Sustainable formation of tricarballylic acid from citric acid over highly stable Pd/Nb2O5·nH2O catalysts

[Display omitted] •Nb2O5·nH2O proved to be a stable and efficient catalyst for the dehydration of citric acid at mild reaction temperatures.•Investigation of the interaction of citric acid with the Nb2O5·nH2O surface by 13C MAS NMR.•Synthesis of bifunctional Pd/Nb2O5·nH2O via a low-temperature reduc...

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Veröffentlicht in:Journal of catalysis Jg. 408; S. 88 - 97
Hauptverfasser: Stuyck, Wouter, Bugaev, Aram L., Nelis, Tom, de Oliveira-Silva, Rodrigo, Smolders, Simon, Usoltsev, Oleg A., Arenas Esteban, Daniel, Bals, Sara, Sakellariou, Dimitrios, De Vos, Dirk
Format: Journal Article
Sprache:Englisch
Veröffentlicht: Elsevier Inc 01.04.2022
Schlagworte:
acidity
Bifunctional catalysts
Biomass
catalysts
catalytic activity
citric acid
Dehydration
Heterogeneous catalysis
Hydrogenation
Niobium oxides
Palladium
plasticizers
temperature
zeolites
Bifunctional catalysts
ppb
ATR-FTIR
XANES
Palladium
ATBC
Biomass
XAS
Dehydration
Hydrogenation
Heterogeneous catalysis
BTHC
WI
PC
DEHP
Niobium oxides
ICP
MSA
PVC
PTA
GVL
MAS NMR
ISSN:0021-9517
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Zusammenfassung:[Display omitted] •Nb2O5·nH2O proved to be a stable and efficient catalyst for the dehydration of citric acid at mild reaction temperatures.•Investigation of the interaction of citric acid with the Nb2O5·nH2O surface by 13C MAS NMR.•Synthesis of bifunctional Pd/Nb2O5·nH2O via a low-temperature reduction method to preserve the acid properties of the support.•Yields of tricarballylic acid exceeding 90% over multiple runs. Recently, a reaction sequence was developed for the production of tricarballylic acid, an interesting plasticiser precursor, from citric acid by using a H-Beta zeolite and Pd/C catalyst. Although yields of 85% of tricarballylic acid were obtained, citric acid elicited Al leaching from the zeolite framework, resulting in loss of activity. In this work, Nb2O5·nH2O was found to be a stable and performant catalyst for this reaction, and a strong involvement of the hydroxyl group of citric acid with the Nb2O5·nH2O surface was observed by 13C MAS NMR. Next, Pd/Nb2O5·nH2O catalysts were synthesized via a low temperature reduction method to preserve the acidity of the Nb2O5·nH2O support; the nature of the Pd phase was examined by XAS. In presence of a 0.6 wt% Pd/Nb2O5·nH2O catalyst, yields over 90% of tricarballylic acid were obtained over multiple runs. Finally, this catalyst was also suitable for the dehydration-hydrogenation of other monohydroxy carboxylic acids.
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ISSN:0021-9517
DOI:10.1016/j.jcat.2022.02.013