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Journal Cover Microporous and Mesoporous Materials
  [SJR: 1.243]   [H-I: 116]   [6 followers]  Follow
    
   Hybrid Journal Hybrid journal (It can contain Open Access articles)
   ISSN (Print) 1387-1811
   Published by Elsevier Homepage  [3039 journals]
  • Preparation and characterization of super-microporous alumina with
           crystalline structure
    • Abstract: Publication date: 1 May 2017
      Source:Microporous and Mesoporous Materials, Volume 243
      Author(s): Yongfeng Li, Jiaojiao Su, Ruifeng Li
      Super-microporous alumina (pore size between 1 and 2 nm) with polycrystalline walls and high surface area (more than 650 m2/g) was synthesized successfully via an evaporation induced self-assembly (EISA) pathway using readily available and inexpensive nonionic surfactant fatty alcohol polyoxyethylene ether (AEO-7) as the template. N2 adsorption-desorption results showed that the obtained materials are super-microporous when removing the template at 400 °C, then if the calcination temperature increase from 600 °C to 1000 °C, a breakdown of the walls separating adjacent pores allows the transformation to mesopores (pore size > 2 nm). FTIR pyridine adsorption and NH3-TPD measurement suggested the presence of strong Lewis acid sites. Transmission electron microscopy (TEM) measurements indicated that the alumina possesses the disordered “wormhole-like” super-microporous structure with polycrystalline walls. Loaded with copper, the catalyst exhibited outstanding activity in the selective catalytic reduction of NO with methane and could achieve a NOx conversion 100% when the reaction temperature is over 600 °C.
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      PubDate: 2017-02-14T17:55:07Z
       
  • Novel Ce-incorporated zeolite modified-carbon paste electrode for
           simultaneous trace electroanalysis of lead and cadmium
    • Abstract: Publication date: 1 May 2017
      Source:Microporous and Mesoporous Materials, Volume 243
      Author(s): A. Kawde, A. Ismail, A.R. Al-Betar, O. Muraza
      Cerium incorporated zeolite-modified carbon paste electrode (Ce-ZCPME) was studied for the anodic stripping voltammetric detection of lead and cadmium ions. The modified electrode which was fabricated in-house by a prior hydrothermal synthesis of Ce-impregnated zeolite displayed satisfactory results compared to other reported electrodes. Deposition of the metal was achieved at a potential of −1.2 V (vs. Ag/AgCl) for 120 s followed by a square wave stripping scan from −1.6–0.0 V. Various experimental conditions which include nature of supporting electrolyte, pH, amplitude, frequency, deposition potential and deposition time were optimized prior to the analyses. The fabricated electrode revealed a linear behavior over the metal ion concentrations with a LOD (S/N = 3) of 0.07 ppb and 0.46 ppb for lead and cadmium detection, as well as a good reproducibility (RSD 2.23%) respectively. The fabricated electrode has the potential to be used in the analysis of environmental samples due to its lack of toxicity, ease of fabrication and relative inexpensiveness.
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      PubDate: 2017-02-14T17:55:07Z
       
  • Temperature-dependent synthesis of Pd@ZIF-L catalysts via an assembly
           method
    • Abstract: Publication date: 1 May 2017
      Source:Microporous and Mesoporous Materials, Volume 243
      Author(s): Hong Jiang, Songlin Xue, Yefei Liu, Weihong Xing, Rizhi Chen
      The Pd@ZIF-L catalysts with uniform crosshair-star shape and a size of about 20 μm were synthesized by an assembly method, in which a two-dimensional layered zeolitic imidazolate framework-L (ZIF-L) was used as the support to immobilize Pd nanoparticles. Their catalytic activities were evaluated by the catalytic reduction of p-nitrophenol to p-aminophenol. The results highlight that the physical-chemical and catalytic properties of the Pd@ZIF-L catalysts are greatly affected by the synthesis temperature. The temperature variation can make the catalysts transform from two-dimensional flakes to zero-dimensional spheres. High temperature is beneficial for increasing Pd loading and encapsulating Pd nanoparticles within the ZIF-L matrix. However, under the temperature larger than 30 °C, the dense dia(Zn) structures are formed. Increasing Pd loading in the Pd@ZIF-L catalysts leads to a significantly higher p-nitrophenol conversion. The relative dense structure of the as-synthesized catalysts makes p-nitrophenol access the active centers difficultly and a lower catalytic activity is observed. These findings would aid the development of high-performance Pd@ZIF-L catalysts.
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      PubDate: 2017-02-14T17:55:07Z
       
  • Adsorption of As4O6 from flue gas by zeolites: Influence of pore structure
           and Al substitution
    • Abstract: Publication date: 1 May 2017
      Source:Microporous and Mesoporous Materials, Volume 243
      Author(s): Xuesen Du, Jiyun Tang, Yanrong Chen, Xin Yang, Jingyu Ran, Li Zhang
      Efficient storage of arsenic is very important to its capture in the flue gas of power plants. In this study, Grand Canonical Monte Carlo method and Density Functional Theory were used to study the adsorption of arsenic in zeolites with various Si/Al ratios and pore sizes. The results show that pores with diameter of 7 Å are optimal for As4O6 adsorption in zeolites. High porosity can also promote the adsorption of As4O6 in a specific amount of zeolite. Al substitutions are beneficial for As4O6 adsorption. Experiments were used to test the adsorption of As4O6 using H-ZSM-5 zeolites with different Si/Al ratios. The results show the same trend with the theoretical study. The influences of possible compositions in flue gas including SO2, NO, H2O, CO2 and N2 were also tested using Grand Canonical Monte Carlo method. SO2 and NO can cause notable drop of As4O6 adsorption.
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      PubDate: 2017-02-14T17:55:07Z
       
  • Preparation of binderless activated carbon monoliths from cocoa bean husk
    • Abstract: Publication date: 1 May 2017
      Source:Microporous and Mesoporous Materials, Volume 243
      Author(s): M. Plaza-Recobert, G. Trautwein, M. Pérez-Cadenas, J. Alcañiz-Monge
      Binderless activated carbon monoliths were prepared from a new lignocellulosic precursor: cocoa bean husk. This study focussed on analysing the role of a lignocellusic-type precursor in the development of binderless carbon monoliths, and the characterisation of the porous texture and mechanical performance of the activated carbon monoliths. The results prove that an adequate combination of the macromolecular components of the cocoa bean husk (lignocellulosic molecules, gums, pectin and fats) together with a laminate macromolecular microstructure made it more suitable for obtaining binderless carbon monoliths, than other lignocellulosic precursors. In addition, the activation of these carbon monoliths gives activated carbon with a higher micropore volume and good mechanical performance.
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      PubDate: 2017-02-14T17:55:07Z
       
  • Liquid adsorption and catalytic degradation of
           4-methylnitrosamino-1-3-pyridyl-1-butanone (NNK) by zeolite
    • Abstract: Publication date: 1 May 2017
      Source:Microporous and Mesoporous Materials, Volume 243
      Author(s): Xiao Dan Sun, Shuo Hao Li, Xin Yu Ming Dong, Lei-jun Wang, Wen-bo Gu, Wei-miao Wang, Zheng-yu Yang, Ying Wang, Jian Hua Zhu
      Adsorption of 4-methylnitrosamino-1-3-pyridyl-1-butanone (NNK) along with N’-nitrosonornicotine (NNN) in water is studied for the first time with the monitoring of LC-MS/MS. In the mixed aqueous solution of NNK and NNN, NaZSM-5 zeolite uniquely captured NNK but refused NNN. And the influence of initial concentration, adsorption time and type of sorbents were systemically investigated. Degradation of NNK adsorbed on zeolite is studied with TG/MS and FTIR methods for the first time. It was degraded to NO, pyridine, amine and propanal at around 600 K, avoiding formation of volatile nitrosamines and secondary pollution.
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      PubDate: 2017-02-14T17:55:07Z
       
  • Hexavalent chromium removal from water by ionic liquid modified
           metal-organic frameworks adsorbent
    • Abstract: Publication date: 1 May 2017
      Source:Microporous and Mesoporous Materials, Volume 243
      Author(s): A. Nasrollahpour, S.E. Moradi
      In this work, carbonized Ag core metal-organic frameworks (MOFs) shell was prapered and used for the removal of some PAHs. The structural order and textural properties of the metal-organic frameworks were studied by X-ray powder diffraction (XRD), thermogravimetric (TGA), BET surface area, and Fourier transform infrared spectroscopy (FTIR) analysis. Batch sorption experiments were conducted to study the effect of contact time, initial concentration and agitation speed for the removal of chromate ion from aqueous solution. The sorption was maximum for the initial pH of 2.0. The kinetic data were best fitted to the pseudo-second order model. The sorption of metal-organic frameworks to chromate ion fits to the Langmuir model with R 2 of 0.9998, χ 2 of 0.092 and q max at 285.71 mg/g. Values of thermodynamic parameters viz. ΔG°, ΔH° and ΔS° were calculated and found to be −6.7 kJ/mol, 126.4 kJ/mol and 31.4 kJ/mol.K, respectively at 298 K. The values of ΔG° were found to be negative at all temperatures indicating the spontaneity of the removal process. A positive value of ΔH° further confirms the endothermic nature of removal process. The higher sorption capacity of ionic liquids loaded metal-organic frameworks for chromate ion is mainly due to the ionic liquid groups loaded on the surface of metal-organic frameworks which can react with Cr(VI) to form a complex deposited on the surface of metal-organic frameworks.
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      PubDate: 2017-02-14T17:55:07Z
       
  • The impact of the hydrodechlorination process on the physicochemical
           properties of bimetallic Ag-CuBeta zeolite catalysts
    • Abstract: Publication date: 1 May 2017
      Source:Microporous and Mesoporous Materials, Volume 243
      Author(s): A. Śrębowata, Izabela I. Kamińska, S. Casale, D. Brouri, C. Calers, S. Dzwigaj
      Beta zeolites with two Si/Al ratios of 17 and 1300 were used for synthesis of Ag2.0Cu2.0HAlBeta and Ag2.0Cu2.0SiBeta zeolites by conventional wet impregnation and two-step postsynthesis methods, respectively. The calcination of Ag2.0Cu2.0HAlBeta and Ag2.0Cu2.0SiBeta at 773 K for 3 h in air led to formation of C-Ag2.0Cu2.0HAlBeta and C-Ag2.0Cu2.0SiBeta. After reduction at 873 K for 3 h in flowing 10% H2/Ar, red-C- Ag2.0Cu2.0HAlBeta and red-C-Ag2.0Cu2.0SiBeta were obtained and investigated as the catalysts in gas phase hydrodechlorination of 1,2-dichloroethane at atmospheric pressure, at relatively low reaction temperature (523 K). The state of silver and copper in catalysts at different stages of their biography was characterized by low-temperature N2 sorption, temperature – programmed reduction (TPR), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and temperature-programmed hydrogenation (TPH). We have shown that the state of silver and copper species change under HDC conditions. After catalytic run both agglomeration of metal particles and their re-dispersion took place. According to TPH, XRD and XPS measurements we postulate that the cause of this phenomenon is the formation of chlorine containing species in spent zeolite catalysts.
      Graphical abstract image

      PubDate: 2017-02-14T17:55:07Z
       
  • Synthesis of ZIF-11 - Effect of water residues in the solvent onto the
           phase transition from ZIF-11 to ZIF-7-III
    • Abstract: Publication date: 1 May 2017
      Source:Microporous and Mesoporous Materials, Volume 243
      Author(s): Benjamin Reif, Florian Fabisch, Maximilian Hovestadt, Martin Hartmann, Wilhelm Schwieger
      The syntheses of MOFs and ZIFs are often accompanied by the formation of unwanted byproducts. Also for the ZIF-11 synthesis in N,N-Diethylformamide (DEF), phase impurities have been reported. In this systematic study, water residues in the reaction mixture could be identified as one major reason for the formation of the phase impurity ZIF-7-III within the ZIF-11 synthesis. The parameters ‘crystallinity’ and ‘phase index’ were introduced to quantify the phase transition.
      Graphical abstract image

      PubDate: 2017-02-14T17:55:07Z
       
  • Enhancement of fluorescence from one- and two-photon absorption of
           hemicyanine dyes by confinement in silicalite-1 nanochannels
    • Abstract: Publication date: 1 May 2017
      Source:Microporous and Mesoporous Materials, Volume 243
      Author(s): Dain Kim, Hyun Sung Kim
      We prepared unique organic–inorganic composite possessing strong one- and two-photon florescence properties by encapsulating hemicyanine molecules in nanosized silicalite-1 zeolite. The free hemicyanine dye in solvent and confined hemicyanine dye in nanochannels of silicalite-1 showed identical optical one- and two-photon absorption coefficients. By contrast, the fluorescence quantum yields of confined hemicyanine molecules in silicalite-1 channels from one and two-photon absorption were 5- and 3.3-fold, respectively, higher than those of free hemicyanine solution. Such contrasting behaviors in fluorescence were attributed to the isolation and confinement of hemicyanine in nanochannels of silicalite-1. This study represents a promising new strategy in the development of one- and two-photon fluorescence materials and a novel direction for zeolite research and its application in the development of optical materials.
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      PubDate: 2017-02-14T17:55:07Z
       
  • Synthesis and modification of titanium containing wrinkled mesoporous
           silica for cyclohexene epoxidation
    • Abstract: Publication date: 1 May 2017
      Source:Microporous and Mesoporous Materials, Volume 243
      Author(s): Zijie Wang, Kenneth J. Balkus
      Ti containing wrinkled mesoporous silica (Ti-WMS) has been prepared by direct synthesis with various Si/Ti ratios. Under similar conditions, Ti containing periodic mesoporous organosilicas (Ti-PMO) has been prepared with benzene bridges in the framework while maintaining the wrinkled structure. Both Ti-WMS and Ti-PMO samples have the radial wrinkled structure, and were further modified by trimethylsilylation to adjust the surface hydrophobicity. All catalysts were tested for the oxidation of cyclohexene with and without solvent using tert-butyl hydroperoxide as the oxidant. Ti-WMS catalysts showed superior catalytic performance over conventional Ti-MCM-41 when acetonitrile was used as the solvent. The radial wrinkled structure ensures better diffusion pathways for the reactants. For the catalytic reaction without solvent, Ti-WMS catalysts exhibit similar behavior to the conventional Ti-MCM-41 catalyst. Silylation was demonstrated to be an effective methodology to improve the catalytic activity because of enhanced surface hydrophobicity. The maximum turnover frequency was 1401 h−1 with an epoxide selectivity of 95% obtained using the silylated Ti-WMS catalyst with a Si/Ti ratio of 209.
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      PubDate: 2017-02-14T17:55:07Z
       
  • Monitoring instability of linear amine impregnated UiO-66 by in-situ
           temperature resolved powder X-ray diffraction
    • Abstract: Publication date: 1 May 2017
      Source:Microporous and Mesoporous Materials, Volume 243
      Author(s): Youngdong Song, Damien Thirion, Saravanan Subramanian, Myoung Soo Lah, Cafer T. Yavuz
      Carbon dioxide capture requires stable porous solids like zirconium based metal-organic frameworks (MOFs) in order to make sequestration efforts feasible. Because of the weak binding at low CO2 partial pressures, oligomeric amines are commonly loaded on porous supports to maximize CO2 capture while attempting to keep porosity for enhanced diffusion. Here we show the first temperature resolved stability study of linear-amine impregnated UiO-66 by in-situ monitoring of the PXRD pattern. Our findings show that the crystal structure shows a contraction at temperatures as low as 80 °C and deforms considerably above 120 °C, leading to significant doubts about their applicability in CO2 capture from lean feeds. We confirm that all MOFs need to be thoroughly analyzed at least by means of PXRD at the process relevant temperatures, and reinforced before any plausible plans of application in CO2 capture.
      Graphical abstract image

      PubDate: 2017-02-14T17:55:07Z
       
  • Kaolin-issued zeolite A as efficient adsorbent for Bezanyl Yellow and
           Nylomine Green anionic dyes
    • Abstract: Publication date: 1 May 2017
      Source:Microporous and Mesoporous Materials, Volume 243
      Author(s): Nor-El-Houda Fardjaoui, Fatima Zohra El Berrichi, Faouzi Ayari
      Zeolite A was synthesized by the autoclave method in alkaline medium using the DD3 Algerian clay, and then characterized by SEM, XRF, N2 physisorption at −196 °C, and XRD. In the temperature range 25–60 °C, the synthesized zeolite A can be efficiently used for Bezanyl Yellow (BY) and Nylomine Green (NG) adsorption (25 mg L −1) at very low adsorbent doses (5 × 10−4 g zeolite A g s o l u t i o n − 1 ) and neutral pH (∼7). The changes of free energy (ΔG°), enthalpy (ΔH°), and entropy (ΔS°) during physisorption were carefully evaluated. On the other hand, Freundlich isotherm and pseudo–second–order kinetics were found to be the most appropriate models to describe the endothermic physisorption of BY (E a = 23.4 ± 1 kJ mol−1) and NG (E a = 18.34 kJ mol−1). The synthesized zeolite A exhibited superior adsorption capacities and percentages of anionic dyes removal compared to DD3, bentonite and commercial zeolite A.
      Graphical abstract image

      PubDate: 2017-02-14T17:55:07Z
       
  • From 1-D to 3-D zeolite structures: performance assessment in catalysis of
           vapour-phase methanol dehydration to DME
    • Abstract: Publication date: 1 May 2017
      Source:Microporous and Mesoporous Materials, Volume 243
      Author(s): Enrico Catizzone, Alfredo Aloise, Massimo Migliori, Girolamo Giordano
      A series of molecular sieves from silico-aluminate (zeolites) to silico-aluminophosphate (SAPO-34) were synthesised, characterized and tested as catalysts for DME production via vapour-phase methanol-dehydration also benchmarking with a commercial γ−Al2O3. Both high methanol conversion and DME yield were achieved on zeolites but catalyst stability and coke formation was strongly dependent upon the channels configuration. 1-dimensional channels structures with large openings and/or side pockets suffered of high carbon deposition, causing catalyst deactivation whilst the 2-dimensional small pore channel system of FER structure ensures a high resistance to deactivation by inhibiting coke deposition. 3-dimensional structures showed a pronounced tendency to deposit heavier molecules in the coke phase, strongly affecting the catalytic performances. In fact, carbon deposit phase mainly consists in poly-substituted benzenes with a substitution level depending on the channel system (size and topology). Considering catalytic performances in terms of methanol conversion, DME selectivity and deactivation, ferrierite (Si/Al = 8.4) exhibited the best performances being a reliable catalyst for DME production via vapour-phase methanol dehydration.
      Graphical abstract image

      PubDate: 2017-02-14T17:55:07Z
       
  • Synthesis of ZSM-5 aggregates made of zeolite nanocrystals through a
           simple solvent-free method
    • Abstract: Publication date: 1 May 2017
      Source:Microporous and Mesoporous Materials, Volume 243
      Author(s): Wei Luo, Xuanyu Yang, Zhengren Wang, Wenfeng Huang, Jinyang Chen, Wan Jiang, Lianjun Wang, Xiaowei Cheng, Yonghui Deng, Dongyuan Zhao
      In the traditional hydrothermal synthesis of zeolites, the solvent of water is necessary for crystallization, so large amount of wastewater containing NaOH and organic pollutants could be inevitably produced. The solvent-free route is considered to remarkably enhance the synthesis efficiency and reduce the energy and pollutants in large scale production of zeolites, but the zeolites obtained usually consist of micrometer sized single crystals which only possess micropores and long diffusion pathway for molecules. In this study, a novel solvent-free synthesis system made of solid raw materials of anhydrous silica and aluminum sources, organic template and Na2CO3·10H2O, was demonstrated to synthesize ZSM-5 zeolite particles composed of nanocrystals of about 10–40 nm in size. The obtained ZSM-5 particles possess high crystallinity and surface area, and well-developed mesoporosity (5.2 nm) and excellent catalytic activity in polymer cracking, such as low-density polyethylene (LDPE), which is the main source of white pollution. The ZSM-5 aggregate particles with the micro-/meso- porous structure have the potential used as catalysts and adsorbents in industry.
      Graphical abstract image

      PubDate: 2017-02-14T17:55:07Z
       
  • Adsorption breakthrough behavior of 1-butanol from an ABE model solution
           with high-silica zeolite: Comparison with zeolitic imidazolate frameworks
           (ZIF-8)
    • Abstract: Publication date: 1 May 2017
      Source:Microporous and Mesoporous Materials, Volume 243
      Author(s): Chunping Gao, Jinglan Wu, Qi Shi, Hanjie Ying, Jinxiang Dong
      Adsorption breakthrough behavior of 1-butanol was studied on the hydrophobic materials ZSM-5, ZSM-12, and Beta zeolites and compared with the zeolitic imidazolate framework ZIF-8 from an ABE (acetone-1-butnaol-ethanol) model solution. Adsorption equilibrium and adsorption kinetics were analyzed in single-component systems. Our results showed that the equilibrium adsorption amounts for ZIF-8 were much higher than that of the zeolites but zeolites equilibrium time are shorter (10 min) than that of ZIF-8 (60 min). These phenomena were the result of kinetics effects and flexibility in the ZIF-8. We also evaluated the breakthrough characteristics of the fixed-bed in ABE ternary-component systems, and found that the adsorptive separation mechanism of zeolites was the thermodynamic effect, and that of ZIF-8 was a combination of thermodynamic and kinetic effects. We show that zeolite, especially Beta, is a very attractive material because it exhibits shorter equilibrium time for 1-butanol and better separation breakthrough performance for an ABE model solution and more suitable industrial application.
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      PubDate: 2017-02-14T17:55:07Z
       
  • Catalysis by the entangled complexes in matrix structure of zeolite-Y over
           α-pinene
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): Nisheeth C. Desai, Jiten A. Chudasama, Bonny Y. Patel, Krunalsinh A. Jadeja, Tushar J. Karkar, Jignasu P. Mehta, Dinesh R. Godhani
      Zeolite-Y entangled complexes based heterogeneous catalysts of VO(IV), Mn(II), Fe(II), Co(II), Ni(II) and Cu(II) and Schiff base ligand HMIMMPP = 4-(((2-hydroxy-5-methylphenyl)imino)methyl)-3-methyl-1-phenyl-1H-pyrazol-5-ol were prepared. The products were characterized by BET, FTIR, elemental analysis, SEM, thermogravimetric analysis, XRD and UV–Vis analysis. All entangled complexes and their neat complexes were utilized in the catalysis of α-pinene via tBuOOH as oxidative agent. α-pinene yielded verbenol and verbenone as major products due to the oxidative reaction. Conversion of products from reactant were in decreasing order as: [VO(HMIMMPP)(H2O)]-Y > [VO(HMIMMPP)(H2O)] > [Co(HMIMMPP)(H2O)]-Y > [Cu(HMIMMPP)(H2O)]-Y > [Ni(HMIMMPP)(H2O)]-Y > VO-Y > [Fe(HMIMMPP)(H2O)3]-Y > [Mn(HMIMMPP)(H2O)3]-Y > Na-Y. The entangled catalysts showed no metal leaching, easily recovery and reusability.
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      PubDate: 2017-02-14T17:55:07Z
       
  • FAU-type zeolite nanosheets from additives-free system
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): Stanislav Ferdov
      The existing concept for preparation of faujasite (FAU) type zeolite nanosheet assemblies is based on use of organic or extra inorganic morphology-directing templates or agents. Herein, a repetitive branching of hierarchically arranged nanolayers of FAU zeolite without employment of any morphology modifiers is demonstrated. This type of crystal growth is achieved only by kinetic control of carefully chosen conditions that border the co-crystallization of FAU- and EMT-type of zeolites. Furthermore, we provide evidence that the branching originates from recrystallization of zeolite nanoparticles followed by formation of submicron faceted crystals that further serve as nutrient for nanosheet structures. These findings open up a simple route to intergrowth of two-dimensional nanostructures of zeolites and may contribute to their scaled up production.
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      PubDate: 2017-02-08T22:00:28Z
       
  • Synthesis of binder-free granulated low-modular zeolites using ultrasound
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): Valery Yu. Prokof'ev, Natalya E. Gordina, Alexandra P. Khramtsova, Ekaterina M. Konstantinova, Darya S. Cherednikova
      Synthesis of binder-free granulated low-modular zeolites has been studied. As starting material, the aqueous suspensions of Na2SiO3·5H2O, Al2O3, and SiO2 have been used. The mixtures with atomic ratios Si:Al equal 1 and 2 have been prepared. For the pre-activation of the reaction mixtures, the ultrasound with a frequency of 22 kHz has been used. Moulding pastes have been prepared from the suspensions and then the pellets of 3 mm diameter have been extruded. The pellets have been calcined at 650 °C and then have been subjected to the hydrothermal crystallization in NaOH solutions with concentrations of 2 and 6 mol l−1. XRD, SEM, and FT-IR have been used for testing. It was found that at the ratio of Si: Al = 1 after the thermal treatment, sodium aluminosilicates of cubic syngony have been synthesized, and with an atomic ratio of 2, orthorhombic and monoclinic Na2Si2O5 have been formed. The hydrothermal crystallization of the pellets with an Si:Al = 1 resulted in forming three types of zeolites (NaP, sodalite, NaA). When the ratio Si:Al in the pellets was 2, NaP and sodalite have been synthesized. It was found that ultrasonic treatment caused a change in the morphology of the solid phase, which was traced at all stages of the preparation of granulated zeolites. The morphological differences determined the phase composition and crystallite size after hydrothermal crystallization. It was shown that at the ratio of Si:Al = 2 using sonication of the suspension and crystallization pellets in 2 M alkali solution, the pure phase of NaP zeolite has been synthesized, and the solid phase had a wool-like morphology.
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      PubDate: 2017-02-08T22:00:28Z
       
  • An investigation into mechanism of cation adsorption by reconstruction of
           calcined layered double hydroxide
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): Mengjie Wu, Jia Zhang, Yongqiang Peng, Jizhi Zhou, Xiuxiu Ruan, Jianyong Liu, Qiang Liu, Yunfei Xi, Ray Frost, Guangren Qian
      This work investigated the mechanism and limit of cation adsorption by reconstruction of calcined layered double hydroxide (CHT) for the first time. MgxAl-CHT was used to adsorb Zn2+ and Ni2+ from aqueous solution. As a result, adsorption amount of cation was approximately equal to dissolved amount of Mg2+ from CHT. In other words, the molar ratio was close to 1:1 between exchanged cation (Zn2+ or Ni2+) and released Mg2+. Besides, Zn2+ adsorption and Mg2+ dissolution took place synchronously until equilibrium. XRD and SEM indicated that CHT rebuilt layered double hydroxide (LDH) after adsorbing Zn2+ and Ni2+. Furthermore, molar ratios of Mg2+/Zn2+ and Mg2+/Ni2+ were 1:1 in reconstructed CHT regardless of the original Mg2+/Al3+ ratio. Based on these results, it was proposed that half of octahedral Al3+ in LDH transformed into tetrahedral ones after calcination, resulting in half of Mg2+ bond being distorted in CHT and ready for a potential exchange. When CHT was used to adsorb bivalent cation (Me2+), the maximum amount of adsorption was the half amount of Mg2+, and MgMeAl-LDH was formed by dissociation-deposition.
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      PubDate: 2017-02-08T22:00:28Z
       
  • Synthesis of ZSM-5 with hierarchical porosity: In-situ conversion of the
           mesoporous silica-alumina species to hierarchical zeolite
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): Teng Xue, Huaping Liu, Ying Zhang, Haihong Wu, Peng Wu, Mingyuan He
      Hierarchical ZSM-5 aggregates were fabricated using the conventional surfactant cetyltrimethylammonium bromide (CTABr) as the mesoporogen together with 1, 6-diaminohexane (HDA) as structure-directing agent. The competition of the templates and the subsequent phase separation were effectively avoided. A possible formation mechanism was proposed based on the investigation of the crystallization process. The obtained hierarchical ZSM-5 aggregates were highly crystallized, possessing large external surface area, mesopore volume and regular mesopore size distributions. And they were proved to be more efficient in catalytic LDPE cracking due to improved accessibility of large polymer molecules to the active sites. This method was facile and cost-effective, applicable within a wide SiO2/Al2O3 ratio by using various silica sources.
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      PubDate: 2017-02-08T22:00:28Z
       
  • Nanostructured hybrid materials as precursors of mesoporous NiMo-based
           catalysts for the propane oxidative dehydrogenation
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): Benjamin Farin, Michel Devillers, Eric M. Gaigneaux
      Nanostructured hybrid materials made of guest ions and a self-assembled copolymer were used as precursors for the preparation of NiMo-based catalysts. The hybrids were calcined in air and the recovered materials were characterized and tested in propane oxidative dehydrogenation. A 6-fold improvement of the yield to propene is obtained as compared with classically prepared catalysts. The exothermic degradation profile of the copolymer is the key point of our approach as it allows to prepare a porous β-NiMoO4, namely the phase particularly desired for its superior propene selectivity. More precisely, the polar backbone and the aliphatic side chains of the copolymer burn at different temperatures. The former ignites at moderate temperatures and initiates the early crystallization of β-NiMoO4. Occurring at higher temperature, the decomposition of the aliphatic part then induces the formation of mesopores. A β-NiMoO4 can thus be prepared at moderate temperatures whereas elevated calcination temperatures (>650 °C) are usually required. This peculiar behavior enables to prevent the texture of NiMoO4 from sintering and to maintain at high levels its mesoporosity, specific area and thus catalytic activity. At the end, the use of our tailor designed copolymer template allows reaching the remarkably high propene yields obtained.
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      PubDate: 2017-02-08T22:00:28Z
       
  • Promotional effect of Ni2P on mixed and separated phase MoS2/Al-SBA-15
           (10) catalyst for hydrodenitrogenation of ortho-Propylaniline
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): P. Santhana Krishnan, R. Ramya, S. Umasankar, K. Shanthi
      Mixed phase MoS2(Ni2P)/Al-SBA-15 (10) catalyst was prepared by incipient wet impregnation method using soft chemical approach by low temperature decomposition ATTM and separated phase Ni2P//MoS2/Al-SBA-15 (10) catalyst was set by simple mechanical separation of Ni2P/Al-SBA-15 (10) and MoS2/Al-SBA-15 (10) in a fixed bed reactor tube. The efficiency of both the catalysts was investigated for hydrodenitrogenation (HDN) of ortho-Propylaniline (OPA). The promotional effect of Ni2P in the mixed phase catalyst was correlated with spill-over hydrogen, hydrogenation active sites and acid sites. The synthesized catalysts were extensively characterized by various techniques such as XRD, BET, TPD/TPR, HR-SEM, HR-TEM, DRS-UV-Vis and XPS. The H2 pulse chemisorption study in correlation with HDN activity revealed that mixed phase MoS2(Ni2P)/Al-SBA-15 (10) catalyst possesses high spill-over hydrogen and high surface acidity. This study concluded that promotional effect and synergetic factor of Ni2P promoted MoS2/Al-SBA-15 (10) in the mixed phase catalyst is competitive over the separated phase Ni2P promoted MoS2/Al-SBA-15 (10) for HDN of OPA at atmospheric pressure.
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      PubDate: 2017-02-08T22:00:28Z
       
  • A crystal seeds-assisted synthesis of microporous and mesoporous
           silicalite-1 and their CO2/N2/CH4/C2H6 adsorption properties
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): Chang Wang, Jiaqi Liu, Jiangfeng Yang, Jinping Li
      Synthesis of ultra-high silica (SiO2/Al2O3 > 1800) MFI type zeolite such as silicalite-1 is still considered to be luxury because of the long synthesis time (5–12 days). Here, this material with a highly uniform mesoporous (20 nm) structure was crystallized in a shorter time (20 h) using a crystal-seeds method when an appropriate amount of potassium fluoride was added. Characterization techniques including XRD, SEM, TEM and liquid nitrogen adsorption provided detailed information on the two kinds of porous structure silicalite-1. Due to the “smooth” adsorption surface of silicalite-1 containing few equilibrium ions, it is ideal for the separation of gas mixtures containing non-polar molecules with similar physical properties. Moreover, the CH4, N2, CO2 and C2H6 adsorption properties were also investigated. Microporous silicalite-1 has a high adsorption capacity for CH4, N2, CO2 and C2H6 and adsorption selectivity for CH4/N2, CO2/N2, CO2/CH4 and C2H6/CH4. Although a lower adsorption capacity was observed for mesoporous silicalite-1, the pore size did not affect the outstanding adsorption selectivity, on the contrary, the selectivity of mesoporous silicalite-1 was improved.
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      PubDate: 2017-02-08T22:00:28Z
       
  • Adsorption characteristics of cesium onto mesoporous geopolymers
           containing nano-crystalline zeolites
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): N.K. Lee, Hammad R. Khalid, H.K. Lee
      The present study investigates the adsorption of cesium onto high-strength bulk-type mesoporous geopolymers containing nano-crystalline zeolites. Fly ash/slag-based mesoporous geopolymers were synthesized by a hydrothermal treatment. Batch adsorption studies were carried out with different initial cesium concentrations, solution pH values, and contact time with adsorbent. Kinetic and isothermal studies were also conducted against the experimental results to comprehend the mechanism and equilibrium condition of adsorption process. A higher removal efficiency of 96% (against 100 mg/L initial concentration) was observed and the maximum adsorption capacity of the mesoporous geopolymers was found to be 15.24 mg/g. The results showed that these mesoporous geopolymer adsorbents have the potential to be used for the removal of hazardous contaminants from aqueous solutions as self-supporting sieves.
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      PubDate: 2017-02-08T22:00:28Z
       
  • Keggin-Al30 pillared montmorillonite
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): Jianxi Zhu, Ke Wen, Ping Zhang, Yuebo Wang, Lingya Ma, Yunfei Xi, Runliang Zhu, Hongmei Liu, Hongping He
      Pillared interlayered clays (PILCs) draw intensive attention in the fields of chemistry and material sciences, owing to their strong surface acidity and large microporosity. These materials are superior selective heterogeneous catalysts and adsorbents. However, conventional hydroxy-aluminum pillared clays are based on Al13, which cannot provide desirable properties due to its inherent limitation of size. Herein, a convenient method has been developed to prepare Al30 PILCs from montmorillonite (Mt) and a base-hydrolyzed solution of Al (III) chloride. To the best of our knowledge, this is the first time that porous pillared interlayered Mt with large Al30 pillars (2×1×1 nm) has been successfully prepared. This fundamental work may open up entirely new avenues for developing novel PILCs as heterogeneous catalysts and porous adsorbents.
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      PubDate: 2017-02-08T22:00:28Z
       
  • Synthesis of CoMoO4@RGO nanocomposites as high-performance supercapacitor
           electrodes
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): Lv Jinlong, Yang Meng, Ken Suzuki, Hideo Miura
      Pure CoMoO4 nanoplate arrays grew on nickel foam by one-step hydrothermal process, while flower-like nanoflake CoMoO4@RGO nanocomposites grew on nickel foam. Flower-like nanoflake CoMoO4@RGO nanocomposites electrode exhibited higher capacitance than pure CoMoO4 nanoplate arrays electrode. Maximum specific capacitance of 856.2 F g−1 was obtained at current density of 1 A g−1 for CoMoO4@RGO nanocomposites electrode. In addition, after 2000 cycles of continuous galvanostatic charge–discharge cycles, only 5.5% degradation of specific capacitance was found for CoMoO4@RGO nanocomposites. CoMoO4@RGO nanocomposites exhibited lower electrochemical resistance than pure-CoMoO4. This was because that the former had larger specific surface area and average pore diameter than the latter. The flower-like nanoflake CoMoO4 facilitated electrolyte movement during charge or discharge process and provided more active sites for the electrochemical reactions. In addition, the synergetic effect between RGO and CoMoO4 also improved the supercapacitor performance.
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      PubDate: 2017-02-08T22:00:28Z
       
  • Multifunctional mesoporous silica nanoparticles for cancer-targeted,
           controlled drug delivery and imaging
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): Luiza Baptista de Oliveira Freitas, Laura de Melo Corgosinho, Jerusa Araújo Quintão Arantes Faria, Virgílio Mateus dos Santos, Jarbas Magalhães Resende, Alexandre Soares Leal, Dawidson Assis Gomes, Edésia Martins Barros de Sousa
      Ordered mesoporous silica materials exhibit potential features to be used as multifunctional nanostructured drug delivery systems due to their biocompatibility, as well as to their textural and structural properties. Moreover, combining mesoporous silica nanoparticles and 64Cu becomes this system promising as theranostic device for early stage cancers since radioisotope carriers could be able to act in the treatment and imaging diagnosis simultaneously. In this paper, a multifunctional nanotheranostic system based on MCM-41 was prepared through post-synthesis functionalization of mesoporous silica MCM-41 with the tumor-homing peptide CREKA and DTPA, a ligand for copper ions. The obtained material was characterized by different techniques in order to investigate its physical-chemical properties. Additionally, the nanoparticles were loaded with the clinically approved anticancer drug methotrexate and the drug release kinetics profile was investigated. As a proof-of-concept, we also demonstrated successful activation of copper ions in a nuclear reactor to the radionuclide 64Cu. Besides, cell viability assays were conducted to prove the potential of the nanoparticles to be used for in vivo studies and to show that they do not affect the pharmacological action of MTX. Taken together, we believe that the multifunctional silica-based theranostic system could serve as a platform for cancer-targeted, controlled drug delivery and PET imaging to be applied in cancer therapy.
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      PubDate: 2017-02-08T22:00:28Z
       
  • Photocatalytic properties of mesoporous alumina containing Ni doped CdS
           nanostructures
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): Sachin G. Ghugal, Rakesh R. Mahalik, Pranali S. Charde, Suresh S. Umare, Sanjay B. Kokane, V. Sudarsan, Rajamma Sasikala
      A stable and visible light responsive photocatalyst, Ni doped CdS dispersed on mesoporous Al2O3, exhibits enhanced photocatalytic activity for methyl orange (MO) degradation compared to CdS-Al2O3, CdS and Ni doped CdS. A significant adsorption of MO is observed in mesoporous alumina and the composite. Solid state MAS NMR studies suggest a strong interaction between CdS and Al2O3 in this new combination of heterostructured photocatalyst. This interaction between CdS and Al2O3 helps in a good dispersion of CdS on alumina, which in turn enhances the photocatalytic activity. In the composite, CdS shows wurtzite type structure where as Al2O3 (γ-Al2O3) shows cubic spinel structure. Ni doped CdS-Al2O3 nanocomposite shows improved visible light absorption compared to undoped CdS. Photoelectrochemical studies suggest that better separation of charge carriers occurs in 1Ni-CdS and 1Ni-85CA compared to CdS. The enhanced activity of Ni doped composite nanostructure is attributed to increased adsorption of MO in the composite, increased surface area, better separation of photogenerated charge carriers and improved visible light absorption. Total organic carbon analysis of the dye solution after irradiation indicates the mineralization of the dye during photocatalytic reaction. Photodegradation in the presence of different quenchers suggests that e− plays a significant role in the degradation of methyl orange.
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      PubDate: 2017-02-08T22:00:28Z
       
  • Applications of molecular simulations for separation and adsorption in
           zeolites
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): Amira Abdelrasoul, Hongyu Zhang, Chil-Hung Cheng, Huu Doan
      Zeolites are fascinating and versatile materials which are vital for a wide range of industries, due to their unique structural and chemical properties, which are the basis of applications in gas separation, ion exchange, and catalysis. Given their economic impact, there is a powerful incentive for smart design of new materials with enhanced functionalities for maximizing their application performance. This review article intends to summarize the published reports on the applications of molecular simulation in adsorption, separation and diffusion. The theoretical aspects, adsorption thermodynamics, adsorption isotherm were comprehensively studied in relation to the adsorption applications and how the adsorbates' characteristics influence the adsorption. This review comprehensively discusses the theoretical and computational aspects of diffusion of pure components, long chain hydrocarbons or mixture diffusion, including the molecular dynamics simulations and kinetic Monte Carlo. Furthermore, the cation-zeolite-adsorbate interactions are thoroughly examined so as to elucidate the role of cations in zeolites applications and how the cation exchange influences structural dynamics and properties of zeolites. This study also focuses on the role of cations in gas/liquid adsorption and separations.
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      PubDate: 2017-02-08T22:00:28Z
       
  • New non-covalent functionalized phenyl-methyl-silica for biomolecules
           immobilization: Experimental and theoretical insights of interactions
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): Claudia Bernal, Frank Ramirez, Juan C. Poveda-Jaramillo, Monica Mesa
      A new strategy for functionalization of porous silica with phenyl-methyl groups is developed and demonstrated in this work. Bare silica, a hierarchical bimodal porous material, was functionalized with non-hydrolysable alkylsilane (trimethylphenylsilane) by liquid phase grafting, without the use of additional catalyst. The analyses carried out by FTIR, zeta potential and 29Si NMR of modified material indicating that the silane is efficiently and stably adsorbed on silica surface. Computational simulations showing the interaction between silane and silica is by formation of bridges between phenyl ring of silane and silanol groups of silica, with interaction energies similar to those found for hydrogen bridges. Additionally, this modification generates a change on hydrophobicity of silica (11% more hydrophobic than bare silica) that allows the success immobilization of lipase from Thermomyces lanuginosus, used as probe biomolecule. This biocatalyst exhibits a specific activity of 45.7 IU (50% more than those obtained with bare silica) and a half-life of 89.9 h at 45 °C in acetone, which is 5-fold higher than for the biocatalyst prepared with the bare silica. These results could contribute to the preparation of new and efficient materials to be used as supports for biocatalysts, delivery drugs and remediation.
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      PubDate: 2017-02-02T08:29:51Z
       
  • Solventless synthesis of AEL-type aluminophosphate molecular sieve from
           mechanochemically pretreated low-templated reactants
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): Xinhong Zhao, Xiangping Gao, Xiaoxiao Zhang, Zhixin Hao
      One of the main obstacles that hamper the application of zeolites is the high consumption of expensive structure-directing agent. Herein, we reported the mechanochemisty-mediated solventless synthesis of AlPO4-11 aluminophosphate molecular sieve with low dosage of diisopropylamine (DIPA) as the structure-directing agent. The influences of DIPA/Al2O3 ratio, fluoride ions, seed crystals and high-energy mechanochemical pretreatment on the synthesis of AEL-type zeolite were investigated in detail. Both DIPA and fluoride ions are indispensable for the successful synthesis of AEL phase. The resultant AEL molecular sieves were characterized by XRD, SEM, TG-DTA, CHN elements analysis, and N2 physisorption. The results indicate that the introduction of seed crystals cannot improve the phase purity and crystallinity of the resulting products. On the other hand, high-energy mechanochemical pretreatment not only can affect the morphology of AEL zeolite, but more importantly, can also reduce the consumption of structure-directing agent.
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      PubDate: 2017-02-02T08:29:51Z
       
  • New continuous process developed for synthesizing sponge-type polyimide
           membrane and its pore size control method via non-solvent induced phase
           separation (NIPS)
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): Myeongsoo Kim, Gunhwi Kim, Jinyoung Kim, Daero Lee, Sangrae Lee, Jinuk Kwon, Haksoo Han
      In this study, the improvement of synthesizing method of sponge-type polyimide (PI) membrane and its newly developed pore size control techniques are mainly described. The sponge-type polyimide membrane with large pore size (0.1–10 µm) and high permeability was successfully synthesized by using non-solvent phase separation method (NIPS) in continuous process and its full polyimidization is confirmed via Fourier-transform infrared technique. The theoretical approach in this research induced by Jurin's law which describes the height of a liquid within a thin capillary tube. In this theory, the pore size of membrane is highly influenced by the interactive tension between the polymer and solvents during synthesizing process of polymer membrane. There are two ways of controlling pore size established from Jurin's law. The validity of the application of Jurin's law was proven via comparison with theoretical and experimental data. Its inner structure of membrane and pore size are identified by field emission-scanning electron microscopy.
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      PubDate: 2017-02-02T08:29:51Z
       
  • Exploration of amination reactions on highly extendable active sites of
           Pd(II)-3-allylsalicylaldiminophenol (ASIP) complex over thiofunctionalized
           SBA-15
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): Anish Lazar, C.P. Vinod, A.P. Singh
      An effective and impressive heterogeneous catalyst, Pd(II)-3-allylsalicylaldiminophenol-SBA-15, dubbed as Pd(II)ASIP@SBA-15, for amination reactions of aryl halides to synthesize secondary amines (20), has been synthesized and characterized. Pd(II)ASIP@SBA-15 has been synthesized by the covalent anchoring of 3-allylsalicylaldehyde over thiofunctionalized SBA-15, then further reaction with 2-aminophenol, followed by metallation process by using Pd(II)(OAc)2. A specifically designed cheap and easily available organic ligand, 3-allylsalicylaldiminophenol (ASIP), was synthesized from 3-allylsalicylaldehyde and 2-aminophenol. Using this, the synthesis of Pd(II)ASIP@SBA-15 was carried out whereby the ligand providing an active co-ordination or chelating sites for palladium metal. This strategy helped in exposing the Pd(II)ASIP active sites from surface to channels of SBA-15 support during the reactions. The synthesized catalyst were characterized by CHN analysis, PXRD, Nitrogen sorption analyses, TG & DTA, FTIR, 13C and 29Si CPMASS NMR spectra, XPS, UV–Visible, SEM, EDAX and TEM. Pd(II)ASIP@SBA-15 catalyst was screened in heterogeneous amination reactions of aryl halides to produce N-aryl derivatives or secondary amines with high catalytic activity as revealed by turn over frequency (TOF) calculations. To explore the heterogeneous nature of catalysts, amination reactions were carried with neat Pd(II)ASIP complex and Pd(II)(OAc)2 catalysts. The catalyst was recycled several times without much loss of activity and Sheldon hot filtration test has been performed.
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      PubDate: 2017-02-02T08:29:51Z
       
  • Novel templated mesoporous carbons as electrode for electrochemical
           capacitors with aqueous neutral electrolytes
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): Josefa Ortiz-Bustos, Silvia Graciela Real, Manuel Cruz, Jesùs Santos-Peña
      In search for new electrodes for electrochemical capacitors, two template mesoporous carbons (TMC) are prepared with the replica method by using Plugged Hexagonal Templated Silica (PHTS) and Mesostructured Cellular Foam (MCF) as hard templates. No subsequent activation after synthesis is carried out in order to correlate textural and electrochemical properties in neutral sulfate electrolytes. TMC show interesting textural and conductive properties for capacitor electrode purposes: specific surface areas higher than 1000 m2 g−1, and low D/G bands ratio in the Raman spectra. Mesopore presence accounts for the fast formation of the double layer and the decrease of resistive properties which implies increased power properties referred to activated carbons. Symmetric carbon/carbon devices can provide energy densities 7–9 Wh kg−1 and maximal powers higher than 50 kW kg−1. These values compare well with 9 Wh kg−1 and 26 Wh kg−1 furnished by activated carbons. Nevertheless, such TMCs show two major issues for performing better than activated carbons in aqueous electrolyte capacitors. Firstly, they show surface carbon functionalities, narrowing the electrochemical window of the capacitor and decreasing the capacitor cycling life. Secondly, pore saturation is evidenced in these systems, unlike activated carbon, showing higher specific surface area and micropores content. Under prolonged cycling, our TMC electrode performance is poorer than that of activated carbon. However, mesoporosity positively affects the electrode response against increasing power. Beyond a power of 1.4 kW kg−1, only TMCs provide stable energy densities (>6.5 Wh kg−1), comparable or higher than those observed for activated carbons in corrosive electrolytes.
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      PubDate: 2017-02-02T08:29:51Z
       
  • Synthesis and characterization of magnetic core with two shells: Mordenite
           zeolite and CuO to form Fe3O4@MOR@CuO core-shell: As a visible light
           driven photocatalyst
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): S.K. Rajabi, Sh. Sohrabnezhad
      In the present study, for the first time the synthesis of magnetic Fe3O4 as core with separate two shells, mordenite (MOR) zeolitic shells and CuO shells, was suggested. The new core-shell (Fe3O4@MOR@CuO) was prepared in three steps: (i) preparation of iron oxide magnetite core via hydrothermal method with diameter size between 120 and 150 nm, (ii) development of mordenite (MOR) zeolite as first shells on the Fe3O4 cores (Fe3O4@MOR) by hydrothermal method with thickness between 30 and 50 nm and (iii) coating of second shells from CuO by post-synthesis method with average thickness 215 nm. The properties of prepared magnetic core-shells were characterized by diffuse reflectance spectroscopy (DRS), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), nitrogen adsorption–desorption measurement and vibration sample magnetometer (VSM). Based on EDX results, the weight percentage (wt%) of Fe3O4 cores, MOR and CuO shells were calculated 68.13, 28.17 and 3.7%, respectively. The XRD results indicated diffraction peaks for each three compounds in core-shell. The diffuse reflectance spectrum of Fe3O4@MOR@CuO photocatalyst presented a strong absorption in the 400–800 nm range, indicating the introduction of MOR broadened the visible light absorption ability. The photodecolorization of Fe3O4@MOR@CuO core-shell was investigated in the absence and presence of H2O2. The results showed that, zeolitic shells and Fe3O4 enhanced charge separation efficiency compared with that of the pure CuO and Fe3O4@CuO core-shell in photodegradation of methylene blue (MB) dye. The photocatalyst exhibited an enhanced and stable activity for the degradation of MB under visible light. The mechanism of separation of the photogenerated electrons and holes of the Fe3O4@MOR@CuO photocatalyst was discussed.
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      PubDate: 2017-01-27T08:16:22Z
       
  • Synthesis, temperature-dependent X-ray diffraction and Raman spectroscopic
           characterization of the sodalite to nosean phase-transformation of
           Na7.7(1)(MnO4)1.7(2)(H2O)0.8(2) [AlSiO4]6
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): Hilke Petersen, Lars Robben, Malik Šehović, Thorsten M. Gesing
      Investigations of hydrothermal synthesis in the basic Na2O-Al2O3-SiO2-MnO4-H2O -system with variations of synthesis temperature and NaOH concentration were carried out. A permanganate bearing sodalite Na7.7(1)(MnO4)1.7(2)(H2O)0.8(2) [AlSiO4]6 could be obtained. The crystal structure and temperature-dependent behavior of this sodalite was examined by TG-DTA, in-situ temperature-dependent (TD) PXRD and Raman spectroscopy. Two phase transitions were observed: The first one at 600 K raises the symmetry from P 4 ¯ 3 n to P m 3 ¯ n due to the thermal expansion leading to a fully expanded framework. The second one at 900 K lowers the symmetry to P 23 , which is driven by the thermal decomposition reaction of the MnO4 − ion, resulting in different fillings of the (nearest) neighboring cages forming a respective nosean type structure. The template-framework interactions were examined by temperature-dependent pre-resonance Raman spectroscopy and show the blocking of the template vibration through stronger template-framework interactions representing a solid state below ambient temperatures, whereas at elevated temperature the interaction strength decreases leading to a quasi-liquid single molecule template behavior.
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      PubDate: 2017-01-27T08:16:22Z
       
  • Preparation mechanism and catalytic performance of porous copper-doped
           calcium phosphate material
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): Weiwei Xu, Shiping Wang, Jia Yao, Haoran Li
      Through a hydrothermal process, materials contained copper-doped calcium phosphate (copper content 0.04–35.2 wt%) were prepared, which possessed space structure (specific surface area 18.4–89.6 m2/g) and maintained the activity of copper. The conditions of hydrothermal reaction were optimized, such as adding different organic compounds, adjusting pH, the concentration of reagents, reaction time, and temperature. By employing transmission electron microscope, scanning electron microscope, X-ray diffraction, Fourier transform infrared spectroscopy and other detection methods, to monitor the formation of the material, a mechanism was proposed. The material showed acceptable activity (better conversion than copper phosphate) and good recyclability (more than 5 recycles) in the aerobic oxidation of cyclohexene. The kinetic experiments at different temperature (40–60 °C) and time (0–12 h) indicated the reaction order with respect to cyclohexene was zero.
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      PubDate: 2017-01-20T20:40:24Z
       
  • Triphenylamine-based porous organic polymers: Synthesis and application
           for supporting phosphomolybdate to fabricate efficient olefin oxidation
           catalysts
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): Xiaojing Song, Wanchun Zhu, Yan Yan, Hongcheng Gao, Wenxiu Gao, Wenxiang Zhang, Mingjun Jia
      Two kinds of triphenylamine-based porous organic polymers (POPs) were synthesized by FeCl3-triggered Friedel-Crafts polymerization of triphenylamine (TPA) and formaldehyde dimethylacetal (FDA) in the absence or presence of benzene (Ph), which are denoted as POP-I (without additional Ph) and POP-II (with additional Ph as linker), respectively. Various characterization results confirm the successful synthesis of TPA-based polymers with different bridged linkers and hierarchical pore structure. Phosphomolybdic acid (HPMA) and cobalt phosphomolybdate (CoPMA) were immobilized onto the POPs, to form phosphomolybdate (PMA) functionalized POPs catalysts, and their catalytic properties were investigated for the selective oxidation of olefins with H2O2. All the PMA functionalized POPs materials are catalytically active for the epoxidation/oxidation of olefins, while CoPMA/POP-II shows the highest activity, stability and recyclability. TPA-based POPs have distinctive electron-donating and transferring ability, which can be further tuned by introducing more bridged linkers of -Ph and -CH2 groups. Multi-interactions between PMA and POPs supports could be built through the electronic and geometric effects exerted by the 3-D POPs supports on the PMA clusters. Moreover, the existence of Co cations may further strengthen the interactions between PMA and POPs supports by forming electrostatic or coordination interactions with the TPA ligands, thus resulting in the high stability of the CoPMA/POP-II against leaching of active species during the H2O2 mediated catalytic oxidation process.
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      PubDate: 2017-01-20T20:40:24Z
       
  • Fabrication of ordered mesoporous solid super base with high thermal
           stability from mesoporous carbons
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): Song Song Peng, Meng He Yang, Wen Ke Zhang, Xue Ni Li, Cheng Wang, Ming Bo Yue
      Mesoporous solid super bases with high thermal stabilities are highly attractive for use as green catalysts in various reactions. The decomposition of alkali-metal nitrates on mesoporous supports is a facile approach to the preparation of mesoporous super bases. However, the decomposition of nitrates needs a high temperature and the generated basic oxides destroy the mesoporous support structures because of the low electronegativities of the alkali metals. In the present study, highly ordered mesoporous solid super bases were prepared using ordered mesoporous carbons (OMCs) as supports. The dispersion and decomposition of the base precursor (KNO3) on the OMCs were studied using in-situ X-ray diffraction. The results show that the KNO3 decomposed into potassium oxides at low temperature and then these potassium oxides reacted with carbon at high temperature to form strong bases. The OMCs provided supports with highly ordered meso-structures and promoted KNO3 transformation to strongly basic sites. Transmission electron microscopy and N2 adsorption-desorption isotherm studies showed that the meso-structure was well preserved even after calcination at 800 °C. The obtained materials were strong bases and had high catalytic activities in dimethyl carbonate synthesis by transesterification. A dimethyl carbonate yield of 72% was achieved.
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      PubDate: 2017-01-20T20:40:24Z
       
  • Ultra-sensitive determination of insulin on pencil graphite electrode
           modified by cerium salen encapsulated zeolite (CS@Z-PGE)
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): Sima Pourbeyram, Maryam Moosavifar, Laleh Ashtari
      In this study, cerium salen encapsulated into dealuminated zeolite Y (CS@Z) was prepared through template synthesis method. This heterogeneous catalyst was characterized by XRD, FT-IR, SEM and EDS analysis. The amount of CS in the nanocage of zeolite was obtained 0.0846 g/g of support. Pencil graphite electrode modified by CS@Z was applied for electrochemical ultra-sensitive determination of insulin. Parameters influencing the method were optimized. A linear range calibration curve from 0.05 to 50 nM of insulin with a detection limit of [12.8 (±0.6) pM] (based on S/N = 3) and sensitivity of [44.3 (±0.8) μA μM−1] was observed at pH 7.4 and applied potential of 0.45 V by amperometry. The results demonstrated that the sensor can be used for the determination of insulin in the commercially available injections.
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      PubDate: 2017-01-20T20:40:24Z
       
  • Enhanced dispersion of Cr nanoparticles over nanostructured ZrO2-doped
           ZSM-5 used in CO2-oxydehydrogenation of ethane
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): Farhad Rahmani, Mohammad Haghighi, Bahman Mohammadkhani
      To develop an efficient Cr-based catalyst for CO2-oxydehydrogenation of ethane, H-ZSM-5 was modified with a series amount of ZrO2 (0–30 wt%) via the one-pot hydrothermal method and then, impregnated with aqueous solution of Cr(NO3)3. Several techniques including XRD, FESEM, EDX, TEM, BET, ICP, FTIR and H2-TPR were applied to characterize the physicochemical properties of as-synthesized samples. The successful synthesis of ZrO2-doped ZSM-5 supports was verified by XRD, EDX and ICP results. It was found that the existence of ZrO2 promoted the dispersion of Cr species, leading to smaller particle size of chromium oxide, which enhanced the catalyst reducibility and strengthened the interaction of the modified support with Cr species, thus facilitating a faster reduction-oxidation cycle. However, the excessive loadings of ZrO2 alleviate its synergetic effect due to the significant decrease of surface area, appearance of more number of agglomerations and surface coverage of ZSM-5. The results revealed that the highest catalytic activity was reached on Cr supported ZrO2-doped ZSM-5 containing 10 wt% zirconia. Besides, it exhibited stable activity during the course of running the reaction for about 5 h at 700 °C, suggesting that the presence of ZrO2 modifier not only boost the Cr/ZSM-5 activity but also makes it less sensitive to the deactivation. Accordingly, the optimum zirconia content in the ZrO2-doped ZSM-5 support of Cr-based catalysts seems to be 10 wt%.
      Graphical abstract image

      PubDate: 2017-01-20T20:40:24Z
       
  • Microwave-assisted synthesis of magnetic Fe3O4-mesoporous magnesium
           silicate core-shell composites for the removal of heavy metal ions
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): Zhengfu Zhao, Xian Zhang, Hongjian Zhou, Gang Liu, Mingguang Kong, Guozhong Wang
      An ultrafast and facile microwave assisted hydrothermal approach was applied to synthesize magnetic Fe3O4-mesoporous magnesium silicate (FMMS) core-shell composites for effective removal of Cu2+, Cd2+ and Pb2+ from aqueous solutions. The FMMS composites have mesoporous magnesium silicate shells encapsulated Fe3O4 spheres core structures, and the mesoporous shell assembled by a large number of intercrossed nanosheets with a diameter of 4.0 nm pores, thus exhibited the excellent capability to remove Pb2+ (223.2 mg/g) and Cu2+ (53.5 mg/g) ions from aqueous solutions. The superior removal capacity of the FMMS composites can be ascribed to its mesoporous structures with abundant adsorption active sites. The competitive adsorption studies showed that the adsorbent affinity order of three metal ions by FMMS composites is Cu2+>Pb2+>Cd2+. It is noteworthy that the heavy metal ions could not only adsorb on the surface of FMMS composites, but also intercalate into the intercrossed nanosheets of mesoporous magnesium silicate shell, which reveals the synergistic effect of the electrostatic attraction, surface complexation and ion exchange coupled with the adsorption bonding with surface hydroxyl groups. Furthermore, the FMMS composites exhibited excellent sorption-regeneration performance, which can be easily separated and recovered by external magnet. All results demonstrated that the magnetic FMMS core-shell composite was a promising sorbent material for the preconcentration and separation of heavy metal ions from the waste water.
      Graphical abstract image

      PubDate: 2017-01-20T20:40:24Z
       
  • Polyamine-based spin probes for the study of siliceous structures
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): Vadim V. Annenkov, Elena N. Danilovtseva, Spartak S. Khutsishvili, Viktor A. Pal'shin, Yuliya F. Polienko, Vitaliy V. Saraev, Tamara I. Vakul'skaya, Stanislav N. Zelinskiy, Igor A. Grigor'ev
      Three new spin probes containing polyamine chains (2 or 3 nitrogen atoms) and nitroxide were synthesized. These compounds are stable in aqueous media at pH 5–10, and shape and intensity of their ESR spectra do not depend on pH in this range. The involvement of the spin probes in association in solution results in decrease of the spin mobility which appears as spectral anisotropy. The polyamine spin probes bind to siliceous nanoparticles in solution resulting in a reversible decrease in spectral intensity. These observations open a new way for monitoring silicic acid condensation. Sorption of the spin probes on solid silica gives rise to anisotropic spectra. The polyamine spin probes penetrate into growing cells of diatom algae in a similar manner to polyamine-containing fluorescent dyes.
      Graphical abstract image

      PubDate: 2017-01-20T20:40:24Z
       
  • Water wettable, compressible, and hierarchically porous polymer composite
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): Tae Jin Choi, Do Yeon Kim, Ji Young Chang
      Compressible and hierarchically porous polymer composite (PUS-MOP-A) was prepared by carrying out Sonogashira-Hagihara coupling reaction of 1,3,5-triethynyl benzene, 1.4-diiodobenzene and 2,5-diiodobenzoic acid in a polyurethane sponge (PUS). 2,5-Diiodobenzoic acid was used as a co-monomer to provide acidic functionality to the pore surface. The microporous organic polymer (MOP-A) formed inside the PUS network showed fibrous morphology when 1,4-diiodobenzene was used as a major aryl halide. For the synthesis of PUS-MOP-A, the molar ratio between 1,4-diiodobenzene and 2,5-diiodobenzoic acid was chosen as 4:1. The Brunauer-Emmett-Teller (BET) surface area of PUS-MOP-A was 306 m2 g-1. PUS-MOP-A was treated with KOH, which converted the carboxyl groups on the MOP-A backbone to the carboxylate anions. The resulting polymer composite (PUS-MOP-Aa) absorbed water quickly, showing a water contact angle of 0°. Adsorption ability of PUS and PUS-MOP-Aa to remove chemical pollutants in an aqueous solution was studied using a cationic dye, Methylene Blue (MB) and an anionic dye, Methylene Orange (MO) as a model chemical. PUS-MOP-Aa could be manually compressed and released in an aqueous solution of MB, resulting in the fast dye removal. When an aqueous solution contained both the anionic and the cationic dye, PUS-MOP-Aa preferentially removed the cationic dye. PUS-MOP-Aa was recyclable after removing the adsorbed dyes by treating with an acid and washing.
      Graphical abstract image

      PubDate: 2017-01-20T20:40:24Z
       
  • Ag supported on meso-structured SiO2 with different morphologies for CO
           oxidation: On the inherent factors influencing the activity of Ag
           catalysts
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): Juan Xu, Jingyan Zhang, Honggen Peng, Xianglan Xu, Wenming Liu, Zheng Wang, Ning Zhang, Xiang Wang
      With the objective to prepare better CO oxidation catalysts and explore the inherent factors to determine the activity of supported Ag catalysts, KCC-1, SBA-15 and MCM-41, a series of mesoporous SiO2 with different morphologies, have been synthesized and used as supports for Ag to prepare catalysts (7% Ag/KCC-1, 7% Ag/SBA-15 and 7% Ag/MCM-41) for CO oxidation. It is found that the morphologies of the SiO2 supports influence the dispersion of the supported Ag species, thus resulting in catalysts with different Ag grain sizes and active metallic surface areas, as proved by XRD and H2 adsorption-desorption results. With fibrous KCC-1 silica spheres as the support, the mobilization and aggregation of the Ag particles can be effectively hindered by the open access surface mesopores. Therefore, compared with SBA-15 and MCM-41, Ag nanoparticles with much smaller grain sizes have been achieved, thus resulting in a catalyst with significantly improved activity. Furthermore, a linear relationship has been found between the differential CO oxidation rates and the Ag grain size. Therefore, it is concluded that the active Ag metal surface area is the determining factor for the activity of the silica supported Ag catalysts.
      Graphical abstract image

      PubDate: 2017-01-20T20:40:24Z
       
  • Synthesis, characterization and evaluation of MFI zeolites as matrixes for
           rhynchophorol prolonged release
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): Ingrid G. Ramos, Arão C. Viana, Edeilza L. dos Santos, Artur J.S. Mascarenhas, Antônio E.G. Sant'Ana, Henrique F. Goulart, Janice I. Druzian, Heloysa M.C. Andrade
      Rhynchophorol has been used as lure for monitoring and controlling the beetle Rhynchophorus palmarum L. in palm tree culture. However, for the efficient use of techniques based on pheromone it is required a constant and adequate release of this compound for long period, while adult insects are present. In order to evaluate the potential use of MFI zeolites (ZSM-5 and silicalite-1) as matrixes to slow down the release of rhynchophorol, the silicalite-1 and ZSM-5 zeolites in SiO2/Al2O3 molar ratio (SAR) of 24, 41 and 52 were synthesized and characterized by XRD, ED XRF, 27Al MAS NMR, FTIR, TG, SEM, textural analysis and NH3-TPD. Recovery studies showed that the rhynchophorol was completely degraded in ZSM-5, independently of the SAR. The degradation mechanism was proposed to occur via an intramolecular E1 elimination. Recovery above 90% was obtained only from silicalite-1 (SAR = ∞). This result indicated that not only acidity, but diffusional effects determine the stability of rhynchophorol in MFI zeolites.
      Graphical abstract image

      PubDate: 2017-01-20T20:40:24Z
       
  • Improved adsorption characteristics data for AQSOA types zeolites and
           water systems under static and dynamic conditions
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): How Wei Benjamin Teo, Anutosh Chakraborty, Wu Fan
      In this manuscript, the amount of water vapour uptakes on zeolites (types AQSOA-Z01, Z02 and Z05) under static and dynamic conditions were measured for the temperatures ranging from 298 K to 333 K and pressures up to saturated conditions. These data are fitted with the theoretical isotherms and kinetics equations, which are developed from Langmurian analogy. The experimentally measured isotherms data varying from Henry's region to the saturated pressure are also expressed in pressure–temperature–uptake co-ordinate system for the calculation of the isosteric heat of adsorption. The variations of isosteric heats are ranged from 1 to 1.4 times of the heat of vaporization. The AQSOA type zeolites show type V isotherms. For better understanding of adsorption and desorption processes, the hysteresis behaviours are also investigated.
      Graphical abstract image

      PubDate: 2017-01-20T20:40:24Z
       
  • Shape selectivity in toluene disproportionation into para-xylene generated
           by chemical vapor deposition of tetramethoxysilane on MFI zeolite catalyst
           
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): Daisuke Mitsuyoshi, Koji Kuroiwa, Yuta Kataoka, Takuya Nakagawa, Misaki Kosaka, Koshiro Nakamura, Satoshi Suganuma, Yasuhiro Araki, Naonobu Katada
      Dependence of shape selectivity for para-xylene production by toluene disproportionation on conditions of chemical vapor deposition (CVD) of tetramethoxysilane on MFI (ZSM-5) zeolite were investigated in detail. The CVD after pelletization was necessary to obtain 0.7–1 mm particles with high selectivity. The influences of preparation conditions on the selectivity were investigated in detail to find the optimum conditions. The parent zeolite with small number of Brønsted acid sites on the external surface brought the high selectivity after the CVD. The catalyst prepared in the optimized conditions showed the selectivity 99.7% at ca. 10% of the toluene conversion.
      Graphical abstract image

      PubDate: 2017-01-20T20:40:24Z
       
  • Understanding the hydrothermal, thermal, mechanical and hydrolytic
           stability of mesoporous KIT-6: A comprehensive study
    • Abstract: Publication date: April 2017
      Source:Microporous and Mesoporous Materials, Volume 242
      Author(s): Rupak Kishor, Aloke Kumar Ghoshal
      The three dimensional KIT-6 with interconnected mesoporous was synthesized using triblock copolymer (P123) in mild acidic condition. The hydrothermal, thermal, mechanical and hydrolytic stability of KIT-6 were comprehensively investigated by N2 adsorption/desorption, small-angle X-ray scattering and electron micrograph. In the initial stage of synthesis, washing of as-synthesized KIT-6 with water improves the textural property such as surface area and pore volume. The size of primary mesopores and pore volume of the material could be tailored by ageing the solution without any loss in structural morphology. KIT-6 shows the high mechanical stability up-to 4680 bar and preserves its mesopore surface area possibly due to the presence of thicker pore wall and cubical structure. KIT-6 shows the gradual decrease in surface area, pore volume and diameter with increasing calcination temperature from 823 to 1173 K, due to sintering/shrinkage of silica structure. It also shows the stable structural properties even after ageing for 6 months in atmospheric conditions and 1 month in water at room temperature. However, after 3 days of ageing in boiling water, KIT-6 still retains its porosity. In presence of ultra-high pressure, CO2 shows good surface interaction towards KIT-6 with sorption capacity of 1.42 mol/kg (1 bar) and 10.1 mol/kg (20 bar) at 273 K without significant damage to its structure. Additionally, it also shows 2.38 wt% H2 storage capacity at 30 bar and 77 K. The highly stable KIT-6 is considered to be a good material for catalyst support, nano structure, CO2 separation and H2 storage.
      Graphical abstract image

      PubDate: 2017-01-20T20:40:24Z
       
 
 
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