Monitoring Aqueous Phase Reactions by Operando ATR‐IR Spectroscopy at High Temperature and Pressure: A Biomass Conversion Showcase

Spectroscopic insight into aqueous phase catalytic reactions under realistic conditions aids detailed understanding and fosters further improvements. However, this is also very challenging, particularly in the liquid phase, given the typically elevated temperatures and pressures employed. Here, we r...

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Vydáno v:Chemistry methods Ročník 1; číslo 11; s. 468 - 476
Hlavní autoři: Khalili, Khaled N. M., Peinder, Peter, Bruijnincx, Pieter C. A., Weckhuysen, Bert M.
Médium: Journal Article
Jazyk:angličtina
Vydáno: Weinheim John Wiley & Sons, Inc 01.11.2021
Témata:
aqueous phase reforming
ATR-IR spectroscopy
Biomass
Catalysis
Cellulose
chemometrics
Gases
High temperature
Hydrogen
Light
Lignin
Lignocellulose
operando spectroscopy
Reagents
Solvents
ISSN:2628-9725, 2628-9725
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Shrnutí:Spectroscopic insight into aqueous phase catalytic reactions under realistic conditions aids detailed understanding and fosters further improvements. However, this is also very challenging, particularly in the liquid phase, given the typically elevated temperatures and pressures employed. Here, we report an operando Attenuated Total Reflectance‐Infrared (ATR‐IR) spectroscopic method to monitor the Aqueous Phase Reforming (APR) of Kraft lignin at 225 °C and 30 bar over a Pt/Al2O3 catalyst. This is a showcase reaction, while the presented method developed is more generic. In addition to the high temperature and pressures conditions, spectral interference from bulk water is a major challenge. Other challenges include self‐absorption of IR light, molecular interactions, high substrate loadings and the noise resulting from water vapor and CO2. We present a protocol utilizing the temperature‐dependent single‐beam method to obtain high‐quality ATR‐IR spectra virtually free from temperature, background and matrix effects. The protocol allowed for effective correction for the aqueous solvent as a function of reaction temperature. A comparison with conventional spectral acquisition and correction shows the advantages of this approach. Operando infrared spectroscopy of aqueous phase reactions at high temperature and pressure is very appealing yet highly challenging, in particular for complex biomass‐derived feedstock such as lignin. A comprehensive protocol is presented to address the challenges associated with spectral acquisition under these reaction conditions. This protocol serves as a basis for successful implementation of on‐line monitoring technologies of aqueous/liquid phase processes, for example, in future biorefineries.
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ISSN:2628-9725
2628-9725
DOI:10.1002/cmtd.202100041