Micro-batch reactor for catching intermediates and monitoring kinetics of rapid and exothermic homogeneous reactions

Kashid, Madhvanand N.; Detraz, Olivier; Moya, Mireia Santacana; Yuranov, Igor; Prechtl, Petra; Membrez, Jacques; Renken, Albert; Kiwi‐Minsker, Lioubov

doi:10.1016/j.cej.2012.10.019

Cited by 12 publications

(17 citation statements)

References 24 publications

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“…This confirms the results published by Kashid et al [13] and [14], who showed that a ratio of acid:pseudoionone in the order of 5 is required for the reaction to complete.…”

Section: Reduction Of Solvent Masssupporting

confidence: 82%

“…Kashid et al. characterized the two first reaction steps, whose quasi-instantaneous intrinsic kinetics are difficult to monitor [13]. Hence, temperature control during the two first reaction steps is challenging.…”

Section: Model Reactionmentioning

confidence: 99%

“…Due to the very fast kinetics, mixing plays a crucial role since the acid concentrations influence product distribution and the global transformation rate. The target products, α-and β-ionone, are used in perfumery and in the synthesis of vitamin Kashid et al proposed a reaction scheme and investigated the kinetics including the different reaction steps under homogeneous conditions using 1-nitropropane as solvent [13] and [14].…”

Section: Model Reactionmentioning

confidence: 99%

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Intensification of highly exothermic fast reaction by multi-injection microstructured reactor

Haber

Jiang

Maeder

et al. 2014

Chemical Engineering and Processing: Process Intensification

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Microstructured reactors (MSR) with characteristic dimensions below 100 µm are warranted to maintain close to isothermal conditions when carrying out quasi-instantaneous highly exothermic reactions. Unfortunately, such small dimensions increase the risk of clogging, create high pressure drop and are costly to number-up. The multi-injection (MI) MSR, where one of the reactants is added stepwise along the reactor length, allows working with larger dimensions (diameter >500 µm) while maintaining good temperature control. Herein presented MI-MSR is made of low temperature co-fired ceramics (LTCC) with herringbone mixing structure inside the reactor channels and is shown to mix efficiently in a large range of Reynolds numbers Re = 20-130. The cyclization of pseudoionone is studied as a model of a highly exothermic fast reaction. The temperature profiles are characterized by a quantitative infrared thermography. The developed LTCC MI-MSR allows ∼8-fold reduction of hot spot temperature as compared to the adiabatic temperature rise. Moreover, ∼500-fold intensification is achieved as compared to the conventional semi-batch process with reduced solvent mass by a factor of 2 while attaining a yield of target product above 98%. n reaction order, [-]

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“…This confirms the results published by Kashid et al [13] and [14], who showed that a ratio of acid:pseudoionone in the order of 5 is required for the reaction to complete.…”

Section: Reduction Of Solvent Masssupporting

confidence: 82%

Section: Model Reactionmentioning

confidence: 99%

Section: Model Reactionmentioning

confidence: 99%

See 1 more Smart Citation

Intensification of highly exothermic fast reaction by multi-injection microstructured reactor

Haber

Jiang

Maeder

et al. 2014

Chemical Engineering and Processing: Process Intensification

Self Cite

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show abstract

“…Under certain reaction conditions, α-ionone can be transformed to β-ionone (isomerization). Kashid et al [18,21] recently published two studies giving deeper insight into the reaction mechanism of the cyclisation of pseudoionone to β-ionone. At first, they carried out kinetic measurements of the relatively slow and slightly endothermic isomerization reaction in a batch reactor with nitropropane as solvent maintaining the molar ratio of pseudoionone to H 2 SO 4 at 1:4.8.…”

Section: Model Reactionmentioning

confidence: 99%

“…The isomerization follows first order kinetics with respect to α-ionone with an activation energy of E A = 65 kJ/mol and a frequency factor of k 0 = 5.4⋅10 10 1/s [18]. Subsequently, the very exothermic cyclization of pseudoionone to the final product β-ionone was studied [21]. Due to the rapidity of the reaction, they switched from a batch vessel to a microreactor based system.…”

Section: Model Reactionmentioning

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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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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Overview of Micro Reaction Engineering

2014

Microstructured Devices for Chemical Processing

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Micro-batch reactor for catching intermediates and monitoring kinetics of rapid and exothermic homogeneous reactions

Cited by 12 publications

References 24 publications

Intensification of highly exothermic fast reaction by multi-injection microstructured reactor

Intensification of highly exothermic fast reaction by multi-injection microstructured reactor

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

Overview of Micro Reaction Engineering

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