Unexpected formation of a 1,2-dichloroacenaphthylene in a friedel-crafts reaction with chloral hydrate

An unprecedented rearrangement was encountered during an attempted alkylation of an electron-rich naphthalene with chloral hydrate. The reaction produced a dichlorinated acenaphthylene and presumably involves the intermediate formation of a chloronium ion which is opened to produce the five-membered ring of the final product

Impact Tests and Computed Tomography Scans of Prismatic Battery Cells

Recently, the use of prismatic cells in electric vehicles has increased significantly. Unlike the cylindrical or pouch format, the prismatic cell format has not been sufficiently investigated. In this study, quasi-static mechanical tests are performed on prismatic cells. The tests include a cylindrical and a hemispherical impactor that mechanically load the cells in all three spatial directions. In both in-plane directions, a cell stack consisting of three cells is tested to capture the influence and loading of the outer cells of a cell stack. It is found out that, in the in-plane tests, short-circuiting occurs first in the outer cells and subsequently in the middle cell, which is targeted by the impactor. This result can also be supported by computed tomography scans. The results illustrate that, when evaluating the crash safety of battery cells, several cells should always be tested in order to capture the different loading of the cells

Kinetic and Scale-up Investigations of a Michael Addition in Microreactors

Microreactors are an efficient tool for process development and intensification. However, the scale-up from lab studies to small-scale commercial production is challenging, since a change in the channel dimensions requires good knowledge of heat and mass transfer phenomena. In this work, complete process development for an exothermic Michael addition is presented. In a systematic scale-up approach, kinetic studies and experimental characterization of the employed reactors provide key parameters for detailed reactor modelling. The residence time distribution, reactant mixing, and removal of reaction heat are taken into account. It is exemplarily shown how preliminary experiments can be the basis for the prediction of scale-up effects and the development of a continuous production process. Plug flow behavior and short mixing times could be confirmed for all investigated flow reactors. Furthermore, interactions of reaction kinetics and the formation of hot spots in the reactor channel were investigated. For the examined reaction, the simulations predicted the product yield under production conditions in good accuracy

Verbesserung der Gewinnungstechnik im Floez Zollverein 7/8 durch Einsatz einer Gleithobelanlage 9.30 v der GEW Luenen

SIGLEDEGerman

Fast and Efficient Acquisition of Kinetic Data in Microreactors Using In-Line Raman Analysis

This study demonstrates that a microreactor setup with fast in-line reaction monitoring by Raman spectroscopy can be a highly efficient laboratory tool for kinetic studies and process development. Using a coaxial probe and commercial spectrometer to perform real-time measurements in the microchannel prevents the need for reaction quenching, sampling, and time-consuming off-line analysis methods such as GC or HPLC. A specially designed, temperature-controlled aluminum plate microreactor was developed and tested in the exothermic synthesis of 3-piperidino propionic acid ethyl ester by Michael addition. In-line measurements through a fused quartz screen in the reactor channel, which had an increasing cross-sectional area, allowed time-series kinetic data to be collected over nearly the full range of reaction conversions. An optimum flow rate range in which nearly ideal plug flow behavior can be assumed was identified. Furthermore, a time gradient was applied to the reactant flow rates, and the product concentration was simultaneously and repeatedly measured at various locations in the reactor channel. With this approach, the experiment duration and material consumption are significantly reduced relative to those of conventional steady-state experiments. Two hundred data points with residence times ranging from 0.3 to 49 s were collected in less than 1 h. Thus, this method can be used for the high-throughput screening of reaction parameters in a microreactor