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Opis: Manganese plays an important role in redox catalysis using zeolites as inorganic support materials, but the formation of the preferred redox manganese species (framework or extraframework) is still not well understood. Herein, the influence of the amount of manganese together with conventional and microwave-assisted hydrothermal synthesis paths on the formation of manganese species within the zeolite silicalite-1 (S-1) with MFI structure was investigated. It was found out that both synthesis procedures led to the formation of framework and extraframework manganese species, but in different molar ratios. However, the conventional synthesis procedure with all Mn/Si molar ratios generates more framework Mn in comparison to the microwave procedure. Additionally, the diminution of the zeolite crystals to nanoscale from 100 to 200 nm was achieved via the conventional procedure for the first time. UV–vis, Raman, and X-ray absorption spectroscopic analyses revealed different local environments of manganese: Mn3+ incorporated into the silicalite-1 framework as “framework manganese” and Mn2+/3+ present as “extraframework manganese” (Mn2O3, Mn3O4). TEM reveals the presence of Mn3O4 nanorods. Both framework manganese and extraframework manganese exhibit good catalytic activity for styrene epoxidation. Catalytic results suggest that, in oxidation reactions of hydrocarbons, framework manganese is more active at lower Mn contents (Mn/Si < 0.015), whereas extraframework manganese is more active at higher loadings (Mn/Si > 0.015).
Ključne besede: MnS-1 Nanocrystals, Mn XANES, EXAFS, zeolites, microwave-assisted hydrothermal synthesis
Objavljeno v RUNG: 06.05.2019; Ogledov: 3384; Prenosov: 0
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Opis: A new metals-polymeric composite, Metx-EPS (I), was prepared to be used as catalyst in water or in two-phase aqueous conditions. The metals source was an exhausted catalytic converter that was grinded and treated with an acidic solution at room temperature. After filtration, the solution was concentrated, neutralized and added to a broth of Klebsiella oxytoca DSM 29614 to produce (I) where metals are embedded in a peculiar polysaccharide structure (EPS). The composite was easily recovered from the fermentation broth and purified. The process protocol was verified many times and was shown to be reproducible satisfactorily. The % recovery of metals, originally present in the converter, was good as determined by atomic absorption. The morphology and the chemical state of main metals in (I) were investigated by X-ray absorption spectroscopy methods (XANES and EXAFS). No metallic alloy seems to be evident. The catalytic activity and a possible synergic effect due to the presence of the different metals was valuated in the hydrogenation of some substrates, valuable precursors for theproduction of fine chemicals.
Ključne besede: Biogenerated polymetallic exopolysaccharide, biphasic catalysis, hydrogenation, metals-polymeric composite, new catalyst from metallic wastes, EXAFS, XANES
Objavljeno v RUNG: 06.05.2019; Ogledov: 3228; Prenosov: 0
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Opis: Properties of mixed-metal MOFs depend on the distribution of different metals within their frameworks. Determination of this distribution is often very challenging. Using an example of aluminum- and iron-containing MIL-100, we demonstrate that 27Al NMR spectroscopy, when combined with first-principles calculations and magnetic, X-band electron paramagnetic resonance, Fe K-edge extended X-ray absorption fine structure, and Mössbauer measurements, enables one to accurately determine the arrangement of Al and Fe within the metal trimers, which are the basic building units of MIL-100. In this particular material, the incorporation of Fe and Al on the framework metal sites is random. Crucial for deciphering the arrangement is detecting NMR signals, shifted because of the strong hyperfine interaction between the 27Al nuclei and the unpaired electronic spins of Fe3+ ions, assigning the shifted signals aided by first-principles calculations of hyperfine couplings, and quantitatively evaluating the NMR intensities and the measured effective magnetic moment.
Ključne besede: Fe EXAFS, XANES, MIL100, MOF, magnetizem
Objavljeno v RUNG: 26.03.2019; Ogledov: 3230; Prenosov: 0
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Ključne besede: samoevalvacijsko poročilo
Objavljeno v RUNG: 20.12.2018; Ogledov: 3655; Prenosov: 0
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Opis: The European Synchrotron and free-electron laser (FEL) User Organisation (ESUO) established in 2010 [1] today represents about 30.000 users. We aim at representing the users from all European countries. Each country is represented within ESUO by one up to four national delegate(s), depending on the size of the user community in the respective country. ESUO’s main objectives are (i) to promote an integrated approach throughout Europe for the use of European synchrotron and FEL facilities, (ii) to enable all European scientists to make use of the existing European synchrotron and FEL research infrastructures, solely based on scientific merit of their submitted proposals for beamtime requests, and this independently from the financial situation of the user (country), (iii) to facilitate open transnational access to European light sources through programmes of the European Union, (iv) to disseminate information about scientific opportunities and funding mechanisms for access to synchrotron and FEL facilities, and (v) to be a discussion and acting partner regarding the coordination of the synchrotron and FEL user activities within Europe. In the past few years, ESUO has contributed to several joint activities in the frame of successfully completed European FP7 projects such as ELISA (March 2009 - August 2011) and CALIPSO (June 2012 - May 2015). Some past ESUO activities concern, amongst others:  the user representation in e.g. the CALIPSO and BioStruct-X European projects by ESUO delegates;  the contribution to the CALIPSOplus project application;  the dissemination of ESUO activities by means of e.g. poster presentations and talks delivered at international conferences, specialized user meetings/workshops, and;  several initiatives which have been attended to promote transnational access activities [3] and to favor the continuation of transnational user access to national facilities in Europe within the new European Framework Program Horizon 2020 [4]. Today, chance is given to ESUO to keep constructively acting for the users in the frame of joint networking activities being part of the HORIZON 2020 project CALIPSOplus [5] (May 2017 – April 2021, Grant Agreement No 730872) coordinated by Helmholtz-Zentrum Dresden-Rossendorf (HZDR). In the framework of CALIPSOplus, ESUO is contributing to project networking activities which are, amongst others, shown in the present contribution. With the aim to further prepare the future science at European synchrotron and FEL user facilities, ESUO is contributing to the League of European Accelerator-based Photon Sources (LEAPS) initiative [6].
Ključne besede: European synchrotron user organisation, Transnational access, FEL, CALIPSO
Objavljeno v RUNG: 01.10.2018; Ogledov: 3433; Prenosov: 0
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