Development of an Industrial Multi‐Injection Microreactor for Fast and Exothermic Reactions – Part II

Roberge, Dominique M.; Bieler, Nikolaus; Mathier, Meinrad; Eyholzer, Markus; Zimmermann, Bertin; Barthe, Philippe; Guermeur, Céline; Lobet, Olivier; Moreno, Maxime; Woehl, Pierre

doi:10.1002/ceat.200800131

Cited by 70 publications

(64 citation statements)

References 18 publications

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“…As already pointed out by Roberge et al [10], the advantage gained by increasing from one injection point to three injection points are more important compared to the ones obtained by moving from three to five injection points (see Figure 4). Therefore, in general, more than six injection points do not lead to a decisive gain as seen from Figure 4.…”

Section: Simulation Resultssupporting

confidence: 50%

“…Among other strategies to carry out very fast exothermic reactions [8,10], the multi-injection microstructured reactor represents a promising solution to control temperature while keeping the channel diameter in a reasonable range ( > 100 μm). Compared to a single-injection reactor, where both reactants are fed together at the inlet, in the multi-injection reactor one of the reactants is fed at several distinct points along reactor length.…”

Section: Introductionmentioning

confidence: 99%

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Multi-injection microstructured reactor for intensification of fast exothermic reactions: proof of concept

Haber

Jiang²,

Maeder

et al. 2013

Green Processing and Synthesis

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Quasi-instantaneous exothermic reactions lead to the formation of unwanted hot spots even when carried out in conventional microstructured reactors (MSR) with tube diameter of 100-1000 μm. For this reason, alternative MSR designs are warranted to enable process intensification of fast reactions with characteristic reaction times < 1 s. The continuous multi-injection MSR, where one of the reactants is successively added to the main flow of reactants along reactor length, may improve temperature control. The latter was studied first theoretically using numerical simulations and then experimentally with the cyclisation of pseudoionone to α-and β-ionones as a model reaction. The multi-injection MSR made of low temperature co-fired ceramics (LTCC) led to a yield of α-ionone and β-ionone > 0.98 reaching a 500-fold process intensification as compared to the conventional semibatch process. The temperature profiles monitored by quantitative infrared thermal imaging confirmed an 8-fold reduced temperature rise compared to adiabatic temperature rise, which was achieved by injecting the reactants at three different injection points.Keywords: exothermic; microstructured reactor; multiinjection; pseudoionone; temperature. Dimensionless numbersRe Reynolds number u⋅d h /ν [-]

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Section: Simulation Resultssupporting

confidence: 50%

Section: Introductionmentioning

confidence: 99%

Multi-injection microstructured reactor for intensification of fast exothermic reactions: proof of concept

Haber

Jiang²,

Maeder

et al. 2013

Green Processing and Synthesis

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“…An application of this multi-injection protocol was the Grignard reaction between phenylethylmagnesium bromide and 2-chloropropionyl chloride. 82 A four-injection strategy was sufficient to temper the exotherm of the reaction and allowed to increase the selectivity of the reaction up to 50% yield. Furthermore, the heat management in microreactor systems can also be improved by applying a multi-stage temperature ramping approach.…”

Section: Heat Transport Phenomenamentioning

confidence: 99%

Beyond Organometallic Flow Chemistry: The Principles Behind the Use of Continuous-Flow Reactors for Synthesis

Noël

Hessel

2015

Topics in Organometallic Chemistry

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Flow chemistry is typically used to enable challenging reactions which are difficult to carry out in conventional batch equipment. Consequently, the use of continuous-flow reactors for applications in organometallic and organic chemistry has witnessed a spectacular increase in interest from the chemistry community in the last decade. However, flow chemistry is more than just pumping reagents through a capillary and the engineering behind the observed phenomena can help to exploit the technology's full potential. Here, we give an overview of the most important engineering aspects associated with flow chemistry. This includes a discussion of mass-, heat-, and photon-transport phenomena which are relevant to carry out chemical reactions in a microreactor. Next, determination of intrinsic kinetics, automation of chemical processes, solids handling and multistep reaction sequences in flow are discussed. Safety is one of the main drivers to implement continuous-flow microreactor technology in an existing process and a brief overview is given here as well. Finally, the scale-up potential of microreactor technology is reviewed.

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“…Continuous-flow reactors (CFRs) represent an emerging technology that is becoming more accepted in industrial settings due to the advantages they offer over batch reactors. Advantages include more efficient mixing schemes, rapid heat transfer, and improved user safety [2][3][4][5]. These advantages allow for consistent, reproducible, and continuous production of chemical compounds.…”

Section: Introductionmentioning

confidence: 99%

“…The ylide can now collapse by intermolecular hydrogen transfer to form dimethylsufide and the carbonyl product (10). (8) and (9), styrene, and recovery of alcohol (4) Potential side reactions (the area outside of the central column in Figure 1): At temperatures over −30°C, intermediate 1 (3) can undergo a Pummerer rearrangement reaction and form methylthiometyl trifluoroacetate (7). In the presence of base, (7) can experience a base catalyzed alcoholysis with S-1-phenylethanol (4) to form sec-phenethyl trifluoroacetate (9).…”

Section: Introductionmentioning

confidence: 99%

Moffat-Swern Oxidation of Alcohols: Translating a Batch Reaction to a Continuous-Flow Reaction

Bleie¹,

Roberto²,

Dearing³

et al. 2015

J Flow Chem

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The Moffatt-Swern oxidation (MSO) is a multistep, versatile, metal-free reaction by which alcohols are transformed into aldehydes and ketones. Batch MSO requires low temperatures (−70°C) due to a highly exothermic reaction step that generates intermediates. This work shows that a rigorous investigation of the MSO in batch can be used as a stepping-stone to its implementation in a continuous-flow reactor (CFR). This work has two parts: the first part details the investigation of MSO in batch; the second covers the translation of the knowledge derived from batch to a CFR. The MSO batch reaction was performed under cryogenic conditions with real-time process monitoring. The reaction was monitored with Raman spectroscopy and could be tracked throughout the reaction. All concentrations were validated using offline high-performance liquid chromatography (HPLC) and gas chromatography-mass spectrometry (GC-MS). Two configurations of the CFR were produced. Configuration 1 used the traditional batch methodology in terms of reagent addition and reaction conditions. Configuration 2 used the information derived from the batch reaction, changing the order of the reagent addition and increasing the temperature of the reactor. Real-time quantitative monitoring of chemical yield in the CFR was demonstrated via Raman spectroscopy and partial least squares (PLS) regression modeling. Reaction yield was accurately predicted every 15 s, reducing the need for chromatographic validation once the model was built. Configuration 2 was shown to perform comparably to configuration 1 at low temperature and far outperforming it at higher temperatures. Both CFR configurations performed significantly better than the batch setup in terms of temperature and yield, as was expected.

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Development of an Industrial Multi‐Injection Microreactor for Fast and Exothermic Reactions – Part II

Cited by 70 publications

References 18 publications

Multi-injection microstructured reactor for intensification of fast exothermic reactions: proof of concept

Multi-injection microstructured reactor for intensification of fast exothermic reactions: proof of concept

Beyond Organometallic Flow Chemistry: The Principles Behind the Use of Continuous-Flow Reactors for Synthesis

Moffat-Swern Oxidation of Alcohols: Translating a Batch Reaction to a Continuous-Flow Reaction

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