Modeling ethyl diazoacetate synthesis in an adiabatic microchemical system

Lü, Yangcheng; Xin, Dawei; Zhang, Jisong; Luo, Guangsheng

doi:10.1016/j.cej.2015.03.028

Cited by 10 publications

(6 citation statements)

References 27 publications

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“…For the ring‐opening reaction of ECH with NDA, the residence time in the microreactor (10 min) was much longer than the characteristic mixing time (typical in the range of 0.01–1 s), 21 thus the mixing performance has little effect on the reaction. The heat exchange capability of the microreaction system is excellent, 22 so rapid heating can be achieved even at very low flow velocity. In all the experiments shown in this work, the selection range of flow velocity is relatively free from 0.03 to 1.1 cm·s −1 .…”

Section: Resultsmentioning

confidence: 99%

Highly efficient two‐stage ring‐opening of epichlorohydrin with carboxylic acid in a microreaction system

et al. 2022

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Ring-opening of epoxides with carboxylic acids has been widely used to prepare many high value intermediates in the polymer and pharmaceutical industries. Most of conventional processes proceeded in batch stirred reactors. As such they always suffer from low productivity and selectivity. Here we developed an advanced technology to perform the ring-opening reaction of epichlorohydrin with neodecanoic acid (NDA) for continuous production of 3-chloro-2-hydroxypropyl neodecanoate in a more efficient and safer way. A microreaction system where a microreactor connected to a stirred reactor was established. When the conversion of NDA rapidly reaching around 90% in a microreactor at 110 C, the reaction solution was transferred to a stirred reactor at 90 C. This two-stage operating mode can reduce the reaction time and improve the selectivity through free switching of temperature in the consecutive two reactors, thus substantially reducing the consumption of energy and materials.

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Section: Resultsmentioning

confidence: 99%

Highly efficient two‐stage ring‐opening of epichlorohydrin with carboxylic acid in a microreaction system

et al. 2022

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“…These are the primary reactions taking place. The formed carbene can undergo numerous secondary reactions, forming dimers, oligomers, or an alcohol by the reaction with water molecules [37,38]. These reactions, due to growing complexity, are not considered here.…”

Section: Reaction Model For Diazo Acetonitrile Synthesis and Decompos...mentioning

confidence: 99%

Continuous Synthesis of Diazo Acetonitrile: From Experiments to Physical and Grey‐Box Modeling

Baldan,

Blauth,

Bošković

et al. 2024

Chemie Ingenieur Technik

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Diazo compounds are gathering interest for their potential in promoting greener synthesis routes. We investigate, at a lab‐scale, the continuous synthesis of diazo acetonitrile (DAN) using a micro‐structured flow reactor and a flow reaction calorimeter. Data concerning DAN formation in the former, and relative to reaction heat and gas flow rate in the latter, are collected. We present a physical and a grey‐box model, both of which are calibrated to our data. Compared to the physical model, the grey‐box approach allows to better incorporate the complex chemical reaction pathways of DAN.

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“…31−34 Besides, the microtube reactors have enhanced heat transfer performance to inhibit the formation of hot spot effectively. 35−37 By now, microtube reactors have been successfully used to measure the kinetics of different reactions in gas phase, 38 liquid phase, 39 and heterogeneous catalytic system. 40 In this work, we carried out kinetic measurements on the thermal decomposition of EDA using microtube reactor by monitoring the concentrations of EDA and main products at various residence times and established a quantitative model considering simplified multistep reaction mechanism based on a comprehensive experiment data regression.…”

Section: N Chco Etmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

“…To this end, experimental data corresponding to strictly controlled reaction conditions and residence time are required, which are difficult to obtain in a conventional stirred reactor because the decomposition of EDA seems to be fast and highly exothermic The microtube reactor with the characteristic dimension less than 1 mm is a device that could transfer the reaction time into reaction pipeline volume precisely, so it has precise control ability for reaction time. − This property makes the microtube reactors especially appropriate for handling the reactions involving active reactants, products, or intermediates with a short lifetime under reaction conditions. − Besides, the microtube reactors have enhanced heat transfer performance to inhibit the formation of hot spot effectively. − By now, microtube reactors have been successfully used to measure the kinetics of different reactions in gas phase, liquid phase, and heterogeneous catalytic system …”

Section: Introductionmentioning

confidence: 99%

See 1 more Smart Citation

Thermal Decomposition of Ethyl Diazoacetate in Microtube Reactor: A Kinetics Study

Xin

2018

ACS Omega

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Ethyl diazoacetate (EDA) commonly experiences intensive decomposition as well as complex conversion concerning safety and efficiency. In this work, a careful kinetics study on the thermal decomposition of EDA was isothermally conducted in a microtube reactor to establish a mechanism-based kinetic model. The model parameters were well calibrated with experimental data including the yield of dimmers and the conversion of EDA, confirming the rationality of the proposed three-step reaction route. It allows the model to concisely describe the complex species transformations during EDA decomposition, which is unavailable for an apparent kinetic model. Considering an isothermal reaction system and the tolerance of EDA consumption by thermal decomposition, this work could help reveal the requirement on the kinetic characteristics of the desired catalytic reaction in which EDA is involved, as a reference on reaction process modeling and regulation.

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Modeling ethyl diazoacetate synthesis in an adiabatic microchemical system

Cited by 10 publications

References 27 publications

Highly efficient two‐stage ring‐opening of epichlorohydrin with carboxylic acid in a microreaction system

Highly efficient two‐stage ring‐opening of epichlorohydrin with carboxylic acid in a microreaction system

Continuous Synthesis of Diazo Acetonitrile: From Experiments to Physical and Grey‐Box Modeling

Thermal Decomposition of Ethyl Diazoacetate in Microtube Reactor: A Kinetics Study

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