kinetic investigations.

This paper contains a machine-learning-based approach to detect duplicities in ontologies. Ontologies are formal specifications of shared conceptualizations of application domains. Merging and enhancing ontologies may cause the introduction of duplicities into them. The approach to duplicities proposed in this work presents a solution that does not...

Organolithium compounds have been used successfully in flow chemistry since the recent past. Most of the studies dealt with the use in halogen-lithium exchanges. So far, however, there has been a lack of use in substitution reactions. The use of flow microreactors makes the highly reactive organolithium compounds more controllable and thus creates...

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...

The flexibility and performance of digital laboratory elements such as remote labs, VR/AR or simulations summarized under the term cross-reality labs (CrossLabs), can be seen with the development in last and has been proven under the pandemic situation. Even though the potential of cross-reality labs is obvious referring to availability and flexibi...

In an extraction column, counter-current two-phase flow is generated. The value component is separated from a continuous liquid phase by conveying into a second non-miscible liquid. This work in progress presents a digital revision of this laboratory experiment. It consists of two pedagogically and technically flexible combinable parts. Both parts...

Continuous flow calorimeters are a promising tool in process development and safety engineering, particularly for flow chemistry applications. An isoperibolic flow calorimeter is presented for the characterization of exothermic reactions. The calorimeter is adapted to commercially available plate microreactors made of glass and uses Seebeck element...

Enzyme activity data for biocatalytic applications are currently often not annotated with standardized conditions andterms. This makes it extremely hard to retrieve, compare, and reuse enzymatic data. With advances in the fields of artificialintelligence (AI) and machine learning (ML), the automated usability of data in the form of machine-readable...

In Modular Automation, the orchestration creates the link between process equipment assemblies (PEA) and processes towards operation. This paper presents a general methodology, so-called type-based orchestration, on how to design a fully functional modular process plant based on the module type package (MTP). In a number of discussion rounds, the s...

DNA-encoded library technologies require high-throughput, compatible, and well automatable platforms for chemistry development, building block rehearsal, and library synthesis. An affinity-based process using Watson–Crick interactions was developed that enables purification of DNA-tagged compounds from complex reaction mixtures. The purification re...

Among thermal separation methods, solvent extraction with countercurrent flow is one of the most energy-efficient processes. The separation efficiency is highest close to the flooding point, which characterizes the maximum possible liquid throughput. However, this point is the limiting parameter in the entire extraction process since the flow of at...

The National Research Data Infrastructure for Catalysis-Related Sciences (NFDI4Cat) is one of the disciplinary consortia formed within the German national research data infrastructure (NFDI), an effort undertaken by the German federal and state governments to advance the digitalization of all scientific research data within the German academic syst...

Modularization helps overcome the challenges of changing production environmants in process industries. ABB and partners have developed pilot applications to validate the new concepts in process automation communication and control that modularization needs. What are the results from these pilots.

The modularization of production plants and their automation in the pharmaceutical and (bio‐)chemical industry is currently gaining attention and is subject of standardization efforts. The combination of modular and monolithic (bio‐)chemical plants and related engineering processes, i.e., hybrid process plants and hybrid engineering, respectively,...

Liquid–liquid contacting with mass transfer and chemical reactions can often be found in process industries and exhibit a complex nature. Liquid–liquid extraction, or solvent extraction, is a widely used separation process in the laboratory and chemical, petroleum, pharmaceutical, hydrometallurgical, and food industries. This section describes the...

The design and engineering of piping and instrumentation diagrams (P&ID) is a very time-consuming and labor-intensive process. Although P&IDs show common patterns that could be reused during development, the drawing is usually created manually and built up from scratch for each process. The aim of this paper is to recognize these patterns with the...

Volatile markets and increasing demands for quality and fast availability of specialty chemical products have motivated the rise of small-scale, integrated, and modular continuous processing plants. As a significant unit operation used for product isolation and purification, cooling crystallization is part of this trend. Here, the small-scale and i...

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 (di=1.59 mm, dc=28.8 mm)...

Online process supervision is enabled by smart sensor development, hence attracting increasing attention in pharmaceutical and chemical process engineering. Additional sensor data enable more precise process control as additional process parameters can be monitored. They are easy to integrate into modular plants, and their provided additional proce...

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 %...

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 t...

Calorimetric data from chemical reactions such as reaction enthalpy, adiabatic temperature rise, and activation energy are essential for reaction safety and scale-up from laboratory investigations to reactor design and operation. Typically, these data are gained from batch calorimeters with sophisticated setups and elaborate measurement procedures....

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 de...

Industrial Draft Tube Baffle (DTB) crystallizers are well known and can be found in many applications; however, DTBs are rarely investigated on the laboratory scale. A miniaturized DTB for continuous cooling crystallization with integrated fine-grain dissolution was designed, set up, and characterized. A typical DTB from the m³-scale was scaled dow...

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 proce...

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 au...

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. Sim...

Continuous small-scale production is currently of utmost interest for fine chemicals and pharmaceuticals. For this purpose, equipment and process concepts in consideration of the hurdles for solids handling are required to transfer conventional batch processing to continuous operation. Based on empirical equations, pressure loss constraints, and an...

Taylor bubbles are bubbles that are filling a capillary fixed or rising in a liquid flow. Due to their well-defined size, shape and velocity the flow field around Taylor bubbles is well controllable. Furthermore, only a small amount of gas and liquid is required for experiments, making the study of Taylor bubbles simple and safe. In this chapter, T...

The Front Cover illustrates the dynamics and complexity of catalysis. Handling data in catalysis research in a sharable and re‐usable way is an unsolved challenge. A concept is proposed by the initiative NFDI4Cat, a consortium in the German NFDI (National Research Data Infrastructure), that serves all aspects of catalysis research. Indicated in the...

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...

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 m...

Self-optimisation constitutes a very helpful tool for chemical process development, both in lab and in industrial applications. However, research on the application of model-free autonomous optimisation strategies (based on experimental investigation) for complex reactions of high industrial significance, which involve considerable intermediate and...

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-...

Nucleation in continuously operated capillary coiled cooling crystallizers is experimentally investigated under the influence of ultrasound. It was found that there is no sharp boundary but rather a transition zone for nucleation under sonication. For this purpose, a tube with an inner diameter of 1.6 mm and a length of 6 m was winded in a coiled f...