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Catalyst stability assessment in a lab-scale liquid-solid (LS)² plug-flow reactor

(2019) CATALYSTS. 9(9).
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Abstract
A packed-bed plug-flow reactor, denoted as the lab-scale liquid-solid (LS)² reactor, has been developed for the assessment of heterogeneous catalyst deactivation in liquid-phase reactions. The possibility to measure intrinsic kinetics was first verified with the model transesterification of ethyl acetate with methanol, catalyzed by the stable commercial resin Lewatit K2629, for which a turnover frequency (TOF) of 6.2 ± 0.4 × 10−3 s−1 was obtained. The absence of temperature and concentration gradients was verified with correlations and experimental tests. The potential for assessing the deactivation of a catalyst was demonstrated by a second intrinsic kinetics evaluation where a methylaminopropyl (MAP)-functionalized mesoporous silica catalyst was used for the aldol reaction of acetone with 4-nitrobenzaldehyde in different solvents. The cooperative MAP catalyst deactivated as a function of time on stream when using hexane as solvent. Yet, the monofunctional MAP catalyst exhibited stable activity for at least 4 h on stream, which resulted in a TOF of 1.2 ± 0.1 × 10−3 s−1. It did, however, deactivate with dry acetone or DMSO as solvent due to the formation of site-blocking species. This deactivation was mitigated by co-feeding 2 wt % of water to DMSO, resulting in stable catalyst activity.
Keywords
Physical and Theoretical Chemistry, Catalysis, continuous-flow reactor, catalyst deactivation, aldol reaction, transesterification, ION-EXCHANGE-RESINS, ONE-POT SYNTHESIS, ALDOL-CONDENSATION, REUSABLE CATALYST, ETHYL-ACETATE, ACID, TRANSESTERIFICATION, DEACTIVATION, EFFICIENT, METHANOL

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Citation

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MLA
De Vylder, Anton, et al. “Catalyst Stability Assessment in a Lab-Scale Liquid-Solid (LS)2 Plug-Flow Reactor.” CATALYSTS, vol. 9, no. 9, 2019.
APA
De Vylder, A., Lauwaert, J., Van Auwenis, S., De Clercq, J., & Thybaut, J. (2019). Catalyst stability assessment in a lab-scale liquid-solid (LS)2 plug-flow reactor. CATALYSTS, 9(9).
Chicago author-date
De Vylder, Anton, Jeroen Lauwaert, Stijn Van Auwenis, Jeriffa De Clercq, and Joris Thybaut. 2019. “Catalyst Stability Assessment in a Lab-Scale Liquid-Solid (LS)2 Plug-Flow Reactor.” CATALYSTS 9 (9).
Chicago author-date (all authors)
De Vylder, Anton, Jeroen Lauwaert, Stijn Van Auwenis, Jeriffa De Clercq, and Joris Thybaut. 2019. “Catalyst Stability Assessment in a Lab-Scale Liquid-Solid (LS)2 Plug-Flow Reactor.” CATALYSTS 9 (9).
Vancouver
1.
De Vylder A, Lauwaert J, Van Auwenis S, De Clercq J, Thybaut J. Catalyst stability assessment in a lab-scale liquid-solid (LS)2 plug-flow reactor. CATALYSTS. 2019;9(9).
IEEE
[1]
A. De Vylder, J. Lauwaert, S. Van Auwenis, J. De Clercq, and J. Thybaut, “Catalyst stability assessment in a lab-scale liquid-solid (LS)2 plug-flow reactor,” CATALYSTS, vol. 9, no. 9, 2019.
@article{8628008,
  abstract     = {A packed-bed plug-flow reactor, denoted as the lab-scale liquid-solid (LS)² reactor, has been developed for the assessment of heterogeneous catalyst deactivation in liquid-phase reactions. The possibility to measure intrinsic kinetics was first verified with the model transesterification of ethyl acetate with methanol, catalyzed by the stable commercial resin Lewatit K2629, for which a turnover frequency (TOF) of 6.2 ± 0.4 × 10−3 s−1 was obtained. The absence of temperature and concentration gradients was verified with correlations and experimental tests. The potential for assessing the deactivation of a catalyst was demonstrated by a second intrinsic kinetics evaluation where a methylaminopropyl (MAP)-functionalized mesoporous silica catalyst was used for the aldol reaction of acetone with 4-nitrobenzaldehyde in different solvents. The cooperative MAP catalyst deactivated as a function of time on stream when using hexane as solvent. Yet, the monofunctional MAP catalyst exhibited stable activity for at least 4 h on stream, which resulted in a TOF of 1.2 ± 0.1 × 10−3 s−1. It did, however, deactivate with dry acetone or DMSO as solvent due to the formation of site-blocking species. This deactivation was mitigated by co-feeding 2 wt % of water to DMSO, resulting in stable catalyst activity.},
  articleno    = {755},
  author       = {De Vylder, Anton and Lauwaert, Jeroen and Van Auwenis, Stijn and De Clercq, Jeriffa and Thybaut, Joris},
  issn         = {2073-4344},
  journal      = {CATALYSTS},
  keywords     = {Physical and Theoretical Chemistry,Catalysis,continuous-flow reactor,catalyst deactivation,aldol reaction,transesterification,ION-EXCHANGE-RESINS,ONE-POT SYNTHESIS,ALDOL-CONDENSATION,REUSABLE CATALYST,ETHYL-ACETATE,ACID,TRANSESTERIFICATION,DEACTIVATION,EFFICIENT,METHANOL},
  language     = {eng},
  number       = {9},
  pages        = {17},
  title        = {Catalyst stability assessment in a lab-scale liquid-solid (LS)² plug-flow reactor},
  url          = {http://dx.doi.org/10.3390/catal9090755},
  volume       = {9},
  year         = {2019},
}

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