Coupling Continuous Flow Microreactors to MicroNIR Spectroscopy: Ultracompact Device for Facile In-Line Reaction Monitoring,Organic Process Research & Development

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Coupling Continuous Flow Microreactors to MicroNIR Spectroscopy: Ultracompact Device for Facile In-Line Reaction Monitoring
Organic Process Research & Development ( IF 3.1 ) Pub Date : 2018-06-12 00:00:00 , DOI: 10.1021/acs.oprd.8b00060
Renan Galaverna ₁ , Rafael L. Ribessi ₁ , Jarbas J. R. Rohwedder ₁ , Julio C. Pastre ₁

Affiliation

In this study, we applied a portable near-infrared spectrophotometer (MicroNIR) for in-line monitoring of the synthesis of 5-hydroxymethylfurfural (5-HMF) in a continuous flow microreactor. Under the best reaction conditions using isopropyl alcohol/dimethyl sulfoxide as the reaction solvent and a fixed-bed reactor packed with solid acid catalyst, total conversion of d-fructose was observed, and 5-HMF was obtained in 95% yield with a residence time of just 11.2 min. Principal component analyses and construction of multivariate control charts based on Hotelling’s T² and Q residuals were also performed and proved the excellent response of the compact MicroNIR device for in-line monitoring of 5-HMF production without variation in the yield over 8 h/day during 5 days. Our results demonstrate the great potential for the application of this compact device in the monitoring of laboratory-scale reactions, which can be extended to industrial scales.

中文翻译：

连续流微反应器与MicroNIR光谱的耦合：用于紧凑的在线反应监测的超紧凑设备

在这项研究中，我们应用了便携式近红外分光光度计（MicroNIR）在线监测连续流微反应器中5-羟甲基糠醛（5-HMF）的合成。在使用异丙醇/二甲基亚砜作为反应溶剂和装有固体酸催化剂的固定床反应器的最佳反应条件下，观察到d-果糖的总转化率，并以95％的收率和停留时间获得了5-HMF。仅11.2分钟。基于Hotelling的T ²和Q的主成分分析和多元控制图的构建还进行了残留实验，证明了紧凑型MicroNIR装置对5-HMF生产进行在线监测的出色响应，在5天内，每天8 h的产量没有变化。我们的结果证明了这种紧凑型设备在实验室规模反应监测中的巨大潜力，可以扩展到工业规模。

更新日期：2018-06-12

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