Article
Chemistry, Applied
Filip Horvath-Gerber, King Kuok (Mimi) Hii, Christian Holtze, Eleonore Jeanne Camille Deublein, Klaus Hellgardt
Summary: Diazomethane is a hazardous compound used in organic chemistry, which makes scale-up challenging. The current state-of-the-art methodology for safe laboratory-scale generation, separation, and consumption of diazomethane is using a Teflon AF2400 membrane in a tube-in-tube reactor setup. This study introduces a novel methodology to determine the permeability of diazomethane, which enables the scale-up development of the membrane reactor for production-scale systems.
ORGANIC PROCESS RESEARCH & DEVELOPMENT
(2023)
Review
Agricultural Engineering
Burcu Akkoyunlu, Sorcha Daly, Eoin Casey
Summary: Membrane bioreactors show potential in producing value-added products but face challenges in industrial deployment. Current research focuses on increasing mass transfer rate, maintaining high cell concentrations, and separating inhibitory substances. Challenges such as commercialization trends, high costs, and membrane fouling need to be addressed for wider application in the future.
BIORESOURCE TECHNOLOGY
(2021)
Article
Chemistry, Physical
Deepak Kumar Jaiswal, Dnyaneshwar Aand, Puchakayala Krishna Rao, Sibaji Nandi, Srihari Pabbaraja, Ajay K. Singh
Summary: The deactivation of toxic gases and the separation of liquids through metal-organic frameworks (MOFs) have made significant advancements in this growing field. However, the stability of MOFs and their sensitivity to water are still being developed. In this study, a new strategy using scalable and safely generated continuous flow diazomethane is proposed to seal moisture-sensitive functionality in hydrophobic MOFs, demonstrating improved hydrophobicity and its applications in organic/aqueous phase separation and self-cleaning. This work presents the first attempt to seal sensitive functional groups with diazomethane for hydrophobic MOFs, exploring a new proof of concept for designing stable MOFs with controlled wettability. The concept of MOF diazomethane treatment can also be expanded to design and develop advanced membranes for effectively separating aqueous organic solutions, providing valuable insights.
APPLIED SURFACE SCIENCE
(2023)
Article
Engineering, Chemical
Ilaria Rizzardi, Aldo Bottino, Gustavo Capannelli, Marcello Pagliero, Camilla Costa, Daniele Matteucci, Antonio Comite
Summary: The use of porous membranes can improve the oxygen transfer efficiency at the gas/liquid interface, leading to better aeration in full-scale systems. Compared to traditional disk diffusers, the membrane module operates at lower air flow rates and achieves higher efficiency. However, scaling phenomena were observed on the membrane surface.
JOURNAL OF MEMBRANE SCIENCE
(2023)
Review
Agricultural Engineering
Ayon Tarafdar, Ranjna Sirohi, Vivek Kumar Gaur, Sunil Kumar, Poonam Sharma, Sunita Varjani, Hari Om Pandey, Raveendran Sindhu, Aravind Madhavan, Reshmy Rajasekharan, Sang Jun Sim
Summary: Commercial enzyme production is gaining popularity globally due to its wide applications in traditional and modern industrial sectors. Research efforts focus on improving efficiency, reducing costs, and ensuring sustainability. New engineering interventions and optimization strategies are being introduced to meet the growing demand for industrial enzymes.
BIORESOURCE TECHNOLOGY
(2021)
Article
Engineering, Chemical
Wendy A. Jonkers, Emile R. Cornelissen, Wiebe M. de Vos
Summary: This review provides a comprehensive overview of the rapidly developing field of polymeric hollow fiber nanofiltration, covering membrane and process design, operational parameters, and full-scale applications. Six different methods are currently used to produce HF NF membranes, with PEM based membranes standing out due to their high chemical stability. The combination of geometry and chemical stability makes HF NF a sustainable alternative to spiral wound NF, especially for applications with high fouling load.
JOURNAL OF MEMBRANE SCIENCE
(2023)
Article
Food Science & Technology
Virginia L. Verges, Jarrad W. Gollihue, Glenna E. Joyce, Seth DeBolt
Summary: Whiskey production originated in Scotland in the 15th century and was based on malted barley. Scotch-Irish settlers in the Ohio river valley started fermenting and distilling maize, leading to the creation of American Whiskey. The bourbon industry in Kentucky has experienced significant growth in recent years, with distilleries focusing on innovation, sustainability, and diversifying their products. This study presents a lab-scale method that mimics commercial distillation processes and can be used for training and research purposes.
Article
Chemistry, Applied
Anne M. Gaffney, Natalie Duprez, Kelsey J. Louthan, Brianna Borders, James Gasque, Alexander Siegfried, Thomas G. Stanford, Kenneth L. Roberts, Yousif Alcheikhhamdona, Mina Hoorfar, Bo Chen, Sudip Majumdar, Hannah Murnen
Summary: Previous work by the group used a HYSYS simulator to predict the performance of an ethylene ODH production facility with alternative diluents and separation technology. The study also explored safety and operational improvements, as well as the development of membrane-based separation technology for the ODH process. Various non-cryogenic distillation alternatives were simulated and evaluated alongside membrane separation.
Article
Thermodynamics
Wenjun Zhou, Weixing Zhou, Huayu Qiu, Dun Li, Yu Zhang, Muhammad Sajjad Ahmad, Kawi Sibudjing
Summary: This study investigates the performance of a Ni-coated MoS2 membrane in the methane pyrolysis process. The membrane demonstrates excellent catalytic and separation performance due to its increased specific surface area and reduced pore size. The Ni coating attracts methane, destabilizes the C-H bond, and promotes methane deep crack, while the MoS2 membrane blocks methane and drives H proton transportation for H2 formation. This work provides guidance for bifunctional membranes in methane pyrolysis, with potential to reduce energy cost and greenhouse gas emissions.
ENERGY CONVERSION AND MANAGEMENT
(2023)
Article
Engineering, Chemical
Yaru Zhu, Haiyang Yan, Feipeng Lu, Ya Su, Wei Li, Jin An, Yaoming Wang, Tongwen Xu
Summary: This study integrated electrodialysis (ED), an electro-driven membrane process, into the current pressure-driven membrane processes to separate and concentrate the UF permeate for treating landfill leachate. The results showed that by optimizing parameters such as membrane stack voltage and flow velocity, ED demonstrated excellent performance in handling landfill leachate.
SEPARATION AND PURIFICATION TECHNOLOGY
(2021)
Article
Engineering, Environmental
Muhammad Asif, Syeda Sidra Bibi, Sheraz Ahmed, Muhammad Irshad, Muhammad Shakir Hussain, Hassan Zeb, Muhammad Kashif Khan, Jaehoon Kim
Summary: Sustainable societal growth relies on efficient storage, transportation, and use of renewable energies. Ammonia, with its high hydrogen content and energy density, holds promise as a zero-carbon energy carrier for large-scale storage. Catalytic cracking of ammonia into nitrogen and hydrogen provides an environmentally friendly method for hydrogen regeneration. This review summarizes recent advances in effective ammonia decomposition via various processes and discusses hydrogen separation techniques and techno-economic analyses of the ammonia and hydrogen economy.
CHEMICAL ENGINEERING JOURNAL
(2023)
Review
Polymer Science
Keyu Ji, Chengkun Liu, Haijun He, Xue Mao, Liang Wei, Hao Wang, Mengdi Zhang, Yutong Shen, Runjun Sun, Fenglei Zhou
Summary: In the field of water purification, membrane separation technology, particularly electrospun nanofiber membranes, plays a significant role. These membranes are produced through the electrospinning method, which is straightforward, low cost, and offers functional diversity and process controllability. The structural characteristics of electrospun nanofiber membranes can be flexibly controlled, and various membrane material combinations can be utilized to achieve high-performance water treatment membranes with high porosity, selectivity, and microporous permeability. The current research focuses on creating high-permeability membranes with outstanding selectivity, antifouling performance, physical and chemical performance, and long-term stability. This paper reviews the preparation methods and properties of electrospun nanofiber membranes for water treatment, discusses antifouling technologies, research progress, and future development directions.
Article
Green & Sustainable Science & Technology
Hellen Luisa de Castro e Silva, Maxi Estefany Huaman Cordova, Regina Mambeli Barros, Geraldo Lucio Tiago Filho, Electo Eduardo Silva Lora, Afonso Henriques Moreira Santos, Ivan Felipe Silva dos Santos, Maria Claudia Costa de Oliveira Botan, Juliano Romanzini Pedreira, Barbara Karoline Flauzino
Summary: This study evaluates the technical and economic feasibility of biogas production from swine manure in the Southern of Minas Gerais, Brazil. The results show that the project is economically viable with the sale of organic fertilizer and has positive environmental impacts.
Article
Chemistry, Multidisciplinary
Wenying Shi, Tengfei Li, Hongbin Li, Qiyun Du, Haixia Zhang, Xiaohong Qin
Summary: An integrated process combining esterification, transesterification, and separation steps was used to produce biodiesel from acidic oil. The results showed high conversion rates and compliance with international standards for the biodiesel product.
JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY
(2022)
Article
Chemistry, Multidisciplinary
Wei Yao, Jian Tan, Xiaodong Zhu, Guanglei Liu, Zhenglong Xu, Mingxin Ye, Jianfeng Shen
Summary: Inspired by leaf structure, a carbon felt/PVA solar-driven device was developed for the separation of versatile oily wastewater. This device exhibits superior solar energy absorption and vapor release capacity, enabling efficient purification of different types of wastewater, including high concentration oil-water emulsions and acidic/alkaline wastewater.
CELL REPORTS PHYSICAL SCIENCE
(2022)
Article
Chemistry, Organic
Florian Sommer, C. Oliver Kappe, David Cantillo
Summary: The method described involves the use of a chloride salt as a redox mediator and supporting electrolyte for the selective oxidation of secondary alcohols in the presence of primary alcohols. Active chlorine species generated at the anode selectively oxidize secondary alcohols to ketones, providing good to excellent yields. Furthermore, the chloride salt can be easily recovered for reuse, making the method highly sustainable.
Article
Engineering, Chemical
Stephan Sacher, Ismael Castillo, Jakob Rehrl, Peter Sagmeister, Rene Lebl, Julia Kruisz, Selma Celikovic, Martin Sipek, Jason D. Williams, Dirk Kirschneck, C. Oliver Kappe, Martin Horn
Summary: This study developed a continuous synthesis line for the production of Mesalazine from 2-chlorobenzoic acid, integrated with a multi-instrument PAT strategy for in-line monitoring and automated process control. Process models were crucial for implementing an automation concept to maximize yield and minimize side products.
CHEMICAL ENGINEERING RESEARCH & DESIGN
(2022)
Article
Chemistry, Organic
Bence S. Nagy, Patricia Llanes, Miquel A. Pericas, C. Oliver Kappe, Sandor B. Otvos
Summary: A novel approach for enantioselective flow synthesis of rolipram has been reported, which shows significantly improved productivity compared with earlier methodologies.
Article
Chemistry, Physical
Kevin Simon, Peter Sagmeister, Rachel Munday, Kevin Leslie, Christopher A. Hone, C. Oliver Kappe
Summary: Continuous flow technologies offer solutions to safety, scalability, and sustainability issues in heterogeneous hydrogenation reactions. However, catalyst deactivation due to substrate inhibition is a potential drawback. In this study, an automated continuous flow and real-time analytics platform is used for efficient evaluation of functional group/heterocycle tolerance in heterogeneous hydrogenation reactions. The methodology proves valuable for benchmarking catalytic reactions and the preparation of complex molecules.
CATALYSIS SCIENCE & TECHNOLOGY
(2022)
Article
Chemistry, Multidisciplinary
Peter Sagmeister, Florian F. Ort, Clemens E. Jusner, Dominique Hebrault, Thomas Tampone, Frederic G. Buono, Jason D. Williams, C. Oliver Kappe
Summary: Autonomous flow reactors are increasingly used in the synthesis of organic compounds, but the complexity of chemical reactions and analytical methods remains limited. This study presents a modular platform that combines rapid flow NMR and FTIR measurements with chemometric modeling for efficient and timely analysis of reaction outcomes. The platform is tested in two different reactions and achieves excellent results in a relatively small number of iterations.
Review
Public, Environmental & Occupational Health
Desiree Znidar, Doris Dallinger, C. Oliver Kappe
Summary: This article provides a detailed description of the design of an advanced fluorine gas delivery system using 10% fluorine in nitrogen to address safety issues and technical challenges in handling fluorinated compounds. It also furnishes an overview of suitable flow reactor components and design on laboratory scale.
ACS CHEMICAL HEALTH & SAFETY
(2022)
Article
Chemistry, Applied
Bence S. Nagy, C. Oliver Kappe, Sandor B. otvos
Summary: This study developed a flow chemistry-based process for the oxidation of aldehydes, which enhances process safety by minimizing peracid accumulation. Carboxylic acid formation can be chemically intensified and scalable even in the reactions of deactivated substrates under continuous flow conditions.
ADVANCED SYNTHESIS & CATALYSIS
(2022)
Article
Chemistry, Multidisciplinary
Jason D. Williams, Peter Pochlauer, Yoshiyuki Okumura, Yukari Inami, C. Oliver Kappe
Summary: Dynamic deracemization processes, such as crystallization-induced diastereomer transformations (CIDTs), offer the opportunity to combine racemization and resolution processes, providing high yields of enantiomerically pure compounds. By incorporating photochemical racemization and applying design of experiment principles, it is possible to achieve excellent results in just 4 hours reaction time, opening new avenues for preparation of enantiomerically pure functional molecules on both small and industrially-relevant scales.
CHEMISTRY-A EUROPEAN JOURNAL
(2022)
Article
Chemistry, Applied
Wolfgang Jud, Chase A. Salazar, Joseph Imbrogno, Jenson Verghese, Steven M. Guinness, Jean-Nicolas Desrosiers, C. Oliver Kappe, David Cantillo
Summary: An electrochemical method for converting primary alcohols to carboxylic acids has been developed. This method can be used with various alcohols containing nitrogen-containing heterocycles in both continuous flow and batch modes. The use of a heterogeneous NiOOH electron-proton transfer mediator eliminates the need for homogeneous catalysts, reducing unit operations and process mass intensity.
ORGANIC PROCESS RESEARCH & DEVELOPMENT
(2022)
Article
Automation & Control Systems
Ismael Castillo, Jakob Rehrl, Peter Sagmeister, Rene Lebl, Julia Kruisz, Selma Celikovic, Martin Sipek, Dirk Kirschneck, Martin Horn, Stephan Sacher, David Cantillo, Jason D. Williams, Johannes G. Khinast, Oliver Kappe
Summary: This paper presents the application of Data Driven Modelling (DDM) and Non-Linear Model Predictive Control (NMPC) for the control implementation of a continuous reactor for the production of the Active Pharmaceutical Ingredient (API), Mesalazine. The contribution of this work is to present the overall control architecture, the step-by-step controller design based on DDM, i.e. Neuro-Fuzzy/Local Linear Model Tree Models (LoLiMoT) and NMPC. We demonstrate the advantages of DDM and NMPC, in the presence of non-linear, distributed parameter, multi-variable systems as a suitable, powerful and practical way to approach complex process control challenges. Compared to conventional concepts, the inherent optimization structure of NMPC allows to obtain the desired behaviour of the multi-variable non-linear plant considering the physical constraints of operation regions. The control concept has been implemented in the real system on one central computer, XamControl (Evon),1 with all measurement devices and actuators centrally interconnected. (c) 2022 Elsevier Ltd. All rights reserved.
JOURNAL OF PROCESS CONTROL
(2023)
Article
Chemistry, Applied
Kevin Simon, Desiree Znidar, Julien Boutet, Gerard Guillamot, Jean-Yves Lenoir, Doris Dallinger, C. Oliver Kappe
Summary: A proof-of-concept study for the synthesis of 1,2-difluorobenzene from 2-fluoroaniline via the Balz-Schiemann reaction using HF/pyridine as the fluorinating reagent is reported. The key to success was the photochemically induced fluorodediazoniation of the in situ-generated diazonium salt performed in a continuous flow mode. The use of a high-power 365 nm light-emitting diode improved the reaction performance and allowed the generation of 1,2-difluorobenzene within a 10 min residence time and a product selectivity of >= 95% at full conversion.
ORGANIC PROCESS RESEARCH & DEVELOPMENT
(2023)
Article
Chemistry, Multidisciplinary
Gang Fu, Juncheng Jiang, Christopher A. Hone, C. Oliver Kappe
Summary: This paper demonstrates the reliable measurement of highly exothermic, rapid reactions using a modular 3D printed continuous flow calorimeter. The influence of mixing efficiency on reaction conversion and product selectivity is investigated through computational fluid dynamics simulations. The reaction enthalpies for the synthesis of desired products are successfully deconvoluted. In addition, the exothermic characteristics of a lithium-halogen exchange and iodine quench reaction are studied.
REACTION CHEMISTRY & ENGINEERING
(2023)
Article
Chemistry, Applied
Philipp Petermeier, Christoph Kohlfuerst, Ana Torvisco, Roland C. C. Fischer, Alejandro Mata, Doris Dallinger, C. Oliver Kappe, Joerg H. H. Schrittwieser, Wolfgang Kroutil
Summary: Substituted piperidine rings are efficiently prepared with multiple stereocentres using multi-enzymatic and chemo-enzymatic methods from achiral diketoester precursors. Highly enantioselective transamination and diastereoselective reduction processes enable the synthesis of optically pure piperidines. This approach offers a more streamlined and efficient route for the synthesis of trisubstituted piperidines with potential applications in drug discovery.
ADVANCED SYNTHESIS & CATALYSIS
(2023)
Article
Chemistry, Multidisciplinary
Dominik Polterauer, Dominique M. Roberge, Paul Hanselmann, Ryan Littich, Christopher A. Hone, C. Oliver Kappe
Summary: This article introduces a new continuous flow method for the synthesis of sulfonyl chlorides from disulfides and thiols, using 1,3-dichloro-5,5-dimethylhydantoin (DCH) as the oxidative chlorination reagent. Under optimized conditions, sulfonyl chlorides can be synthesized at high yields, with a high space-time yield.
REACTION CHEMISTRY & ENGINEERING
(2022)
Article
Chemistry, Multidisciplinary
Sebastian Knoll, Clemens E. Jusner, Peter Sagmeister, Jason D. Williams, Christopher A. Hone, Martin Horn, C. Oliver Kappe
Summary: This article describes an optimization workflow based on newly-developed open-source software (Optipus) for automated flow optimization experiments. It highlights the application of the software in optimizing nucleophilic aromatic substitution and photochemical benzylic bromination. The utilization of Optipus enables early generation and use of predictive models, reducing development time and risks.
REACTION CHEMISTRY & ENGINEERING
(2022)