1 Overview of Micro Reaction Engineering
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Design and Engineering of Microreactor and Smart-Scaled Flow Processes
Editorial Special Issue : Design and engineering of microreactor and smart-scaled flow processes Citation for published version (APA): Hessel, V. (2015). Editorial Special Issue : Design and engineering of microreactor and smart-scaled flow processes. Processes, 3(1), 19-22. https://doi.org/10.3390/pr3010019 DOI: 10.3390/pr3010019 Document status and date: Published: 01/01/2015 Document Version: Publisher’s PDF, also known as Version of Record (includes final page, issue and volume numbers) Please check the document version of this publication: • A submitted manuscript is the version of the article upon submission and before peer-review. There can be important differences between the submitted version and the official published version of record. People interested in the research are advised to contact the author for the final version of the publication, or visit the DOI to the publisher's website. • The final author version and the galley proof are versions of the publication after peer review. • The final published version features the final layout of the paper including the volume, issue and page numbers. Link to publication General rights Copyright and moral rights for the publications made accessible in the public portal are retained by the authors and/or other copyright owners and it is a condition of accessing publications that users recognise and abide by the legal requirements associated with these rights. • Users may download and print one copy of any publication from the public portal for the purpose of private study or research. • You may not further distribute the material or use it for any profit-making activity or commercial gain • You may freely distribute the URL identifying the publication in the public portal. -
Tr2013 03 Flow Chemistry.Pdf
What is flow chemistry? Flow chemistry is a process in which a reaction is run Continuously in a flowing stream rather than in batch production Comparison between traditional chemistry and flow chemistry Reaction Stoichiometry: In traditional chemistry this is defined by the concentration of chemical reagents and their volumetric ratio. In flow chemistry this is defined by The concentration of the chemical reagents and the ratio of their flow rate Residence time: In traditional chemistry this is determined by how long a vessel is kept at given temperature. In flow the volumetric residence time is used given by the ratio of the volume of the reactor and the overall flow rate What is residence time? Residence time of a reagent is defined as the amount of time that the reaction is cooled or heated. Residence time = reactor volume/flow rate Continuous flow reactors: a perspective Advantages: 1. Improved thermal management 2. Mixing control 3. Application of the extreme reaction conditions Principles of green chemistry: 1. Prevention of waste O NH HO 2 OH N Solvent -free O reaction temp : 65 oC reaction time : 5.1 min yield : 91% Green chem., 2012, 14, 38-54 2. Atom economy O OH toluene reaction temp : 240 oC pressure : 100 bar yield : 95% O H O O O MeCN O H O reaction temp : 60 oC Green chem., 2012, 14, 38-54 O O N N N N O N O O N O H N electon-withdrawing group O CCl3 Cl O Smallest unit of benzylimidate NaOH (3.4 eq) N N BnOH (7.8 eq) N N o Cl N Cl 0 to 50 C, 2.5 h O N O 81% Org. -
The Fundamentals Behind the Use of Flow Reactors in Electrochemistry
The fundamentals behind the use of flow reactors in electrochemistry Citation for published version (APA): Noël, T., Cao, Y., & Laudadio, G. (2019). The fundamentals behind the use of flow reactors in electrochemistry. Accounts of Chemical Research, 52(10), 2858-2869. https://doi.org/10.1021/acs.accounts.9b00412 DOI: 10.1021/acs.accounts.9b00412 Document status and date: Published: 01/10/2019 Document Version: Publisher’s PDF, also known as Version of Record (includes final page, issue and volume numbers) Please check the document version of this publication: • A submitted manuscript is the version of the article upon submission and before peer-review. There can be important differences between the submitted version and the official published version of record. People interested in the research are advised to contact the author for the final version of the publication, or visit the DOI to the publisher's website. • The final author version and the galley proof are versions of the publication after peer review. • The final published version features the final layout of the paper including the volume, issue and page numbers. Link to publication General rights Copyright and moral rights for the publications made accessible in the public portal are retained by the authors and/or other copyright owners and it is a condition of accessing publications that users recognise and abide by the legal requirements associated with these rights. • Users may download and print one copy of any publication from the public portal for the purpose of private study or research. • You may not further distribute the material or use it for any profit-making activity or commercial gain • You may freely distribute the URL identifying the publication in the public portal. -
Towards More Efficient, Greener Syntheses Through Flow Chemistry
Towards More Efficient, Greener Syntheses through Flow Chemistry The MIT Faculty has made this article openly available. Please share how this access benefits you. Your story matters. Citation Lummiss, Justin A.M. et al. “Towards More Efficient, Greener Syntheses through Flow Chemistry.” The Chemical Record 17, 7 (February 2017): 667–680 © 2017 Wiley-Verlag As Published https://doi.org/10.1002/tcr.201600139 Publisher Wiley Blackwell Version Author's final manuscript Citable link http://hdl.handle.net/1721.1/114543 Terms of Use Creative Commons Attribution-Noncommercial-Share Alike Detailed Terms http://creativecommons.org/licenses/by-nc-sa/4.0/ PERSONAL ACCOUNT Alternatively, entire flow systems with specialized attachments Towards More Efficient, can be purchased from various commercial suppliers.[4b] Greener Syntheses Through Flow Chemistry Justin A.M. Lummiss,[a] Peter D. Morse,[a] Rachel L. Beingessner,[a] and Timothy F. Jamison*[a] Abstract: Technological advances have an important role in the design of greener synthetic processes. In this Personal Account, we describe a wide range of thermal, photochemical, catalytic, and biphasic chemical transformations examined by our group. Each of these demonstrate how the merits of a continuous flow synthesis platform can align with some of the goals put forth by the Twelve Principles of Green Chemistry. In particular, we illustrate the potential for improved reaction efficiency in terms of atom economy, product yield and reaction rates, the ability to design synthetic process with chemical and solvent waste reduction in mind as well as highlight the benefits of the real- time monitoring capabilities in flow for highly controlled synthetic output. -
Development of Catalytic Microreactors by Plasma Processes and Sol-Gel Processes Xi Rao
Development of catalytic microreactors by plasma processes and sol-gel processes Xi Rao To cite this version: Xi Rao. Development of catalytic microreactors by plasma processes and sol-gel processes. Analytical chemistry. Université Pierre et Marie Curie - Paris VI, 2016. English. NNT : 2016PA066145. tel- 01592658 HAL Id: tel-01592658 https://tel.archives-ouvertes.fr/tel-01592658 Submitted on 25 Sep 2017 HAL is a multi-disciplinary open access L’archive ouverte pluridisciplinaire HAL, est archive for the deposit and dissemination of sci- destinée au dépôt et à la diffusion de documents entific research documents, whether they are pub- scientifiques de niveau recherche, publiés ou non, lished or not. The documents may come from émanant des établissements d’enseignement et de teaching and research institutions in France or recherche français ou étrangers, des laboratoires abroad, or from public or private research centers. publics ou privés. Université Pierre et Marie Curie Ecole doctorale 391 : Sciences Mécaniques, Acoustique, Electronique et Robotique de Paris IRCP, UMR 8247 (CNRS-Chimie ParisTech) Equipe Procédés, Plasmas, Microsystèmes Développement de microréacteurs catalytiques par procédés plasma et procédés sol-gel Par RAO Xi Thèse de doctorat en : Chimie - Génie des Procédés Dirigée par TATOULIAN Michaël Présentée et soutenue publiquement le 24 Mai 2016 Devant un jury composé de : Mme. PONCIN-EPAILLARD Fabienne Directeur de recherche CNRS Rapporteur Université du Maine M. LEONARD Didier Professeur des Universités Rapporteur Institut des Sciences Analytiques M. DA COSTA Patrick Professeur des Universités Examinateur UPMC Sorbonne Universités M. ABOU-HASSAN Ali Maître des Conférences, HDR Examinateur UPMC Sorbonne Universités M. GUYON Cédric Maître des Conférences Examinateur Chimie ParisTech, PSL M. -
Flow Chemistry
Flow chemistry Flow chemistry is also known as continuous flow or plug flow chemistry. It involves a chemical reaction run in a continuous flow stream. The process offers potential for the efficient manufacture of chemical products. Recent breakthroughs using Vapourtec systems are in production of Tamoxifen (Breast Cancer) and Artemisinin (Malaria). Reactants are first pu mped into a mixing device. Flow continues through a temperature controlled reactor until the reaction is complete. The reactor can be a simple pipe, tube or complex micro-structured device. The mixing device and reactor are maintained at the temperature to promote the desired reaction. The reactants may also be exposed to an electrical flux or a photon flux to promote an electrochemical or photochemical reaction. Click here for examples of flow chemistry performed in Vapourtec systems Flow chemistry differs from conventional batch chemistry by having the following important features: Flow of reagents In Flow chemistry reagents are pumped under pressure and flow continuously through the reactor. This contrasts with batch reactors where all reagents are loaded into a vessel at the start https://www.vapourtec.com Control of reaction time Reaction time is determined by the time the reagents take to flow through the reactor. This period is called the residence time. Control of stoichiometry Reaction stoichiometry is controlled by the relative flow rates of the reactants. The concentration of one reagent relative to another can be increased simply by pumping that reagent at a higher rate of flow. Heat transfer Flow reactors have excellent heat transfer when compared with batch reactors. This feature is due to the much greater surface area to volume ratio of flow reactors over batch reactors. -
Recent Advances in Microflow Photochemistry
Molecules 2011, 16, 7522-7550; doi:10.3390/molecules16097522 OPEN ACCESS molecules ISSN 1420-3049 www.mdpi.com/journal/molecules Review Recent Advances in Microflow Photochemistry Michael Oelgemöller 1,* and Oksana Shvydkiv 2 1 School of Pharmacy and Molecular Sciences, James Cook University, Townsville, QLD 4811, Australia 2 School of Chemical Sciences, Dublin City University, Dublin 9, Ireland * Author to whom correspondence should be addressed; E-Mail: [email protected]; Tel.: +61-7-4781-4543; Fax: +61-7-4781-6078. Received: 12 August 2011; in revised form: 31 August 2011 / Accepted: 31 August 2011 / Published: 5 September 2011 Abstract: This review summarizes recent advances in microflow photochemical technologies and transformations. The portfolio of reactions comprises homogeneous and heterogeneous types, among them photoadditions, photorearrangements, photoreductions, photodecarboxylations, photooxygenations and photochlorinations. While microflow photochemistry is most commonly employed as a micro-scale synthesis tool, scale-up and technical production processes have already been developed. Keywords: photochemistry; microflow chemistry; microreactor 1. Introduction Synthetic organic photochemistry uses light as an energy source to initiate chemical transformations. Following this approach, a large variety of photoreactions with high selectivity, chemical yields and photon efficiencies have been developed [1-3]. Due to its easy generation, control and handling, light (in particular sunlight) is also considered as a ‘clean and traceless reagent’. Consequently, photochemistry has earned its place among the green and sustainable technologies [4-6]. Despite these advantages, however, photochemical reactions in chemical production or R&D processes are rare. Most technical processes are limited to commodity chemicals and have been developed decades ago [7,8]. -
Application of Catalysts to Metal Microreactor Systems
15 Application of Catalysts to Metal Microreactor Systems Pfeifer Peter Institute for Micro Process Engineering, Karlsruhe Institute of Technology, Germany 1. Introduction Applying microsystems for heterogeneously catalyzed processes means that the surface of tiny channels or structures has to be functionalized. Considering the surface-to-volume ratio of microchannels, volume specific surfaces of microchannels in the order of 105 up to 106 m2/m3 can be obtained. However, when combining the channels to reactors the entire fabrication technique and the necessary connection to conventional equipment lowers the overall surface-to-volume ratio to roughly 2*103 up to 2*104 m2/m3 and thus increases costs for materials and manufacture. Taking into account the demand of catalysis, i.e. the necessary “edges and corners” of the active species and the surface area of conventional catalyst support materials of 107 up to 109 m2/m3, the surface-to-volume ratio of the microsystems is not necessarily sufficient. Reviewing the literature only few cases are reported, where the geometric surface of the microsystem, e.g. channels made in copper or silver metal, is high enough ensuring cost competitive micro process engineering equipment. The reaction rates per surface site need to be very high, so that the volume specific heat flux is in a range that the advantage of microsystems, i.e. the high heat transfer rates, can be utilized for improving chemical processes in terms of process intensification. Two approaches are often applied for increasing the geometric surface, the application of a micro fixed bed, also often called “packed bed microreactors”, or the surface coating with support material and catalytically active species. -
1 Flow Photochemistry – a Green Technology with a Bright Future
1 1 Flow Photochemistry – a Green Technology with a Bright Future Michael Oelgemöller, Tyler Goodine, and Padmakana Malakar 1.1 Introduction to Synthetic Organic Photochemistry According to the International Union of Pure and Applied Chemistry (IUPAC), photochemistry is “the branch of chemistry concerned with the chemical effects of ultraviolet, visible, or infrared radiation” [1]. Owing to the multidisciplinary nature of light, photochemistry thus finds widespread applications in the fields of analytical, environmental, food, inorganic, material, medicinal, organic, phar- maceutical, polymer, and physical chemistry [2, 3]. In terms of organic synthesis, light energy is utilized to activate molecules within their chromophoric groups. For multichromophoric substrates, this activation can be selectively achieved [4]. The amount of energy required for activation corresponds to the wavelength of the light as expressed in the Planck relation (Equation 1.1) [5]: E = h × v = h × c∕ = h × c × ̃ (1.1) where E is the energy of light; h,thePlanckconstant;v, the frequency; c,the velocity of light; , the wavelength; and ̃, the wavenumber. The excited state reached can undergo a multitude of energy- as well as electron-transfer processes, which are commonly shown in a Jablonski diagram [6]. Deactivation processes are common and include fluorescence, phospho- rescence, or internal conversion. Alternatively, the excited state energy can be utilized for chemical changes. Owing to the different structural and physic- ochemical properties of excited states, photochemical reactions can differ significantly from thermal reactions. There are three main photochemical pro- cesses (Scheme 1.1) [1]: direct excitation, photosensitization, and photoinduced electron transfer reactions. In the first case, light is absorbed by the substrate anditssubsequentexcitedstatecanundergoachemicaltransformationeither on its own or by reaction with another (ground-state) molecule. -
Flow Chemistry in Contemporary Chemical Sciences: a Real Variety of Its Applications
molecules Review Flow Chemistry in Contemporary Chemical Sciences: A Real Variety of Its Applications Marek Trojanowicz 1,2 1 Laboratory of Nuclear Analytical Methods, Institute of Nuclear Chemistry and Technology, Dorodna 16, 03–195 Warsaw, Poland; [email protected] 2 Department of Chemistry, University of Warsaw, Pasteura 1, 02–093 Warsaw, Poland Academic Editor: Pawel Ko´scielniak Received: 17 February 2020; Accepted: 16 March 2020; Published: 21 March 2020 Abstract: Flow chemistry is an area of contemporary chemistry exploiting the hydrodynamic conditions of flowing liquids to provide particular environments for chemical reactions. These particular conditions of enhanced and strictly regulated transport of reagents, improved interface contacts, intensification of heat transfer, and safe operation with hazardous chemicals can be utilized in chemical synthesis, both for mechanization and automation of analytical procedures, and for the investigation of the kinetics of ultrafast reactions. Such methods are developed for more than half a century. In the field of chemical synthesis, they are used mostly in pharmaceutical chemistry for efficient syntheses of small amounts of active substances. In analytical chemistry, flow measuring systems are designed for environmental applications and industrial monitoring, as well as medical and pharmaceutical analysis, providing essential enhancement of the yield of analyses and precision of analytical determinations. The main concept of this review is to show the overlapping of development trends in the design of instrumentation and various ways of the utilization of specificity of chemical operations under flow conditions, especially for synthetic and analytical purposes, with a simultaneous presentation of the still rather limited correspondence between these two main areas of flow chemistry. -
Flow Chemistry Presented by 22-23 MAY 2019 Prof
Graz, Austria Das Weitzer FLOW A 2 day course presented by Prof. C Oliver Kappe & Dr Will Watson CHEMISTRY A 1 day Masterclass in Flow Chemistry presented by 22-23 MAY 2019 Prof. C Oliver Kappe NEW Flow Chemistry MASTERCLASS 24 MAY 2019 www.scientificupdate.com | [email protected] FLOW CHEMISTRY Multiple attendees discounts UP TO 15% 22-23 May 2019 Graz, Austria, Das Weitzer available INTRODUCTION COURSE OUTLINE Flow chemistry has been used in 1. Introduction to Flow Chemistry 4. High-Temperature / petrochemical and bulk chemical and Microreactors Pressure Flow Chemistry production for over 100 years but a. General references a. Flow chemistry in high-T/p process has only really been taken up b. Basic principles/advantages of windows (Novel Process Windows), in the pharmaceutical and fine microreactor technology: definitions, translating microwave protocols to chemical industries over the last mixing efficiency, flow regimes, heat flow, flow microwave chemistry 10 years or so. and mass transfer 5. Physical and Analytical Aspects This course aims to give an c. Equipment review: microreactors, of Flow Chemistry introduction to the subject and an mesofluidic/tubular reactors, cartridge- a. Handling solids in flow systems overview of the current state of the based systems b. Inline / online reaction monitoring art. A variety of chemical reactions d. Operative principles in flow: residence c. Regulatory aspects related to the in flow and how to translate a time, flow rate, back pressure, yield development of flow processes conventional reaction in to a flow 2. Microreactor Chemistry Concepts / Problem Session 2 – Group Work process will be described. Examples 6. -
Applications, Benefits and Challenges of Flow Chemistry
flow chemistry Krist V. Gernaey Applications, benefits and challenges of flow chemistry ALEKSANDAR MITIC, SØREN HEINTZ, ROLF H. RINGBORG, VIJAyA BODLA, JOHN M WOODLEy, KRIST V. GERNAEy* *Corresponding author 1. Technical University of Denmark (DTU), Department of Chemical and Biochemical Engineering, Søltofts Plads, Building 229, 2800 Kgs. Lyngby, Denmark KEyWORDS MICRO-CHEMICAL PROCESSING IN ORGANIC SyNTHESIS Flow chemistry; Organic Synthesis; Biocatalysis; Process Organic synthesis can be performed in continuous mode by Analytical Technology (PAT); Microreactor Technology. using mini- and micro-structured flow devices. Small scale continuous flow technology has many potential advantages, such as: rapid heat and mass transfer, increased safety, easy ABSTRACT scale-up/scale-out, fast process characterization, potential for real-time release, operation with unstable reaction Organic synthesis (incorporating both chemo-catalysis species, and so on (9, 10). Due to such advantages and biocatalysis) is essential for the production of a wide integration of these small scale devices in plant architectures range of small-molecule pharmaceuticals. However, has become more common in the last two decades (11). It is traditional production processes are mainly based on important to note here that not all chemical reactions are batch and semi-batch operating modes, which have suited to such small-scale equipment. For example, disadvantages from an economic, environmental according to Roberge et al. (12), chemical reactions with a and manufacturing perspective. A potential solution 4 half-life higher than 10 min should preferably be operated in to resolve these issues is to use flow chemistry in such batch manufacturing mode. However, it has been processes, preferably with applications of micro- and demonstrated that some of these reactions too could be mini-sized equipment.