The hydrogenation of 1,3-pentadiene over an alumina-supported palladium catalyst: an FTIR study

Lundie, David T.; Lear, Timothy; Sutherland, Iain W.; Parker, Stewart F.; Lennon, David

doi:10.1039/b413178a

Cited by 12 publications

(11 citation statements)

References 29 publications

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“…Figure 1 shows the FTIR spectra of the AMPS–TFEMA–AMA membranes before and after crosslinking. An absorption peak at 3080 cm −1 , which was attributed to the CH stretching of the alkene group,22 was observed before the crosslinking (precursor), whereas no absorption peak was observed after the crosslinking (PEM). The first‐step reaction produced a linear‐chain polymer that still had an allyl group.…”

Section: Resultsmentioning

confidence: 99%

Preparation of a crosslinked polyelectrolyte membrane for fuel cells with an allyl methacrylate based two‐step reaction

Kishi

Umeda

2009

J of Applied Polymer Sci

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In this study, a proton-exchange membrane for fuel cells was prepared via a two-step reaction with an allyl methacrylate (AMA) as an asymmetric crosslinking agent. First, a linear-chain polymer was synthesized, consisting of hydrophilic 2-acrylamido-2-methylpropanesulfonic acid (AMPS), hydrophobic 2,2,2-trifluoroethyl methacrylate (TFEMA), and AMA. Subsequently, we crosslinked the linear-chain polymer by reacting the remaining allyl group during dry heating. The proton conductivity of the prepared membrane was 7 Â 10 À2 S/cm at room temperature. The membrane was characterized by Fourier transform infrared spectroscopy, differential scanning calorimetry, and atomic force microscopy. The polymer electrolyte membrane fuel cell (PEMFC) performance was evaluated for a membrane electrode assembly composed of the crosslinked AMPS-TFEMA-AMA/ fluoroalkyl graft polymer (FGP) membrane. As a result of a power-generation test, a maximum power density of 174 mW/cm 2 at a current density of 400 mA/cm 2 was observed for a PEMFC single cell. Consequently, it was confirmed that the AMPS-TFEMA-AMA/FGP membrane for PEMFC could easily be prepared via a two-step reaction at a low cost and that PEMFC exhibited a cell performance and that of cells with the Nafion membrane.

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Section: Resultsmentioning

confidence: 99%

Preparation of a crosslinked polyelectrolyte membrane for fuel cells with an allyl methacrylate based two‐step reaction

Kishi

Umeda

2009

J of Applied Polymer Sci

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“…A methodology used previously was adopted. 30,31 Briefly, the apparatus consisted of a modified heated gas cell (Graseby-Specac 5660) housed within a Nicolet-Avatar 360 FTIR spectrometer. 30,31 The IR cell was connected to the spectrometer's internal gas purge facility via rubber bellows, thereby ensuring that there were minimal complications to the resultant IR spectra as a result of contributions from atmospheric water or carbon dioxide signals.…”

Section: Methodsmentioning

confidence: 99%

Hydrogenation of Benzonitrile over Supported Pd Catalysts: Kinetic and Mechanistic Insight

McAllister

Boulho

Gilpin

et al. 2019

Org. Process Res. Dev.

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The liquid phase hydrogenation of benzonitrile over a 5 wt % Pd/C catalyst using a stirred autoclave is investigated. The reaction conforms to a consecutive reaction sequence: first benzonitrile is hydrogenated to produce benzylamine, which subsequently undergoes a hydrogenolysis step to form toluene. Benzonitrile hydrogenation obeys first-order kinetics with an activation energy of 27.6 kJ mol–1. In contrast, the benzylamine hydrogenolysis stage obeys zero-order kinetics and exhibits an activation energy of 80.1 kJ mol–1. A 1 wt % Pd/Al2O3 catalyst is additionally examined, which is also seen to support hydrogenolysis activity alongside the hydrogenation pathway. Gas phase transmission infrared spectroscopic measurements of the hydrogenation of benzonitrile and benzylamine over the 1 wt % Pd/Al2O3 catalyst utilizing hydrogen and deuterium are undertaken, which enable reaction schemes incorporating adsorption geometries of intermediate adsorption complexes to be proposed.

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“…The hydrogenation of unsaturated species is a process that is conveniently followed by this method and was used to study the hydrogenation of C5 dienes [6,7]. The method is critically dependent on reliable identification and assignment of the modes of each of the species that may be present.…”

Section: Introductionmentioning

confidence: 99%

Structural and spectroscopic characterisation of C4 oxygenates relevant to structure/activity relationships of the hydrogenation of α,β-unsaturated carbonyls

Parker

Silverwood

Hamilton

et al. 2016

Spectrochimica Acta Part A: Molecular and Biomolecular Spectros

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Supported palladium catalysts are widely used in selective hydrogenation reactions, thus it is desirable to correlate product yields with catalyst performance, so as to optimize catalyst productivity. One method to achieve this goal is to use gas phase infrared spectroscopy to follow the evolution of the gas phase composition as a catalytic reaction progresses and hence determine the kinetics of the reaction. The method is critically dependent on reliable identification and assignment of the modes of each of the species that may be present. We plan to use the same method to investigate how the morphology of Pd crystallites can influence selectivity branching in gas phase hydrogenation reactions of α,β-unsaturated carbonyl compounds, specifically by following the hydrogenation of 3-butyne-2-one to 3-butene-2-one to 2-butanone and finally to 2-butanol. In the present work, we have investigated the conformational isomerism and calculated the vibrational spectra of the C4 oxygenates using density functional theory. The calculations are validated by comparison to the inelastic neutron scattering and infrared spectra of the compounds. KeywordsInelastic neutron scattering spectroscopy; Infrared spectroscopy; Density functional theory; Conformational isomerism Highlights• The conformational isomerism in 3-butyne-2-one, 3-butene-2-one, 2-butanone and 2-butanol oxygenates has been investigated.• Complete vibrational assignments for 3-butyne-2-one, 3-butene-2-one, 2-butanone and 2-butanol are obtained from density functional theory.• The assignments have been tested by comparison to inelastic neutron scattering spectra. Graphical abstract3

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The hydrogenation of 1,3-pentadiene over an alumina-supported palladium catalyst: an FTIR study

Cited by 12 publications

References 29 publications

Preparation of a crosslinked polyelectrolyte membrane for fuel cells with an allyl methacrylate based two‐step reaction

Preparation of a crosslinked polyelectrolyte membrane for fuel cells with an allyl methacrylate based two‐step reaction

Hydrogenation of Benzonitrile over Supported Pd Catalysts: Kinetic and Mechanistic Insight

Structural and spectroscopic characterisation of C4 oxygenates relevant to structure/activity relationships of the hydrogenation of α,β-unsaturated carbonyls

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