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Iron-Substituted Cubic Silsesquioxane Pillared Clays: Synthesis, Characterization and Acid Catalytic Activity

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Iron-Substituted Cubic Silsesquioxane Pillared Clays: Synthesis, Characterization and Acid Catalytic Activity View metadata, citation and similar papers at core.ac.uk brought to you by CORE provided by University of Groningen University of Groningen Iron-substituted cubic silsesquioxane pillared clays Potsi, Georgia; Ladavos, Athanasios K.; Petrakis, Dimitrios; Douvalis, Alexios P.; Sanakis, Yiannis; Katsiotis, Marios S.; Papavassiliou, Georgios; Alhassan, Saeed; Gournis, Dimitrios; Rudolf, Petra Published in: Journal of Colloid and Interface Science DOI: 10.1016/j.jcis.2017.09.003 IMPORTANT NOTE: You are advised to consult the publisher's version (publisher's PDF) if you wish to cite from it. Please check the document version below. Document Version Publisher's PDF, also known as Version of record Publication date: 2018 Link to publication in University of Groningen/UMCG research database Citation for published version (APA): Potsi, G., Ladavos, A. K., Petrakis, D., Douvalis, A. P., Sanakis, Y., Katsiotis, M. S., ... Rudolf, P. (2018). Iron-substituted cubic silsesquioxane pillared clays: Synthesis, characterization and acid catalytic activity. Journal of Colloid and Interface Science, 510, 395-406. https://doi.org/10.1016/j.jcis.2017.09.003 Copyright Other than for strictly personal use, it is not permitted to download or to forward/distribute the text or part of it without the consent of the author(s) and/or copyright holder(s), unless the work is under an open content license (like Creative Commons). Take-down policy If you believe that this document breaches copyright please contact us providing details, and we will remove access to the work immediately and investigate your claim. Downloaded from the University of Groningen/UMCG research database (Pure): http://www.rug.nl/research/portal. For technical reasons the number of authors shown on this cover page is limited to 10 maximum. Download date: 12-11-2019 Journal of Colloid and Interface Science 510 (2018) 395–406 Contents lists available at ScienceDirect Journal of Colloid and Interface Science journal homepage: www.elsevier.com/locate/jcis Regular Article Iron-substituted cubic silsesquioxane pillared clays: Synthesis, characterization and acid catalytic activity Georgia Potsi a,b, Athanasios K. Ladavos c, Dimitrios Petrakis d, Alexios P. Douvalis e, Yiannis Sanakis f, ⇑ ⇑ Marios S. Katsiotis g, Georgios Papavassiliou f, Saeed Alhassan g, Dimitrios Gournis a, , Petra Rudolf b, a Department of Materials Science & Engineering, University of Ioannina, 45110 Ioannina, Greece b Zernike Institute for Advanced Materials, University of Groningen, Nijenborgh 4, 9747 AG Groningen, The Netherlands c School of Natural Resources and Enterprise Management, University of Patras, Agrinio 30100, Greece d Department of Chemistry, University of Ioannina, 45110 Ioannina, Greece e Physics Department, University of Ioannina, 45110 Ioannina, Greece f Institute of Nanoscience and Nanotechnology, NCSR ‘‘DEMOKRITOS”, 15310 Ag. Paraskevi-Attikis, Athens, Greece g Department of Chemical Engineering, The Petroleum Institute, PO Box 2533, Abu Dhabi, United Arab Emirates graphical abstract article info abstract Article history: Novel pillared structures were developed from the intercalation of iron-substituted cubic silsesquioxanes Received 17 May 2017 in a sodium and an acid-activated montmorillonite nanoclay and evaluated as acid catalysts. Octameric Revised 1 September 2017 cubic oligosiloxanes were formed upon controlled hydrolytic polycondensation of the corresponding Accepted 1 September 2017 monomer (a diamino-alkoxysilane) and reacted with iron cations to form complexes that were interca- Available online 6 September 2017 lated within the layered nanoclay matrices. Upon calcination iron oxide nanoparticles are formed which are located on the silica cubes (pillars) and on the surfaces of the clay platelets. Acid activation of the nan- Keywords: oclay was performed in order to increase the number of acid active sites in the pristine clay and thus Pillared clays increase its catalytic activity. A plethora of analytical techniques including X-ray diffraction, thermal Montmorillonite Polyhedral silsesquioxanes analyses, Fourier transform infrared, electron paramagnetic resonance, Raman, Mössbauer and X-ray Acid activation photoelectron spectroscopies and porosimetry measurements were used in order to follow the synthesis Abbreviations: POSS, polyhedral oligosilsesquioxanes; Na-T, natural Texas montmorillonite STx-1; HT, acid-activated STx-1; EDAPTMOS, 3-(2-aminoethylamino) propyltrimethoxysilane. ⇑ Corresponding authors. E-mail addresses: [email protected] (G. Potsi), [email protected] (A.K. Ladavos), [email protected] (D. Petrakis), [email protected] (A.P. Douvalis), i.sanakis@inn. demokritos.gr (Y. Sanakis), [email protected] (M.S. Katsiotis), [email protected] (G. Papavassiliou), [email protected] (S. Alhassan), [email protected] (D. Gournis), [email protected] (P. Rudolf). https://doi.org/10.1016/j.jcis.2017.09.003 0021-9797/Ó 2017 Elsevier Inc. All rights reserved. 396 G. Potsi et al. / Journal of Colloid and Interface Science 510 (2018) 395–406 Catalysis steps and to fully characterize the final catalysts. The resulting pillared clays exhibit a high specific area Isopropanol dehydration and show significant acid catalytic activity that was verified using the catalytic dehydration of iso- propanol as a probe reaction. Ó 2017 Elsevier Inc. All rights reserved. 1. Introduction The first attempt to intercalate metal POSS in pillared structures was performed by Khattou et al. [37,38] who intercalated a Cu2+- The field of engineering nanomaterials has a continuing need of octa(diaminoalkyl) siloxane complex into a-zirconium phosphate well-defined building blocks that imbue functionality and allow for and examined the pillaring materials obtained after calcination nanoparticle-by-nanoparticle assembly of a wide variety of materi- by electron paramagnetic resonance (EPR) spectroscopy. In this als with precise control over the nanoarchitecture [1,2]. case the metal ions act as probe for the determination of the evo- Silsesquioxanes possess a pronounced aptitude to form three lution of local symmetry and structure during the pillaring process dimensional cage-like highly symmetric frameworks known as when using an element specific technique. More recently Carniato polyhedral oligosilsesquioxanes (POSS) with cubic, hexagonal, et al.[39] demonstrated the intercalation of a bifunctional proto- octagonal, decagonal, dodecagonal or even open cage-like mor- nated titanium-containing aminopropyl isobutyl POSS, within the phology [3–5]. Cubic silsesquioxanes (cubes), synthesized from interlayer space of a synthetic sodium saponite and its use as filler the hydrolytic condensation of the corresponding trifunctional in a polystyrene-based nanocomposite designed to enhance the organo-silicon monomers, is the most common polyhedral struc- thermooxidative properties. The same group [40] also intercalated ture and provide the opportunity to design and ‘‘construct” Ti-containing aminopropylisobutyl polyhedral oligomeric materials with extremely well-defined dimensions and behaviour silsesquioxane in synthetic saponite and investigated the catalytic [3–13] In this context, cubic silsesquioxanes of the type X8Si8O12 activity of this composite in cyclohexene oxidation. Other catalysts where X is A(CH3)3NH2, A(CH3)3NR2 and A(CH3)3NH(CH2)2NH2 based on clay-POSS hybrids include synthetic laponite clay first have been successfully employed as precursor reagents for pillar- modified by octaaminopropyl polyhedral oligomeric silsesquioxane ing inorganic layered solids such as clays[14–19], metal (IV) hydro- and then used to support a nickel alpha-diimine late-transition- gen phosphates [20–22], photonic titanoniobates [23], graphenes metal catalyst for ethylene polymerization [41]; laponite and and graphene oxide [3,24–26], graphene oxide nanoribbons [27], montmorillonite functionalized with (3-aminopropyl)triethoxysilane halloysite nanotubes [28] and perovskites [29]. Protonation of and use both as supports for the vanadyl(IV) acetylacetonate the amino groups generates oligomeric cationic species with catalysis [42] and POSS intercalated bentonites[30] for metal up expendable and bulky organic groups that can easily be inserted take of copper, cadmium and lead. into the interlayer space of a phyllomorphous clay in amounts In this work we report the intercalation of Fe3+-substituted exceeding the cation exchange capacity of the mineral and can suc- cubic silsesquioxanes in a sodium and an acid-activated montmo- cessively be removed by thermal treatment, resulting in silica pil- rillonite to form novel catalytic pillared structures. Iron was chosen lared structures [15,14]. This excess being in the form of physically as metal catalyst because of its low toxicity and high abundance adsorbed ion pairs influences the free distance between the layers that make it attractive for potential industrial applications [43].A and the surface area as well as the porosity of the silica-pillared plethora of analytical techniques including X-ray diffraction composites. (XRD), thermal analyses (DTA/TGA), Fourier transform infrared On the other hand, these various mono- or bi-functional amino- (FTIR), electron paramagnetic resonance (EPR), Raman, Mössbauer silanes possess the ability to bind metal ions, Mn+ (e.g. Cu2+,Ni2+, and X-ray photoelectron (XPS) spectroscopies and porosimetry 2+ 3+ 3+ n+ Co ,Fe ,Al ), yielding metal complexes, Mx [X8Si8O12]y, and measurements were used in order to follow the synthesis steps thus enabling the design
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