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Characterization of reaction enthalpy and kinetics in a microscale flow platform
Reaction Chemistry & Engineering ( IF 3.4 ) Pub Date : 2020-09-30 , DOI: 10.1039/d0re00304b
Agnieszka Ładosz 1, 2, 3, 4 , Christina Kuhnle 1, 2, 3, 4 , Klavs F. Jensen 1, 2, 3, 4
Affiliation  

We report an isothermal flow calorimeter for characterization of reaction enthalpy and kinetics. The platform consists of a thermoelectric element and a glass–silicon microreactor to measure heat flux and an inline IR spectrometer to monitor reaction conversion. The thermally insulated assembly is calibrated with a thin film heater placed between the microreactor and the thermoelectric element. Without any reconfiguration of hardware, the setup can also be used to efficiently characterize reaction kinetics in transient flow experiments. We tested the calorimeter with hydrolysis of acetic anhydride as a model reaction. We determined the exothermic reaction enthalpy and the endothermic heat of mixing of the reagent to be −63 ± 3.0 kJ mol−1 and +8.8 ± 2.1 kJ mol−1 respectively, in good agreement with literature values and theoretical predictions. Following calorimetry studies, we investigated reaction kinetics by applying carefully controlled residence time ramps at four different temperatures, and we obtained kinetic rate constants of 0.129 min−1 up to 0.522 min−1 for temperatures between 20 °C and 56.3 °C, also fitting well with data reported in the literature.

中文翻译:

微型流动平台中反应焓和动力学的表征

我们报告了等温流动量热仪表征反应焓和动力学。该平台由一个热电元件和一个玻璃硅微反应器(用于测量热通量)和一个在线红外光谱仪(用于监测反应转化)组成。用放置在微反应器和热电元件之间的薄膜加热器对隔热组件进行校准。无需对硬件进行任何重新配置​​,该设置还可用于在瞬态流实验中有效表征反应动力学。我们用乙酸酐水解测试了量热仪,将其作为模型反应。我们确定放热反应焓和试剂混合的吸热为-63±3.0 kJ mol -1和+8.8±2.1 kJ mol -1分别与文献价值和理论预测相吻合。经过量热法研究,我们通过在四个不同温度下应用精心控制的停留时间梯度来研究反应动力学,对于20°C至56.3°C之间的温度,我们获得的动力学速率常数为0.129 min -1至0.522 min -1与文献报道的数据相吻合。
更新日期:2020-10-07
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