Development and sorption characterization of some model mesoporous and microporous silica adsorbents

Esparza, J.M.; Ojeda, María Luisa; Campero, A.; Aguirre, Gerardo; Felipe, Carlos; Asomoza, M.; Cordero, Salomón; Kornhauser, Isaac; Rojas, Fernando

doi:10.1016/j.molcata.2004.09.042

Cited by 50 publications

(26 citation statements)

References 44 publications

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“…Two new peaks at 1982 and 2083 cm -1 reveal the presence of a CO group in the catalyst, and the peak at 722 cm -1 depicts the ortho-metallation of the phenyl ring with Rh I . [44] The FTIR spectra of F after two catalytic cycles (Figure 4f) is similar to the fresh material F, which points to the fact that after reaction there is no change in the composition of the catalyst. …”

Section: Characterisation Of the Catalystmentioning

confidence: 61%

Highly Efficient Hydroformylation of 1‐Hexene over an ortho‐Metallated Rhodium(I) Complex Anchored on a 2D‐Hexagonal Mesoporous Material

et al. 2010

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The hydroformylation reaction is an important class of reaction as it enhances the carbon chain length of an olefin molecule. RhI complexes are conventionally used as the catalyst for this reaction although they possess severe drawbacks with respect to separation and recycling. A phenyl‐functionalised 2D‐hexagonal mesoporous silica material has been synthesised by a surfactant templating pathway. The phenyl group of this mesoporous material was functionalised through nitration, followed by its reduction to the amine derivative. The amine group was further subjected to Schiff‐base condensation, and the RhI complex was then heterogenised over its surface to yield the ortho‐metallated complex anchored on the mesoporous silica matrix. The materials have been characterised by using powder X‐ray diffraction, transmission electron microscopy and nitrogen adsorption/desorption studies. The RhI‐loaded mesoporous material acts as a very efficient catalyst for the hydroformylation reaction of 1‐hexene and exhibits high selectivity towards the formation of n‐heptanal at 343 K in the presence of H2/CO at 50 bar pressure.

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Section: Characterisation Of the Catalystmentioning

confidence: 61%

Highly Efficient Hydroformylation of 1‐Hexene over an ortho‐Metallated Rhodium(I) Complex Anchored on a 2D‐Hexagonal Mesoporous Material

et al. 2010

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“…The pore cavity sizes normally assigned to SBA-16 specimens are ca. 9-10 nm (Esparza et al 2005). Comparison between the experimental characteristic curve for the SBA-15 sample and the calculated characteristic curve for a cylindrical cavity of 7.3 nm diameter.…”

Section: Sba-15 Silicamentioning

confidence: 99%

On Scrutinizing the Classical Polanyi Adsorption Potential Theory for Vapour Uptake Occurring in the Mesopores of Curved Shapes

Ponce

Munguía

Esparza

et al. 2011

Adsorption Science & Technology

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ABSTRACT:One of the essential foundations of the classical Polanyi adsorption potential theory has been assessed with respect to the invariability with temperature of the so-called characteristic adsorption curves. This has been achieved both numerically and experimentally for nitrogen and numerically for argon adsorption onto spherical as well as onto cylindrical mesopore entities at 77.35 K and 87.29 K, respectively. The adsorption results in these spherical and cylindrical pores were obtained from an application of the Broekhoff-de Boer equation and compared to nitrogen experimental sorption data obtained from cylindrical SBA-15 and spherical SBA-16 pore systems. The characteristic curves obtained in both ways were consistent with each other.

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“…These effects are known as advanced [5] and delayed [6] filling (or condensation, or adsorption). These particular effects are pore-pore co-operative in nature, and thus the size of the effects is associated with the random inter-connectivity of pores of various different sizes within disordered solids, and, thence, studies of the more regular structures possessed by templated materials does not help to elucidate the actual extent of these problems in a given disordered material.…”

Section: Introductionmentioning

confidence: 99%

“…Attempts have been made to study pore-pore co-operative effects with gas sorption scanning curves but the data from these experiments are a composite signal from the whole sample, and thus difficult to interpret unambiguously for disordered solids, as opposed to more ordered templated solids [6]. In contrast, the novel integrated gas sorption and mercury porosimetry technique, which involves conducting a series of gas sorption and mercury porosimetry experiments on the same sample, can study pore-pore co-operative effects in particular sub-sets of pores within disordered samples by deconvolving-out the signal from 5 these pores.…”

Section: Introductionmentioning

confidence: 99%

Detection of the delayed condensation effect and determination of its impact on the accuracy of gas adsorption pore size distributions

Rigby

Hasan

Hitchcock

et al. 2017

Colloids and Surfaces A: Physicochemical and Engineering Aspect

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The version presented here may differ from the published version or from the version of record. If you wish to cite this item you are advised to consult the publisher's version. Please see the repository url above for details on accessing the published version and note that access may require a subscription.For more information, please contact eprints@nottingham.ac.uk 1 normally requiring assumptions about the correct model for data analysis. In this work we present a novel method to both expand the range, and obtain greater accuracy, for the information obtained from the main boundary adsorption isotherms by using a combination of data obtained for two adsorptives, namely nitrogen and argon, both before and after mercury porosimetry. The method makes use of the fact that nitrogen and argon apparently 'see' a different pore geometry following mercury entrapment, with argon, relatively, 'ignoring' new metal surfaces produced by mercury porosimetry. The new method permits the study of network and pore-pore co-operative effects during adsorption that substantially affect the accuracy of the characteristic parameters, such as modal pore size, obtained for disordered materials. These effects have been explicitly quantified, for a typical sol-gel silica catalyst support material as a case study. The technique allowed the large discrepancies between modal pore sizes obtained from standard gas adsorption and mercury thermoporometry methods to be attributed to the network-based delayed condensation effect, rather than spinodal adsorption. Once the network-based delayed condensation effect had been accounted for, the simple cylindrical pore model and macroscopic thermodynamic Kelvin-Cohan equation were then found sufficient to accurately describe adsorption in the material studied, rather than needing a more complex microscopic theory. Hence, for disordered mesoporous solids, a proper account of inter-pore interactions is more important than that of intra-pore adsorbate density distribution, to obtain accurate pore size distributions. Detection of the Delayed Condensation Effect and Determination of its

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Development and sorption characterization of some model mesoporous and microporous silica adsorbents

Cited by 50 publications

References 44 publications

Highly Efficient Hydroformylation of 1‐Hexene over an ortho‐Metallated Rhodium(I) Complex Anchored on a 2D‐Hexagonal Mesoporous Material

Highly Efficient Hydroformylation of 1‐Hexene over an ortho‐Metallated Rhodium(I) Complex Anchored on a 2D‐Hexagonal Mesoporous Material

On Scrutinizing the Classical Polanyi Adsorption Potential Theory for Vapour Uptake Occurring in the Mesopores of Curved Shapes

Detection of the delayed condensation effect and determination of its impact on the accuracy of gas adsorption pore size distributions

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