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Flow Toolkit for Measuring Reaction Enthalpy and Application to Highly Exothermic Synthesis of Alkylaluminoxanes
Organic Process Research & Development ( IF 3.1 ) Pub Date : 2022-04-19 , DOI: 10.1021/acs.oprd.2c00072
Mengbo Zhang 1 , Yirong Feng 1 , Linjin Lou 1 , Haomiao Zhang 1 , Jingdai Wang 1 , Yongrong Yang 1
Affiliation  

We present a flow strategy to characterize reaction enthalpy and showcase the application in synthesis of alkylaluminoxanes from the fast and exothermic alkylaluminum hydrolysis. Our platform mainly encompasses a three-dimensional printed micromixer and a tubular reactor in an adiabatic vacuum box, aided by a thermal imaging camera to record temperature profiles. The temperature increase at steady state is used to calculate the released heat, which is further decoupled to quantify the reaction enthalpy and enthalpy of mixing. We validate the concept with the classic neutralization reaction between sulfuric acid and sodium hydroxide, with less than 2% deviation from theoretical values. In application, we determine the exothermic reaction enthalpy and the endothermic enthalpy of mixing to be −143.13 and +7.66 kJ/mol for triisobutylaluminum hydrolysis and −164.63 and +5.03 kJ/mol for trimethylaluminum hydrolysis, respectively. The presented platform, on the one hand, yields new insights into the microreactor scale-up for alkylaluminoxane synthesis and, on the other hand, can be readily used to measure reaction enthalpies of other reactions.

中文翻译:

测量反应焓的流量工具包及其在烷基铝氧烷高放热合成中的应用

我们提出了一种流动策略来表征反应焓,并展示了通过快速和放热的烷基铝水解合成烷基铝氧烷中的应用。我们的平台主要包括一个 3D 打印微型混合器和一个位于绝热真空箱中的管式反应器,并借助热成像相机记录温度曲线。稳态下的温度升高用于计算释放的热量,进一步解耦以量化反应焓和混合焓。我们通过硫酸和氢氧化钠之间的经典中和反应验证了这一概念,与理论值的偏差小于 2%。在应用中,我们确定放热反应焓和混合吸热焓分别为 -143.13 和 +7。三异丁基铝水解为 66 kJ/mol,三甲基铝水解分别为 -164.63 和 +5.03 kJ/mol。一方面,所提出的平台对烷基铝氧烷合成的微反应器放大产生了新的见解,另一方面,可以很容易地用于测量其他反应的反应焓。
更新日期:2022-04-19
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