Self-optimising processes and real-time-optimisation of organic syntheses in a microreactor system using Nelder–Mead and design of experiments

Fath, Verena; Kockmann, Norbert; Otto, Jürgen C.; Röder, Thorsten

doi:10.1039/d0re00081g

Cited by 34 publications

(33 citation statements)

References 97 publications

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“…The first is to design ongoing processes and new product launches with a view to reducing the use of resources. Here, modular equipment setup [30,31] and AI-assisted experimentation will drastically reduce time and lab effort [32,33]. Secondly, reaction times for new product launches (time-to-market), product transfers, but also during ongoing operations can be reduced [34].…”

Section: Realization Of a Digital Twin For A Brownfield Plantmentioning

confidence: 99%

The Digital Twin – Your Ingenious Companion for Process Engineering and Smart Production

et al. 2021

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This essay of the temporary Working Group “100% Digital” of the Association “Process, Apparatus and Plant Engineering” PAAT in ProcessNet addresses characteristics of a digital twin from the user's point of view and is intended to help solution providers to give product development a customer‐oriented direction. For this purpose, the different data models are described which play a role in the life cycles of chemical processes, plants, and products. In particular, for existing (brownfield) plants, essential aspects of the digital twin are subsequently formulated. Further expressions and consequences, e.g., on qualification and training, are deduced from the above.

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Section: Realization Of a Digital Twin For A Brownfield Plantmentioning

confidence: 99%

The Digital Twin – Your Ingenious Companion for Process Engineering and Smart Production

et al. 2021

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“…This work relies on a completely automated self-optimising platform [73], which integrates a microreactor with automated devices (pumps and thermostats) and a successive combination of real-time reaction monitoring through inline FT-IR spectroscopy and online mass spectrometry. Real-time optimisation is steered by a fully automated experimental sequence coded in MATLAB, which assumes control over optimisation strategies and the calculation of the objective function.…”

Section: Self-optimisationmentioning

confidence: 99%

“…In this work, two optimisation strategies, modified Simplex algorithm and Design of Experiments (DoE), are applied, as their performances had already been documented and compared in detail [73].…”

Section: Ms Ratiomentioning

confidence: 99%

Simultaneous self-optimisation of yield and purity through successive combination of inline FT-IR spectroscopy and online mass spectrometry in flow reactions

et al. 2021

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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 by-product formation, is still in an early stage. This article describes the development of an enhanced autonomous microfluidic reactor platform for organolithium and epoxide reactions that incorporates a successive combination of inline FT-IR spectrometer and online mass spectrometer. Experimental data is collected in real-time and used as feedback for the optimisation algorithms (modified Simplex algorithm and Design of Experiments) without time delay. An efficient approach to handle intricate optimisation problems is presented, where the inline FT-IR measurements are used to monitor the reaction’s main components, whereas the mass spectrometer’s high sensitivity permits insights into the formation of by-products. To demonstrate the platform’s flexibility, optimal reaction conditions of two organic syntheses are identified. Both pose several challenges, as complex reaction mechanisms are involved, leading to a large number of variable parameters, and a considerable amount of by-products is generated under non-ideal process conditions. Through multidimensional real-time optimisation, the platform supersedes labor- and cost-intensive work-up procedures, while diminishing waste generation, too. Thus, it renders production processes more efficient and contributes to their overall sustainability. Graphical abstract

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“…In order to decrease the time needed for screening the different selected parameters and increase the level of process understanding, an automated process setup was realized, as shown in Scheme 3. The possibility of process automation is one of the many advantages of continuous manufacturing, as it allows for rapid and controlled screening of process parameters [35][36][37]. On lab scale, automated reaction platforms are enabled by using standard hardware-connectivity to remotely control the equipment, and online analytics to monitor the process parameters in real time [36,38].…”

Section: Introductionmentioning

confidence: 99%

“…CCD was also used to define the optimal carrier and combination of process parameters. The fractional factorial CCD approach was preferred over the full factorial approach and similar approaches such as the Box-Benkhen design due to the lower number of experiments needed per iteration [35,44].…”

Section: Introductionmentioning

confidence: 99%

3D printed ceramics as solid supports for enzyme immobilization: an automated DoE approach for applications in continuous flow

et al. 2021

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In recent years, 3D printing has emerged in the field of chemical engineering as a powerful manufacturing technique to rapidly design and produce tailor-made reaction equipment. In fact, reactors with complex internal geometries can be easily fabricated, optimized and interchanged in order to respond to precise process needs, such as improved mixing and increased surface area. These advantages make them interesting especially for catalytic applications, since customized structured bed reactors can be easily produced. 3D printing applications are not limited to reactor design, it is also possible to realize functional low cost alternatives to analytical equipment that can be used to increase the level of process understanding while keeping the investment costs low. In this work, in-house designed ceramic structured inserts printed via vat photopolymerization (VPP) are presented and characterized. The flow behavior inside these inserts was determined with residence time distribution (RTD) experiments enabled by in-house designed and 3D printed inline photometric flow cells. As a proof of concept, these structured inserts were fitted in an HPLC column to serve as solid inorganic supports for the immobilization of the enzyme Phenolic acid Decarboxylase (bsPAD), which catalyzes the decarboxylation of cinnamic acids. The conversion of coumaric acid to vinylphenol was chosen as a model system to prove the implementation of these engineered inserts in a continuous biocatalytic application with high product yield and process stability. The setup was further automated in order to quickly identify the optimum operating conditions via a Design of Experiments (DoE) approach. The use of a systematic optimization, together with the adaptability of 3D printed equipment to the process requirements, render the presented approach highly promising for a more feasible implementation of biocatalysts in continuous industrial processes.

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Self-optimising processes and real-time-optimisation of organic syntheses in a microreactor system using Nelder–Mead and design of experiments

Abstract: Comparing an enhanced simplex algorithm with model-free design of experiments, this work presents a flexible platform for multi-objective, real-time optimisation.

Cited by 34 publications

References 97 publications

The Digital Twin – Your Ingenious Companion for Process Engineering and Smart Production

The Digital Twin – Your Ingenious Companion for Process Engineering and Smart Production

Simultaneous self-optimisation of yield and purity through successive combination of inline FT-IR spectroscopy and online mass spectrometry in flow reactions

3D printed ceramics as solid supports for enzyme immobilization: an automated DoE approach for applications in continuous flow

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