The effect of phosphate and glycol on the sulfidation mechanism of CoMo/Al2O3 hydrotreating catalysts: an in situ QEXAFS study

Nicosia, Daniele; Prins, R.

doi:10.1016/j.jcat.2005.01.018

Cited by 45 publications

(36 citation statements)

References 17 publications

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“…in the temperature range where the organic compound is still mainly present at the surface of the catalyst as suggested by C analysis. These data illustrate the complex behaviour of this kind of organic compound since Nicosia et al observed no promotion and a faster sulfidation in the case of TEG [25]. In order to discriminate if this slowing down process concerns Co or Mo or both elements, XAS studies were performed at both K-edges after in situ sulfidation at various temperatures.…”

Section: Resultsmentioning

confidence: 53%

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In Situ EXAFS Study of the Sulfidation of an Hydrotreating Catalyst Doped with a Non Chelating Organic Additive

Mazoyer

Geantet

Diehl

et al. 2005

Oil & Gas Science and Technology - Rev. IFP

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Résumé -Étude par absorption X in situ de la sulfuration d'un catalyseur d'hydrotraitement dopé par un composé organique non chélatant -Un catalyseur industriel de type CoMoP supporté sur alumine a été imprégné à sec par une solution aqueuse de diéthyleneglycolbutyléther (DEGbe) puis séché à 393 K pendant 12 h. Après activation sous H 2 /H 2 S, ce catalyseur se révèle plus actif que la référence non modifiée. Afin de comprendre l'effet de cet additif organique sur la cinétique de sulfuration, des analyses in situ par EXAFS au seuils K du cobalt et du molybdène ont été réalisées. Ces caractérisations ont été effectuées sur le catalyseur CoMoP + DEGbe séché à 393 K, sulfuré à température ambiante, puis à 373 et 473 K. La sulfuration du cobalt et surtout celle du molybdène sont inhibées par la présence du composé organique jusqu'à environ 473 K. Les résultats EXAFS obtenus dans le cadre de cette étude ont permis de mieux appréhender le rôle des composés organiques ajoutés aux catalyseurs d'hydrotraitement. Ces composés ralentissent la sulfuration du Mo et du Co présents sur le catalyseur. Abstract -In Situ EXAFS Study of the Sulfidation of an Hydrotreating Catalyst Doped with a Non Chelating Organic Additive -An industrial alumina-supported CoMoP catalyst was impregnated (incipient wetness method) with an aqueous solution of diethyleneglycolbutylether (DEGbe) and then dried at 393 K overnight. After sulfidation under H 2 /H 2 S, this catalyst has a higher activity than the non impregnated CoMoP. In order to check if the presence of such an organic additive in contact with the oxidic form of the active phase influences the kinetics of sulfidation of the cobalt and the molybdenum, EXAFS spectroscopy (K-Co or K- Synchrotron and Neutron Solutions to Oil Industry ProblemsUtilisation des grands instruments analytiques dans l'industrie pétrolière

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Section: Resultsmentioning

confidence: 53%

“…When using glycols, these sites could be blocked and only a weak metal-support interaction could prevail, leading to the highly active type II Co-Mo-S phase. Nicosia and Prins [24,25] studied catalysts prepared from MoO 3 H 3 PO 4 and CoCO 3 as reported in ref. [2].…”

Section: Introductionmentioning

confidence: 99%

In Situ EXAFS Study of the Sulfidation of an Hydrotreating Catalyst Doped with a Non Chelating Organic Additive

Mazoyer

Geantet

Diehl

et al. 2005

Oil & Gas Science and Technology - Rev. IFP

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“…However, no HDS catalyst containing both chelating agent and phosphorus has yet been commercialized 49) . On the other hand, investigation of the additional effect of triethylene glycol, which is not a chelating agent, and phosphorus to the CoMo HDS catalyst concluded that triethylene glycol did not show strong interaction between cobalt, and there was no such effect as seen with chelating agents 50), 51) , as previously suggested 30) 32),34) 36) .…”

Section: Trends In the Development Of Highly Active Hds Catalystsmentioning

confidence: 80%

超低硫黄軽油製造のための新規CoMo系水素化脱硫触媒の工業化

Fujikawa

2007

J. Jpn. Petrol. Inst.

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“…Recently, Prins et al, [28,29] investigated the additional effect of triethylene glycol, which is not a chelating agent, and phosphorus to the CoMo HDS catalyst. They concluded that triethylene glycol did not show strong interaction between cobalt, and there was no such an effect as chelating agents, which Yamada et al, [12][13][14] and Cattaneo et al, [16][17][18] suggested.…”

Section: Catalyst Designmentioning

confidence: 99%

Highly active CoMo HDS catalyst for the production of clean diesel fuels

Fujikawa

2006

Catal Surv Asia

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supported CoMo catalysts with a chelating agent and phosphorus for the hydrodesulfurization (HDS) of diesel fractions were prepared. The activity measurements with the prepared catalysts were carried out with straight-run light gas oil feedstocks in a pilot plant under industrial hydrotreating conditions. As a result, Cosmo Oil Co., Ltd. developed a new CoMoP/ HY-Al 2 O 3 catalyst, C-606A, which had three times higher HDS activity than the conventional CoMoP/Al 2 O 3 catalyst. Commercial operations to produce ultra-low sulfur diesel (ULSD) with C-606A have successfully demonstrated its high performance and high stability. This catalyst has an extremely high activity, which enables to achieve <10-ppm sulfur in products in diesel hydrotreater designed to produce 500-ppm sulfur diesel fuels. Mo K-edge EXAFS, TEM and FT-IR of adsorbed NO were performed to investigate the nature of the active sites on the developed catalysts. The results showed that the new catalyst has multiple layers of MoS 2 slabs and the edges of MoS 2 are mainly occupied by Co-Mo-S phases. XPS and FT-IR were used to investigate the sulfiding behavior of Co and Mo in the formation process of the active sites during sulfidation. The results showed that addition of carboxylic acid to the impregnation solution postponed the sulfidation of Co at low temperatures, thereby increasing formation of the Co-Mo-S phase.

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The effect of phosphate and glycol on the sulfidation mechanism of CoMo/Al2O3 hydrotreating catalysts: an in situ QEXAFS study

Cited by 45 publications

References 17 publications

In Situ EXAFS Study of the Sulfidation of an Hydrotreating Catalyst Doped with a Non Chelating Organic Additive

In Situ EXAFS Study of the Sulfidation of an Hydrotreating Catalyst Doped with a Non Chelating Organic Additive

超低硫黄軽油製造のための新規CoMo系水素化脱硫触媒の工業化

Highly active CoMo HDS catalyst for the production of clean diesel fuels

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