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Development of a Robust and Reusable Microreactor Employing Laser Based Mid-IR Chemical Imaging for the Automated Quantification of Reaction Kinetics
Organic Process Research & Development ( IF 3.4 ) Pub Date : 2017-10-24 00:00:00 , DOI: 10.1021/acs.oprd.7b00245
Hakan Keles 1 , Flavien Susanne 2 , Hamish Livingstone 3 , Sarah Hunter 2 , Charles Wade 4 , Rose Bourdon 1 , Andrew Rutter 2
Affiliation  

A robust, reusable microreactor coupled with laser based mid-IR chemical imaging and automated analysis is reported, for the first time, with its application to monitor and quantify fast organometallic chemistry in flow. We have investigated the subsecond organometallic addition reaction between lithium diisopropylamide and phenyl isocyanate in order to define and tune microfluidic system parameters such as residence time using physical system constraints (flow rate, reactor volume) to aid process development. The selectivity of mid-IR video rate capture of the flow response of reactants and product enabled the qualitative assessment of mixing properties. Furthermore, we report a minimally supervised automated image analysis toolbox that generates concentration as a function of residence time enabling the calculation of reaction rate constant, k, using hyperspectral data cubes. Finally, we report the reproducibility of quantification precision by measuring the rate constant, at three different flow rates with three replicates for each flow rate. These findings show the potential value of the microreactor particularly when coupled with automated mid-IR transmission analysis for the study of flow chemistry at the micron scale, assisting in the understanding of the reaction kinetics and mixing properties and enhancing the value of the chemical imaging based, automated quantification of microfluidics.

中文翻译:

基于激光的中红外化学成像的鲁棒和可重复使用的微反应器的开发,用于反应动力学的自动定量

首次报道了一种坚固,可重复使用的微型反应器,该激光器与基于激光的中红外化学成像和自动化分析相结合,首次用于监测和定量流动中的快速有机金属化学。我们已经研究了二异丙基氨基锂和异氰酸苯酯之间的亚秒有机金属加成反应,以便使用物理系统约束(流速,反应器体积)来定义和调整微流体系统参数,例如停留时间,以帮助工艺开发。对反应物和产物的流响应的中红外视频速率捕获的选择性能够对混合性能进行定性评估。此外,我们报告了一个受监督最少的自动化图像分析工具箱,该工具箱可根据停留时间生成浓度,从而能够计算反应速率常数,k,使用高光谱数据立方体。最后,我们通过测量三种不同流速下的速率常数来报告定量精度的可再现性,每种流速重复三次。这些发现显示了微反应器的潜在价值,特别是与自动中红外透射分析结合使用以研究微米级的流动化学时,有助于理解反应动力学和混合特性并提高基于化学成像的价值。 ,微流体的自动定量。
更新日期:2017-10-25
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