Chemical Speciation by Quick‐XAS and Raman Spectroscopy: Validation of Two Cells for in situ Time‐Resolved Monitoring of the Impregnation and Drying of CoMoP/Al2O3 Catalysts

Author:

Barata Beatriz12ORCID,Legens Christèle1ORCID,Devers Elodie1ORCID,Delpoux Olivier1ORCID,Barthe Laurent2,Roudenko Olga2,Briois Valérie2ORCID

Affiliation:

1. IFP Energies nouvelles Rond-point de l'échangeur de Solaize BP 3 69360 Solaize France

2. SOLEIL Synchrotron L'Orme des Merisiers Départementale 128 91190 Saint-Aubin France

Abstract

AbstractThis paper aims to describe and validate two cells designed to monitor, by in situ quick‐EXAFS, the transformation of Mo based oxidic species occurring during maturation and drying preparation steps of a single hydrodesulfurization catalyst. These transformations occur firstly upon impregnation/maturation, due to the contact of the acidic impregnation solution with the basic alumina support, and furthermore upon drying. The Mo K edge in situ quick‐EXAFS monitoring of these two elementary preparation steps is hereby reported for the first time, providing quantitative results of the Mo‐speciation. Ex situ Raman spectroscopy is used effectively as a complement. It considers an impregnation solution with a Mo concentration of 0.75 M and molar ratios of P/Mo 0.56 and Co/Mo 0.4. A two‐step drying mechanism is proposed to explain the evolution of the Mo‐speciation during in situ drying where Strandberg's, Anderson's and Dawson's HPAs are transformed into lacunary Keggin's HPA, octa‐ and monomolybdates.

Publisher

Wiley

Subject

Inorganic Chemistry,Organic Chemistry,Physical and Theoretical Chemistry,Catalysis

Reference27 articles.

1. U. S. Energy Information Administration “International Energy Outlook” can be found underhttps://www.eia.gov/outlooks/ieo/ 2021 (accessed Oct. 2022).

2. U. N. Environment Program “The global sulphur progress tracker” can be found underhttps://www.unenvironment.org/resources/toolkits-manuals-and-guides/global-sulphur-progress-tracker 2020(accessed Sep. 2022).

3. Atomic-Scale Structure of Single-LayerMoS2Nanoclusters

4. Atomic-Scale Structure of Co–Mo–S Nanoclusters in Hydrotreating Catalysts

5. Hydrotreating Catalysis

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