Enabling low power acoustics for capillary sonoreactors

Capillary reactors demonstrate outstanding potential for on-demand flow chemistry applications. However, non-uniform distribution of multiphase flows, poor solid handling, and the risk of clogging limit their usability for continuous manufacturing. While ultrasonic irradiation has been traditionally applied to address some of these limitations, their acoustic efficiency, uniformity and scalability to larger reactor systems are often disregarded. In this work, high-speed microscopic imaging reveals how cavitation-free ultrasound can unclog and prevent the blockage of capillary reactors. Modeling techniques are then adapted from traditional acoustic designs and applied to simulate and prototype sonoreactors with wider and more uniform sonication areas. Blade-, block- and cylindrical shape sonotrodes are optimized to accommodate longer capillary lengths in sonoreactors resonating at 28 kHz. Finally, a novel helicoidal capillary sonoreactor is proposed to potentially deal with a high concentration of solid particles in miniaturized flow chemistry. The acoustic designs and first principle rationalization presented here offer a transformative step forward in the scale-up of efficient capillary sonoreactors.This research was partially funded by the EU project MAPSYN (Microwave, Acoustic and Plasma SYNtheses) developed in the group of Photochemistry and Electrochemistry of Semiconductors (GFES) at the University of Alicante (Spain), under grant agreement No. CP-IP 309376 of the European Union Seventh Framework Program

Industrial Data Science for Batch Manufacturing Processes

Batch processes show several sources of variability, from raw materials' properties to initial and evolving conditions that change during the different events in the manufacturing process. In this chapter, we will illustrate with an industrial example how to use machine learning to reduce this apparent excess of data while maintaining the relevant information for process engineers. Two common use cases will be presented: 1) AutoML analysis to quickly find correlations in batch process data, and 2) trajectory analysis to monitor and identify anomalous batches leading to process control improvements

Guidelines for the design of efficient sono-microreactors

Possible drawbacks of microreactors are inefficient reactant mixing and the clogging of microchannels when solid-forming reactions are carried out or solid (catalysts) suspensions are used. Ultrasonic irradiation has been successfully implemented for solving these problems in microreactor configurations ranging from capillaries immersed in ultrasonic baths to devices with miniaturized piezoelectric transducers. Moving forward in process intensification and sustainable development, the acoustic energy implementation requires a strategy to optimize the microreactor from an ultrasound viewpoint during its design. In this work, we present a simple analytical model that can be used as a guide to achieving a proper acoustic design of stacked microreactors. An example of this methodology was demonstrated through finite element analysis and it was compared with an experimental study found in the literature.This research is funded by the EU project MAPSYN: Microwave, Acoustic and Plasma SYNtheses, under grant agreement No. CP-IP 309376 of the European Union Seventh Framework Program

Reduction of Dispersion in Ultrasonically-Enhanced Micropacked Beds

Channeling of gas can reduce mass transfer performance in multiphase micropacked-bed reactors. Viscous and capillary forces cause this undesired and often unpredictable phenomenon in systems with catalyst particle sizes of hundreds of micrometers. In this work, we acoustically modify flow in a micropacked-bed reactor to reduce gas channeling by applying high-power sonication at low ultrasonic frequencies (∼40 kHz). Experimental residence time distributions reveal two orders of magnitude reduction in dispersion with ultrasound, allowing for nearly plug-flow behavior at high flow rates in the bed. Sonication appears to partially fluidize the packed-bed under pressurized cocurrent two-phase flow, effectively improving dispersion characteristics.This research was partially funded by the EU project MAPSYN: Microwave, Acoustic and Plasma SYNtheses, under Grant CPIP 309376 of the European Union Seventh Framework Program

Process intensification education contributes to sustainable development goals: Part 2

Achieving the United Nations sustainable development goals requires industry and society to develop tools and processes that work at all scales, enabling goods delivery, services, and technology to large conglomerates and remote regions. Process Intensification (PI) is a technological advance that promises to deliver means to reach these goals, but higher education has yet to totally embrace the program. Here, we present practical examples on how to better teach the principles of PI in the context of the Bloom's taxonomy and summarise the current industrial use and the future demands for PI, as a continuation of the topics discussed in Part 1. In the appendices, we provide details on the existing PI courses around the world, as well as teaching activities that are showcased during these courses to aid students’ lifelong learning. The increasing number of successful commercial cases of PI highlight the importance of PI education for both students in academia and industrial staff.We acknowledge the sponsors of the Lorentz’ workshop on“Educating in PI”: The MESA+Institute of the University of Twente,Sonics and Materials (USA) and the PIN-NL Dutch Process Intensi-fication Network. DFR acknowledges support by The Netherlands Centre for Mul-tiscale Catalytic Energy Conversion (MCEC), an NWO Gravitationprogramme funded by the Ministry of Education, Culture and Sci-ence of the government of The Netherlands. NA acknowledges the Deutsche Forschungsgemeinschaft (DFG)- TRR 63¨Integrierte Chemische Prozesse in flüssigen Mehrphasen-systemen¨(Teilprojekt A10) - 56091768. The participation by Robert Weber in the workshop and thisreport was supported by Laboratory Directed Research and Devel-opment funding at Pacific Northwest National Laboratory (PNNL).PNNL is a multiprogram national laboratory operated for theUS Department of Energy by Battelle under contract DE-AC05-76RL0183

Process intensification education contributes to sustainable development goals : part 1

In 2015 all the United Nations (UN) member states adopted 17 sustainable development goals (UN-SDG) as part of the 2030 Agenda, which is a 15-year plan to meet ambitious targets to eradicate poverty, protect the environment, and improve the quality of life around the world. Although the global community has progressed, the pace of implementation must accelerate to reach the UN-SDG time-line. For this to happen, professionals, institutions, companies, governments and the general public must become cognizant of the challenges that our world faces and the potential technological solutions at hand, including those provided by chemical engineering. Process intensification (PI) is a recent engineering approach with demonstrated potential to significantly improve process efficiency and safety while reducing cost. It offers opportunities for attaining the UN-SDG goals in a cost-effective and timely manner. However, the pedagogical tools to educate undergraduate, graduate students, and professionals active in the field of PI lack clarity and focus. This paper sets out the state-of-the-art, main discussion points and guidelines for enhanced PI teaching, deliberated by experts in PI with either an academic or industrial background, as well as representatives from government and specialists in pedagogy gathered at the Lorentz Center (Leiden, The Netherlands) in June 2019 with the aim of uniting the efforts on education in PI and produce guidelines. In this Part 1, we discuss the societal and industrial needs for an educational strategy in the framework of PI. The terminology and background information on PI, related to educational implementation in industry and academia, are provided as a preamble to Part 2, which presents practical examples that will help educating on Process Intensification

Modeling, Simulation and Optimization of Multiphase Micropacked-Bed Reactors and Capillary Sonoreactors

In the last decades, miniaturized flow chemistry has promised to bring the benefits of process intensification, continuous manufacturing and greener chemistry to the fine chemical industry. However, miniaturized catalytic processes where gas, liquid, and solids are involved have always been impeded by two main drawbacks: multiphase-flow maldistribution (i.e. gas channeling) and clogging of capillary reactors. In this thesis, first principle models have been used to capture the complexity of multiphase flow in micropacked-bed reactors, which can suffer from poor and unpredictable mass-transfer performance. When the particle size ranges 100 µm in diameter, capillary and viscous forces control the hydrodynamics. Under such conditions, the gas —and not the liquid— flows creating preferential channels that cause poor radial dispersion. Experimental observations from the literature were reproduced to validate a physical-based modeling approach, the Phase Field Method (PFM). This simulation strategy sheds light on the impact of the micropacked-bed geometry and wettability on the formation of preferential gas channels. Counterintuitively, to homogenize the two-phase flow hydrodynamics and reduce radial mass-transfer limitations, solvent wettability of the support needs to be restricted, showing best performance when the contact angle ranges 60° and capillary forces are still dominant. Visualization experiments showed that ultrasound irradiation can also be used to partially fluidized the bed and modify the hydrodynamics. Under sonication, residence time distributions (RTD) in micropacked-bed reactors revealed a two-order-of-magnitude reduction in dispersion, allowing for nearly plug-flow behavior at high gas and liquid flow rates. At a reduced scale, surfaces vibrating with a low amplitude were shown to fluidize, prevent and solve capillary tube blockage problems, which are commonly found in the fine chemical industry for continuous product synthesis. The modeling and simulation strategy used in this thesis, enables a fast prototyping methodology for the proper acoustic design of sonoreactors, whose scale-up was achieved by introducing slits in sonotrodes. In addition, a patent-pending helicoidal capillary sonoreactor has shown to transform longitudinal vibrating modes into radial and torsional modes, pioneering a new range of chemistry able to handle a high concentration of particles. The contributions of this thesis made in the fields of reaction engineering and process intensification have demonstrated how computational methods and experimental techniques in other areas of research can be used to foster innovation at a fast pace

Modeling Pore-Scale Two-Phase Flow: How to Avoid Gas-Channeling Phenomena in Micropacked-Bed Reactors via Catalyst Wettability Modification

A model capable of providing a reliable estimation of two-phase flow dynamics and mass-transfer coefficients, is lacking for the design of micropacked-bed reactors via correlations, especially when the particle size of the bed is around 100 μm. In this work, we present a validation of the use of the phase field method for reproducing two-phase flow experiments found in the literature. This numerical simulation strategy sheds light on the impact of the micropacked-bed geometry and wettability on the formation of preferential gas channels. Counterintuitively, to homogenize the two-phase flow hydrodynamics and reduce radial mass-transfer limitations, solvent wettability of the support needs to be restricted, showing best performance when the contact angle ranges to 60° and capillary forces are still dominant. The tuning of gas–liquid–solid interactions by surface wettability modification opens a new window of opportunity for the design and scale-up of micropacked-bed reactors

Aprendizaje basado en problemas aplicado a la asignatura Química Física Avanzada del Grado en Química

En aprendizaje basado en problemas (ABP o PBL, problem-based learning) constituye una metodología del proceso de enseñanza-aprendizaje que todavía no se ha generalizado en la universidad española, a pesar de que ha sido implementada con éxito desde hace años en algunas universidades anglosajonas. En este artículo se pretende dar un ejemplo de diseño de la enseñanza basada en problemas aplicada a la asignatura Química Física Aplicada del tercer curso del Grado en Química de la Universidad de Alicante. Un análisis empírico de los resultados obtenidos con la metodología clásica de enseñanza indica un cambio en el proceso de enseñanza-aprendizaje para esta asignatura. Este artículo se centra en uno de sus temas y abarca tanto los materiales docentes asociados a la metodología ABP que debe preparar el profesorado, como la manera en que deben organizarse las sesiones presenciales y la posible evaluación del alumnado durante las mismas. Asimismo, se discutirán distintos modos de interacción del alumnado con el profesorado durante el desarrollo de las sesiones prácticas y la utilización durante las mismas de diferentes herramientas informáticas. Se analizarán las ventajas e inconvenientes de este tipo de metodología de enseñanza-aprendizaje. En particular, se hará énfasis en el alto grado de implicación que deben mostrar tanto profesorado como alumnado para que el sistema pueda funcionar de manera efectiva

Reduction of Dispersion in Ultrasonically-Enhanced Micropacked Beds

© 2017 American Chemical Society. Channeling of gas can reduce mass transfer performance in multiphase micropacked-bed reactors. Viscous and capillary forces cause this undesired and often unpredictable phenomenon in systems with catalyst particle sizes of hundreds of micrometers. In this work, we acoustically modify flow in a micropacked-bed reactor to reduce gas channeling by applying high-power sonication at low ultrasonic frequencies (∼40 kHz). Experimental residence time distributions reveal two orders of magnitude reduction in dispersion with ultrasound, allowing for nearly plug-flow behavior at high flow rates in the bed. Sonication appears to partially fluidize the packed-bed under pressurized cocurrent two-phase flow, effectively improving dispersion characteristics