03125nas a2200241 4500008004100000022001400041245009700055210006900152260007300221300001200294490000800306520222500314653003402539653002902573653003902602653001402641653002602655100001302681700002202694700001802716700002002734856012902754 2007 eng d a1387-181100aDirect hydrothermal synthesis of mesoporous Sn-SBA-15 materials under weak acidic conditions0 aDirect hydrothermal synthesis of mesoporous SnSBA15 materials un aPO BOX 211, 1000 AE AMSTERDAM, NETHERLANDSbELSEVIER SCIENCE BVcMAR a210-2260 v1003 a

A direct synthetic route for the preparation of Sn-SBA-15 materials with n(Si)/n(Sn), ratios ranging from 100 to 10 under milder acidic conditions than normally employed for the preparation of Si-SBA-15 is reported. The changes in the pH conditions of the gel were made through an adjustment of the molar ratio of n(H2O) to n(HCl) (< 1 pH < 2) during preparation. The samples prepared under three different acidic conditions have been characterized by various techniques. An expansion of the lattice (powder XRD) and an increase in mesopore area (low temperature N-2 adsorption) indicate that the hexagonal structure of the SBA- 15 is maintained with no loss of long range ordering. The UV-vis reflectance spectra of Sn-SBA-15 samples show the presence of Sn4+ ions both in tetrahedral and octahedral environment. Si-29 MAS NMR spectra of samples prepared under an intermediate acid condition show the presence Of Q(3) and Q(4) species. Their ratio increases with a decrease in tin content. The presence of Si in (2Si, 2Sn) i.e., Q(2) environment may point to incorporation of considerable Sn4+ ions in tetrahedral positions. Sn-Mossbauer spectroscopic studies reveal that Sn2+ species form upon reductive treatments and can probably be stabilized in the pore wall upon reoxidation. This to some extent is an indication of the formation and stabilization of Si-O-Sn-O-Si linkages in Sn-SBA-15. A progressive increase in the pH of the medium (increasing the n(H2O) to n(HCl), ratio) results in the location of Sn4+ ions, (a) at the surface of the mesopores (surface of the corona region) as a thin film of SnO2 or small aggregates (loss in mesopore area) depending on the concentration of Sn; (b) at the walls of the mesopore structure, substituting Si4+ ions (some lattice expansion and tetrahedral Sn4+ ions); and/or (c) as a part of the corona region, neutralizing the resulting Si-OH groups (a loss of micropore area and octahedral Sn4+ ions). The studies reveal that the method of preparation, n(H2O)/n(HCl) ratio and the n(Si)/n(Sn) ratio (concentration of SnCl4) of the gel significantly influence the type of tin species in the resulting Sn-SBA-15 samples. (c) 2006 Elsevier Inc. All rights reserved.

10adirect synthesis of Sn-SBA-1510aSi-29 and Sn-119 MAS-NMR10aSn-mossbauer spectroscopic studies10aSn-SBA-1510atin-mesoporous silica1 aShah, P.1 aRamaswamy, A., V.1 aLazar, Karoly1 aRamaswamy, Veda uhttps://library.ncl.res.in/content/direct-hydrothermal-synthesis-mesoporous-sn-sba-15-materials-under-weak-acidic-conditions02412nas a2200217 4500008004100000022001400041245009800055210006900153260007300222300001200295490000800307520162800315653001801943653002201961653001401983653001201997653002202009100001802031700002002049856012502069 2008 eng d a1387-181100aThermal stability of mesoporous SBA-15 and Sn-SBA-15 molecular sieves: an in situ HTXRD study0 aThermal stability of mesoporous SBA15 and SnSBA15 molecular siev aPO BOX 211, 1000 AE AMSTERDAM, NETHERLANDSbELSEVIER SCIENCE BVcSEP a270-2800 v1143 a

Highly ordered SBA-15 and Sn-SBA-15 mesoporous molecular sieves with Si/Sn = 80, 60, 40 and 10 have been prepared through direct synthesis route under milder acidic conditions, which were used for the in situ high temperature X-ray diffraction (HTXRD) studies in the temperature range 298-1573 K for the first time in the literature. SBA-15 is found to be thermally stable up to 1473 K and appearance of alpha-cristobalite was observed at 1573 K also supported by the thermogravimetric (TG) data. A strong negative thermal expansion was observed on heating from 298 to 1573 K (alpha(a) = -4.3 x 10(-6) K-1). Sit containing samples (Si/Sn = 80 and 60) showed a positive thermal expansion (6.75 x 10(-6) K-1 and 9.04 x 10(-6) K-1, respectively). On the other hand, the samples with Si/Sn = 40 and 10 showed a strong negative thermal expansion (-4.12 x 10(-6) K-1 and -7.56 x 10(-6) K-1) similar to SBA-15. The linear thermal expansion coefficient varied in the order: Si/Sn = 60 > 80 > 40 > 0 > 10. Sn4+ ions exhibit both tetrahedral and octahedral coordination depending upon the location of these ions either on the walls of the silica (Si/Sn = 80 and 60) or in the corona region of the structure (Si/Sn = 40 and 10), respectively. The thermal decomposition of the samples (TG data) is correlated to the thermal expansion behavior (HTXRD data). The decomposition behavior of template ions located within the pores is strongly influenced by the presence of Sn in the framework and a `soft' interaction probably exists between the template ions and the Sn sites. (C) 2008 Elsevier Inc. All rights reserved.

10aHTXRD studies10aphase transitions10aSn-SBA-1510aTG data10aThermal expansion1 aShah, Pallavi1 aRamaswamy, Veda uhttps://library.ncl.res.in/content/thermal-stability-mesoporous-sba-15-and-sn-sba-15-molecular-sieves-situ-htxrd-study-002605nas a2200265 4500008004100000022001400041245011500055210006900170260007300239300001200312490000800324520164200332653003001974653001402004653003502018653003602053653001402089100001902103700001702122700001602139700001302155700002402168700001802192856012902210 2009 eng d a1387-181100aIncorporation of tin in different types of pores in SBA-15: synthesis, characterization and catalytic activity0 aIncorporation of tin in different types of pores in SBA15 synthe aPO BOX 211, 1000 AE AMSTERDAM, NETHERLANDSbELSEVIER SCIENCE BVcDEC a234-2440 v1263 a

Mesoporous Sn-SBA-15 has been synthesized by three different methods Such as conventional hydrothermal route, using cocatalyst NH4F and in the presence of organosilane precursor. All the materials are thoroughly characterized by powder X-ray diffraction (XRD), SEM. TEM. N-2 sorption and surface area measurements, diffuse-reflectance UV-visible and FTIR spectroscopy. TG-DTA and elemental analysis through ICP. Nitrogen adsorption data, XRD patterns, and TEM observations Suggests that the textural properties are retained during the isomorphous substitution of silicon by tin. ICP chemical analysis indicates that tin can be substituted in the range of S-l/S-n = 69-162. UV-visible spectra of samples synthesized by the cocatalytic approach exhibit unique absorption band at 213 nm characteristics of tin atom substituted in the smaller pores (2-3 nm) located inside the walls of mesopores. Further, an additional band at 224 nm can be assigned to Sri atoms located in the distorted tetrahedral position along the primary mesopores. In contrary, only one absorption band centered at 224 nm is observed for all the samples synthesized by conventional hydrothermal as well as in the presence of organosilane precursor. F-19 NMR spectra confirmed (no signal) the absence of occluded F- ions in the samples made with NH4F. Observed high catalytic activity in Baeyer-Villiger oxidation and Meerwin-Pondorf-Verly reduction under the liquid-phase conditions suggest the incorporation of a portion of tin in the smaller pores for the Sn-SBA-15 materials synthesized through cocatalyst method. (C) 2009 Elsevier Inc. All rights reserved.

10aBaeyer-Villiger oxidation10acatalysis10aFunctionalization of mesopores10aMeerwin-Pondorf-Verly reduction10aSn-SBA-151 aSasidharan, M.1 aKiyozumi, Y.1 aMal, N., K.1 aPaul, M.1 aRajamohanan, P., R.1 aBhaumik, Asim uhttps://library.ncl.res.in/content/incorporation-tin-different-types-pores-sba-15-synthesis-characterization-and-catalytic-0