Online process monitoring of a batch distillation by medium field NMR spectroscopy
Online process monitoring of a batch distillation by medium field NMR spectroscopy
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DOI：
10.1016/j.ces.2020.115561
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发表时间：
2020-06-29
影响因子：
4.7
通讯作者：
Hasse, Hans
中科院分区：
文献类型：
--
作者：
Friebel, Anne;von Harbou, Erik;Hasse, Hans
中场NMR光谱仪对于在线过程监测是有吸引力的。因此，在目前的工作中，一个单级实验室间歇蒸馏仍然耦合在线与中场核磁共振光谱仪。这使得能够在没有校准的情况下进行定量非侵入性测量。用该技术研究了二甲基亚砜+乙腈+甲酸乙酯和乙酸乙酯+丙酮+乙醚两个三元体系的等压和等温残液曲线，以及乙酸+吡啶和甲醇+二乙胺两个二元体系的沸点曲线和高沸点共沸物。将在线NMR光谱分析的结果与离线分析的结果以及使用文献数据参数化的NRTL参数的热力学建模的结果进行比较。在线过程监测的新方法提供了可靠的结果，非常适合快速和稳健的残留曲线测量。(C)2020爱思唯尔有限公司保留所有权利。
Medium field NMR spectrometers are attractive for online process monitoring. Therefore, in the present work, a single-stage laboratory batch distillation still was coupled online with a medium field NMR spectrometer. This enables quantitative non-invasive measurements without calibration. The technique was used for studying isobaric and isothermal residue curves in two ternary systems: (dimethyl sulfoxide + acetonitrile + ethyl formate) and (ethyl acetate + acetone + diethyl ether) and boiling curves and high-boiling azeotropes in two binary systems: (acetic acid + pyridine) and (methanol + diethylamine). The results of the online NMR spectroscopic analysis were compared to results from offline analysis as well as to results from thermodynamic modeling using NRTL parameters that were parametrized with literature data. The new method for online process monitoring gives reliable results and is well-suited for fast and robust measurements of residue curves. (C) 2020 Elsevier Ltd. All rights reserved.