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Dissertations / Theses on the topic 'Silicalite'

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Published: 4 June 2021

Last updated: 6 September 2023

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1

Halhead, Michael David. "Characterisation of silicalite and post synthesis modified silicalite using adsorption." Master's thesis, University of Cape Town, 2001. http://hdl.handle.net/11427/13894.

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Bibliography: leaves 89-96.
The study of adsorption on microporous materials such as zeolites is of tremendous scientific and industrial interest. The effective development and design of both equipment and processes is reliant on the availability of accurate information on the processes of adsorption in these materials. Zeolites, of the type studied in this thesis, are becoming increasingly important in a wide range of fields such as ion-exchange, purification, separations particularly of close boiling compounds and catalytic processes. The work presented had two primary objectives. The first was the design and construction of a reliable apparatus for the measurement of adsorption isotherms. This adsorption apparatus was based upon the gravimetric technique due to the reliability, high sensitivity and the widespread use of this type of technique. The system constructed was a flow system as opposed to the more commonly used vacuum system. The choice of a flow gravimetric system introduces a number of advantages: * The effect of the heat of adsorption is reduced * The system is better able to replicate industrial conditions * The gravimetric technique is simple to use .

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2

Hargreaves, S. M. "Hydrocarbon adsorption in silicalite : experimental and numerical studies." Thesis, University of Cambridge, 2000. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.603712.

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The work contained in this thesis addresses the single and multicomponent adsorption of hydrocarbons in silicalite. Both experimental and numerical work is presented. Experimental measurements are made using a volumetric technique and many equilibrium adsorption studies are reported for the first time. Multicomponent adsorption studies have revealed several novel adsorption phenomena. Intermolecular interaction within silicalite has been probed using deuterium nuclear magnetic resonance (²H NMR) experiments. For the first time data are presented for both single and multicomponent adsorbates within the structure and the effect of co-adsorption upon molecular microdynamics is investigated. Incorporating ²H NMR data obtained with the network model for the adsorbent in a numerical simulation known as Monte Carlo Lattice Dynamics, has enabled equilibrium predictions to be made for single and multicomponent adsorption. On comparison with the experimental data obtained the results achieved by Monte Carlo Lattice Dynamics are very good and demonstrate the strength of the simulation orthodoxy. Molecular mechanic simulations, together with data obtained from ²H NMR and volumetric studies have also been used to probe the behaviour of the external surface of silicalite in the study of adsorbate uptake kinetics. Results indicate that a surface-moderated insertion can affect the uptake of a component from the gas phase and hence affect the gross adsorption uptake properties of the material. Binary component studies have also been performed in which the interplay between adsorbate surface mobility and molecular desorption rates can affect a separation between components.

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3

Sowerby, Beverley. "Drying of organic vapours by adsorption." Thesis, University of Bath, 1988. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.284567.

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4

Flynn, Tracey Karen. "Some sorption and salt occlusion properties of silicalite-1." Thesis, University of Edinburgh, 1987. http://hdl.handle.net/1842/14868.

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5

Boulicaut, Ludovic. "Sorption and diffusion in silicalite crystals studied by HPLC." Thesis, National Library of Canada = Bibliothèque nationale du Canada, 1997. http://www.collectionscanada.ca/obj/s4/f2/dsk2/ftp04/mq23781.pdf.

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6

Van-Den-Begin, Neil Graham. "A study on diffusion of hydrocarbons in silicalite-1." Thesis, Imperial College London, 1990. http://hdl.handle.net/10044/1/46591.

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7

Simon, Jean-Marc, Nicole Floquet, Jean-Pierre Bellata, and Guy Weber. "Commensurate diffusion effects of n-heptane in silicalite-1." Universitätsbibliothek Leipzig, 2015. http://nbn-resolving.de/urn:nbn:de:bsz:15-qucosa-185690.

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8

Carter, David, Boguslaw Kruczek, and F. Handan Tezel. "Application of Maxwell Stefan equations to characterize silicalite membranes." Universitätsbibliothek Leipzig, 2016. http://nbn-resolving.de/urn:nbn:de:bsz:15-qucosa-198056.

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9

Simon, Jean-Marc, Nicole Floquet, Jean-Pierre Bellata, and Guy Weber. "Commensurate diffusion effects of n-heptane in silicalite-1." Diffusion fundamentals 16 (2011) 73, S. 1-2, 2011. https://ul.qucosa.de/id/qucosa%3A13816.

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10

Carter, David, Boguslaw Kruczek, and F. Handan Tezel. "Application of Maxwell Stefan equations to characterize silicalite membranes." Diffusion fundamentals 24 (2015) 8, S. 1, 2015. https://ul.qucosa.de/id/qucosa%3A14522.

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11

Lee, Seung Ju. "Morphological control of silicalite-1 crystals using microemulsion mediated growth." Diss., Texas A&M University, 2005. http://hdl.handle.net/1969.1/2535.

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Zeolites are crystalline, microporous aluminosilicates that have been extensively used in heterogeneous catalysis, separations, and ion-exchange operations. It has long been understood that particle size and morphology play a central role in the successful application of zeolites. This dissertation reports on controlling the morphology of all-silica zeolite, silicalite-1, made in nonionic/ionic microemulsions under conventional synthesis conditions. Silicalite-1 materials formed in microemulsion-mediated syntheses possess different morphological properties as compared to samples grown using the same synthesis mixture in the absence of the microemulsion. The work presented here is a systematic study showing how parameters such as synthesis temperature, microemulsion composition, silica precursor, alkali content, presence of salt, and the surfactant identity impact the material properties, most notably crystal morphology. In the nonionic microemulsion mediated synthesis, the work demonstrates the possibility of using microemulsions to manipulate the shape and size of silicalite-1 materials, growing both spheres and high-aspect ratio platelets. In both cases these large particles are robust aggregates of small submicron particles. Based on the results presented, a mechanism is proposed illustrating the role of both the confined space presented by the microemulsion as well as the importance of the surfactant-silicate interactions leading to the formation of the large aggregates. In the cationic microemulsion mediated synthesis, it is concluded that the surfactant??silicate interactions are primarily responsible for the modulation of crystal morphology observed. The results indicate that surfactant adsorption on the growing crystal surface, not the confined space afforded by the microemulsion, is essential. The results suggest that this may be a versatile and useful approach to controlling zeolite crystal morphology and growth of crystals obtained from conventional high-silica zeolite synthesis procedures.

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12

Tawalbeh, Muhammad. "Silicalite-1 Membranes Synthesis, Characterization, CO2/N2 Separation and Modeling." Thèse, Université d'Ottawa / University of Ottawa, 2013. http://hdl.handle.net/10393/30330.

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Zeolite membranes are considered to be a promising alternative to polymeric membranes and they have the potential to separate gases under harsh conditions. Silicalite-1 membranes in particular are easy to prepare and suitable for several industrial applications. In this research project, silicalite-1/ceramic composite membranes were prepared using the pore plugging hydrothermal synthesis method and supports with zirconium oxide and/or titanium oxide as active layers. The effect of the support’s pore size on the morphology and permeation performance of the prepared membranes was investigated using five supports with different active layer pore sizes in the range of 0.14 – 1.4 m. The prepared membranes were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), electron diffraction spectrometer (EDS), single gas and binary gas mixtures permeation tests. The results confirmed the presence of a typical silicalite-1 zeolite structure with a high internal crystalline order grown inside the pores of the active layer of the supports, with a dense film covering most of the supports active layers. Silicalite-1 crystals in the prepared membranes were preferably oriented with either a- or b-axes perpendicular to the support surface. Single gas permeation results illustrated that the observed permeances were not directly related to the kinetic diameter of permeants. Instead, the transport of the studied gases through the prepared membranes occurred by adsorption followed by surface diffusion mechanism. Binary gas tests performed with CO2 and N2 mixtures showed that the prepared membranes were selective and very permeable with CO2/N2 permselectivities up to 30 and a CO2 permeances in the order of 10-6 mol m-2 Pa-1 s-1. A model was developed, based on Maxwell−Stefan equations and Extended Langmuir adsorption isotherm, to describe the transport of binary CO2 and N2 mixtures through the prepared silicalite-1 membranes. The model results showed that the exchange diffusivities (D12 and D21) were less dependent on the feed pressure and feed composition compared to the permeances and the permselectivities. Hence, they are more appropriate to characterize the intrinsic transport properties of the prepared silicalite-1 membranes.

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13

Du, Zhimei. "Computer simulation and theoretical studies of hydrocarbon adsorption in silicalite." Thesis, London South Bank University, 2000. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.342841.

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14

Fernandez, Moisés, André Pampel, Jörg Kärger, Dieter Freude, Baten Jasper M. van, and Rajamani Krishna. "Mixture diffusion in silicalite-1 studied by MAS PFG NMR." Universitätsbibliothek Leipzig, 2016. http://nbn-resolving.de/urn:nbn:de:bsz:15-qucosa-193984.

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15

Fernandez, Moisés, André Pampel, Jörg Kärger, Dieter Freude, Baten Jasper M. van, and Rajamani Krishna. "Mixture diffusion in silicalite-1 studied by MAS PFG NMR." Diffusion fundamentals 6 (2007) 61, S. 1-2, 2007. https://ul.qucosa.de/id/qucosa%3A13189.

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16

Vaidya, Prahar S. "PURE AND BINARY ADSORPTION OF METHANE AND NITROGEN ON SILICALITE." Cleveland State University / OhioLINK, 2016. http://rave.ohiolink.edu/etdc/view?acc_num=csu1463751121.

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17

Zhang, Baojian. "Template-directed construction of hierarchically ordered zeolite materials." Thesis, University of Bristol, 2001. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.364867.

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18

Chafin, Raymond William II. "Torlon® and Silicalite Mixed Matrix Membranes for Xylene Isomer Purification." Diss., Georgia Institute of Technology, 2007. http://hdl.handle.net/1853/14562.

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Organic/inorganic materials have a high potential to enable major advances in membrane performance. It has previously been impossible to develop polymeric systems with adequate transport properties for xylene purification. Zeolite membranes have been created with the appropriate selectivities; however low productivity, low mechanical durability, and high capital costs have kept these materials from being utilized. So-called mixed matrix hybrid organic/inorganic membranes combine the mechanical durability and cost effectiveness of polymeric membranes with the enhanced performance of zeolitic structures. This project will focus on investigating polymeric and molecular sieve materials for mixed matrix membrane use in xylene isomer separation as a model system. Torlon polyamide-imide has unique properties that should be potentially useful in a mixed matrix composite. Silicalite will be investigated as the dispersed phased given its proven applicability with xylene isomers. The overarching goal is to establish an approach for creation of mixed matrix materials that can be broadly applied to challenging organic separations. This project has three specific goals: (1) characterization of Torlons inherent properties, processing ability, and important transport potential, (2) characterization of zeolite matching properties and the effect of interfacial engineering on these properties, and (3) development of appropriate approaches to combine the sieve and polymer to obtain a hybrid material with properties that match theoretically predicted separation property enhancements relative to the neat polymer. High temperature pervaporation will be used to evaluate material transport properties, as this experimental setup closely mimics the high activity vapor streams found in many industrial xylene processes. The results of this research will be used to develop a protocol for development of future mixed matrix membranes that may be applied to a variety of organic liquid systems.

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19

Inzoli, Isabella, Signe Kjelstrup, Dick Bedeaux, and Jean-Marc Simon. "The coupled transport of heat and mass across a silicalite surface." Universitätsbibliothek Leipzig, 2015. http://nbn-resolving.de/urn:nbn:de:bsz:15-qucosa-189575.

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20

Inzoli, Isabella, Jean Marc Simon, and Signe Kjelstrup. "Surface resistance to heat and mass transfer in a silicalite membrane." Universitätsbibliothek Leipzig, 2016. http://nbn-resolving.de/urn:nbn:de:bsz:15-qucosa-193396.

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21

Loisruangsin, Arthorn, Siegfried Fritzsche, and Supot Hannongbua. "Potential calculations and MD simulations of n-pentane in silicalite-1." Universitätsbibliothek Leipzig, 2016. http://nbn-resolving.de/urn:nbn:de:bsz:15-qucosa-195428.

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22

Loisruangsin, Arthorn, Siegfried Fritzsche, and Supot Hannongbua. "Potential calculations and MD simulations of n-pentane in silicalite-1." Diffusion fundamentals 2 (2005) 29, S. 1-2, 2005. https://ul.qucosa.de/id/qucosa%3A14359.

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23

Chmelik, Christian, Lars Heinke, Jörg Kärger, Baten Jasper M. van, and Rajamani Krishna. "Diffusion of n-butane/iso-butane mixtures in silicalite-1 investigated using infrared microscopy: Diffusion of n-butane/iso-butane mixtures in silicalite-1investigated using infrared microscopy." Diffusion fundamentals 11 (2009) 25, S. 1-2, 2009. https://ul.qucosa.de/id/qucosa%3A13966.

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24

Zhou, Qianqian. "Pure Component Adsorption of Methane, Ethylene, Propylene and Carbon Dioxide in Silicalite." Cleveland State University / OhioLINK, 2013. http://rave.ohiolink.edu/etdc/view?acc_num=csu1369150380.

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25

Pellenq, Roland Jean-Marc Gabriel. "Theory and computer simulation of absorption of simple molecules in silicalite-1." Thesis, Imperial College London, 1994. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.339443.

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26

Fryčová, Marie, Petr Sysel, Pavel Hrabánek, Milan Kočiřík, Libor Brabec, Arlette Zikánová, Bohumil Bernauer, Pavel Čapek, and Vladimír Hejtmánek. "Helium permeation through mixed matrix membranes based on polyimides and silicalite-1." Universitätsbibliothek Leipzig, 2015. http://nbn-resolving.de/urn:nbn:de:bsz:15-qucosa-188833.

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27

Jalili, S. E. "Monte Carlo simulation and statistical mechanics modelling of mixture adsorption in silicalite." Thesis, University College London (University of London), 2011. http://discovery.ucl.ac.uk/1318086/.

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Adsorption in zeolites is widely and increasingly used in many industrial processes. For the design of new processes and improvement of the performance of existing ones, basic adsorption data is needed but due to the difficulties of experimentation it is lacking. In this thesis, different methods have been used to calculate the adsorption isotherms of benzene, methane, ethane and CO, mixtures as well as Propane, i-butane and n-butane and their binary and ternary mixtures in zeolites. Firstly, Lattice Model has been used to calculate benzene adsorption isotherms in silicalite zeolite whose experimental adsorption isotherms exhibit unusual features. The zeolite is modelled as two types of quasi one- dimensional pores. The lattice model has dimer states to represent molecules lying in extended states with the aromatic ring on average parallel to the pore wall, the monomer state to represent molecules standing perpendicular to the principle axis of the pores. Vacant sites or holes allow for incomplete filling of the lattice sites. For a wide range of interaction parameters the model gives steps in the adsorption isotherms similar to those observed experimentally for benzene adsorption in silicalite. The model attributes the experimentally observed steps in the level of adsorption with rising pressure, to re-orientational transitions amongst molecules in the adsorbed phase. Secondly Conventional Grand Canonical Monte Carlo techniques have been used to calculate methane, ethane and co, binary mixture adsorption isotherms in silicalite as well as propane, i-butane and n-butane equimolar binary and ternary mixture adsorption in silicalite. In the last part of the thesis, studies have made of lattice models of CH, I C,H, and CO, adsorption in silicalite and the results compared with the Monte Carlo data. One dimensional lattice models have also been used to calculate the binary and ternary mixture adsorption of propane, i-butane and n-butane. The isotherms were compared with the Monte Carlo results.

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28

Fryčová, Marie, Petr Sysel, Pavel Hrabánek, Milan Kočiřík, Libor Brabec, Arlette Zikánová, Bohumil Bernauer, Čapek Pavel Pavel, and Vladimír Hejtmánek. "Helium permeation through mixed matrix membranes based on polyimides and silicalite-1." Universitätsbibliothek Leipzig, 2015. http://nbn-resolving.de/urn:nbn:de:bsz:15-qucosa-191331.

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Mixed matrix membranes based on modified polyimides and silicalite-1 were prepared and studied. The novel preparation approach consists in improvement of the interfacial adhesion by employment of the coupling agent 3-aminopropyltriethoxysilane in such a way which leads to forming of chemical bonds between polyimide and silicalite-1. Firstly polyimide chains were endcapped by this agent which subsequently enabled their reaction with groups naturally present on silicalite-1 surface. Membranes with silicalite-1 content up to 60 wt. % were prepared and characterized by SEM, light microscopy and permeation of gases, prevailingly of He. The accessibility of sililicalite-1 pores prior to embedding and after embedding into polymeric matrices was studied by an iodine indicator technique. The permeability of membranes for gases was measured using a semi-open permeation apparatus with a small volume. Helium permeability depended on filler content and increased monotonously with the increasing content of filler. There were, however, significant deviations of the permeability dependences on filler content from shapes predicted by Bruggeman’s model. The qualitative explanation of the data disagreement with the model was proposed based on a stratification of mixed matrix membranes found by SEM.

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29

Fryčová, Marie, Petr Sysel, Pavel Hrabánek, Milan Kočiřík, Libor Brabec, Arlette Zikánová, Bohumil Bernauer, Pavel Čapek, and Vladimír Hejtmánek. "Helium permeation through mixed matrix membranes based on polyimides and silicalite-1." Diffusion fundamentals 11 (2009) 6, S. 1-2, 2009. https://ul.qucosa.de/id/qucosa%3A13926.

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30

Fryčová, Marie, Petr Sysel, Pavel Hrabánek, Milan Kočiřík, Libor Brabec, Arlette Zikánová, Bohumil Bernauer, Čapek Pavel Pavel, and Vladimír Hejtmánek. "Helium permeation through mixed matrix membranes based on polyimides and silicalite-1." Diffusion fundamentals 11 (2009) 90, S. 1-17, 2009. https://ul.qucosa.de/id/qucosa%3A14063.

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Mixed matrix membranes based on modified polyimides and silicalite-1 were prepared and studied. The novel preparation approach consists in improvement of the interfacial adhesion by employment of the coupling agent 3-aminopropyltriethoxysilane in such a way which leads to forming of chemical bonds between polyimide and silicalite-1. Firstly polyimide chains were endcapped by this agent which subsequently enabled their reaction with groups naturally present on silicalite-1 surface. Membranes with silicalite-1 content up to 60 wt. % were prepared and characterized by SEM, light microscopy and permeation of gases, prevailingly of He. The accessibility of sililicalite-1 pores prior to embedding and after embedding into polymeric matrices was studied by an iodine indicator technique. The permeability of membranes for gases was measured using a semi-open permeation apparatus with a small volume. Helium permeability depended on filler content and increased monotonously with the increasing content of filler. There were, however, significant deviations of the permeability dependences on filler content from shapes predicted by Bruggeman’s model. The qualitative explanation of the data disagreement with the model was proposed based on a stratification of mixed matrix membranes found by SEM.

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31

Al-Akwaa, Shaaima. "Synthesis and New Characterization Method of Silicalite-1 Membranes for Gas Separation." Thesis, Université d'Ottawa / University of Ottawa, 2020. http://hdl.handle.net/10393/41577.

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Zeolite membranes have great potential in gas separation applications because of their unique selective properties. The main challenge is in synthesizing defect-free zeolite membranes. In this study, we synthesized silicalite-1 zeolite membranes on ceramic supports composed of Al2O3 and TiO2 using the pore-plugging method. We investigated the effect of the fill-level in the autoclave during the synthesis on the membrane performance. In particular, we were interested in determining the conditions at which the defects' contribution to the total transport is minimized. We adopted and further developed the approach proposed by Carter (2019) to quantify the permeance contribution through defects. Comparing the membrane performance before and after calcination, we proposed several modifications to the original analysis of Carter (2019). Knowing the defect transport contribution, we determined the corrected diffusivity, an intrinsic property of zeolite crystals at a given temperature, of several adsorbed gases on silicalite-1 crystals. The defect's contribution decreased as the autoclave fill-level increased from 94 to 98%. A further increase in the autoclave fill-level introduced more defects and caused the autoclave lid to rupture. Despite the differences in the membranes' performance arising from the autoclave fill-level, the corrected diffusivities of CO2, CH4, and N2 in silicalite-1 showed minimal variation from membrane to membrane. This proves the validity of the proposed characterization method. Moreover, the reported corrected diffusivities are comparable to the literature's values, found using other characterization methods. However, none of the previously used methods is as simple and straightforward as the one we further developed in this study.

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32

Carter, David. "Fabrication and Characterization of Silicalite-1 Membranes for the Separation of the Greenhouse Gases." Thesis, Université d'Ottawa / University of Ottawa, 2019. http://hdl.handle.net/10393/39524.

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Membranes composed of zeolite crystals, in which gas molecules are transported by surface diffusion, are promising for gas separation applications. Since this mode of mass transfer mechanism is controlled by synergistic adsorption and diffusion phenomena, the separation of gas mixtures is not solely dependent on molecular size. However, undesirable defect pathways in zeolite membranes are often present due to factors such as incomplete crystal growth and/or thermal stresses during membrane synthesis and calcination. These pathways cause molecules to bypass the selective zeolite crystal layer and adversely affect membrane performance. Since the fabrication of defect-free zeolite membranes is very challenging, their widespread adoption for industrial processes has been impeded. Quantification of defects in zeolite membranes is therefore important to improve synthesis protocols of these membranes. In this research, zeolite membranes composed of silicalite crystals have been fabricated using the pore plugging method, and their performance was evaluated by developing a method that can be used to describe the selective and non-selective channels that are present in any zeolite membrane. Unlike the other destructive and sophisticated methods, which already exist to discern this information, the proposed method requires only a limited number of in-situ permeation experiments to be conducted using He – a non-adsorbing gas, and N2 – an adsorbing gas. With this method, the volume fraction, effective length, and size of the selective and non-selective channels of multiple membranes have been quantified, and these parameters were used to predict membrane performance at untested conditions, as well as with untested gases such as CH4 and CO2. In addition, by separating surface diffusion from the flow through the defects in gas separation tests with CO2/N2 mixture, the respective transport diffusivities and exchange diffusivity coefficients, which account for mass transfer in zeolite crystals were determined using the Maxwell-Stefan model. These determined exchange diffusivity coefficients are not equal to each other and challenge the Vignes correlation. In addition, transport diffusivities determined in mixed gas permeation experiments at University of Ottawa have then been validated by large single crystal transport diffusivities for mixed gases that were determined from molecular uptake experiments conducted at University of Leipzig in Germany, using Infra-Red Micro-imaging.

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33

Robinson, Denis Joseph. "Catalytic oxidation reactions using titanium silicalite (TS-1) in conjunction with hydrogen peroxide." Thesis, University of Liverpool, 1998. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.367129.

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34

Carleen, Bradford J. "Hydrothermal Synthesis Process for the Production of Silicalite-1 Crystal Aggregate Packing Particles." Digital WPI, 2010. https://digitalcommons.wpi.edu/etd-theses/137.

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Methyl Tertiary-Butyl Ether (MTBE) contamination of groundwater and surface waters has become a relevant environmental and public safety concern in recent years. This anthropogenic compound is now persistent at low concentrations in several valuable ground and surface water locations within the United States due largely to the widespread production of MTBE for use as a fuel oxygenate in conjunction with negligent underground storage practices during the 1980's and 1990's. Though there are several treatment strategies for the remediation of MTBE spill sites, the most efficient strategy may be adsorption of MTBE by a packed column of silicalite-1 adsorbent. Effective adaption of this technology requires cheap production of silicalite-1 sorbent packing particles on the order of 3 millimeters diameter. This work entails the development of a new synthesis process which results in sufficient in-situ crystallization of silicalite-1 aggregates within a 3 millimeter spherical amorphous silica gel source. The crystal aggregates sizes can be tuned from 5 to 70 µm, depending on synthesis parameters, and the finished silicalite-1 aggregate particle takes the shape of the amorphous gel source. These aggregate particles, when containing a small amorphous core, should be suitable for packed adsorption column applications. Multiple hydrothermal synthesis experiments were performed by batch methods featuring silica gel spheres as the sole silica source for the batch. Zeolite nucleation and crystal growth were demonstrated throughout the amorphous bead. Synthesis parameters were optimized both for short synthesis times, optimal mechanical properties, and cost effectiveness. The influence of product crystal size on particle hardness was also investigated. The packing production process is sufficiently ready for supporting pilot scale adsorption studies.

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35

Gabry, Thomas Jacques Andre. "Simulation of the diffusion of endocrine disrupting compounds in silicalite by molecular dynamics." Digital WPI, 2012. https://digitalcommons.wpi.edu/etd-theses/341.

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In this thesis we investigated the separation of two endocrine disrupting chemicals (EDC), bisphenol-A (BPA) and nonylphenol (NP) from water over the defect free silicalite zeolite. Two force-fields were investigated, the OPLS-AA force-field which is an all-atom one, and the OPLS-UA force-field which is a united atom one. In order to be able to simulate BPA, we simulated and studied the diffusion of different molecules in silicalite. We compared two famous bulk water models, the non-rigid TIP3P modified for CHARMM model and the rigid SPC model, to literature and simulated the diffusion of these water molecules at temperatures from 300K to 600K. We found that these models coupled with our parameters for silicalite compared poorly with literature except for values calculated by Yazaydin et al. The mean-square displacements (MSDs) were more important in the x-direction (sinusoidal channel) than in the expected y-direction (straight channels) for both models resulting in small self-diffusion coefficient values. Results tended to improve as temperature increased. We believe that the high number of hydrogen bonds, implying the presence of clusters of water molecules, is responsible for the poor self-diffusion coefficient. The charges chosen to describe our silicalite zeolite, +2.05, may also be a reason of our small self-diffusion coefficient. We then investigated the self-diffusion of aromatic molecules at 300 and 400K. Benzene, phenol and toluene were studied. We found self-diffusion coefficients for benzene that did not compare well to experiments but that was close to simulation work done by Rungsirisakun et al. Our diffusion coefficients for benzene were several orders of magnitude bigger than the experimental values found in literature for both force-fields. The diffusion patterns for both phenol and toluene did not allow us to calculate self-diffusion coefficients for both investigated force-fields. We believe that the jumps in the MSDs of these molecules are due to the rotation that they undergo in the nanopores. Phenol anchors to the framework by hydrogen-bonds between the hydrogen of its alcohol group and the oxygen of the framework. The diffusion seems to happen when the alcohol group is in a line with one channel. The same diffusion phenomenon was seen for toluene molecule but was related to the methyl group attached to its benzene ring. When this group is in front of a channel, the energetic barrier is reduced and the molecule can diffuse through it. Finally bigger molecules were simulated and studied. Neopentane seemed to have a very low self-diffusion coefficient in silicalite if it could move at all. We report values of self-diffusion of 1.3 10-14 m2.s-1 at both 300K and 400K. This value seems a little high compared to benzene experimental self-diffusion coefficient values that are in the same order of magnitude at both temperatures. The linear nonylphenol molecule that we simulated seemed to diffuse through silicalite with patterns that were close to the one seen for phenol. The hydrogen bonding between its alcohol group and the framework slows down its diffusion in silicalite. With the same reasoning as for phenol we decided not to calculate diffusion coefficient for NP. The last molecule investigated was bisphenol-A (BPA). We found that BPA almost did not diffuse through silicalite. The size of the molecule can explain why it did not diffuse, but we believe that the angle between the two phenol groups should be able to bend enough for it to diffuse, slowly, through silicalite. Our conclusion is that the two phenol groups at both ends of the molecules are the most important factor in its very slow diffusion. Hydrogen bonding is taking place at both ends making it very hard for the molecule to move in the framework. We decided to generate self-diffusion coefficients for this molecule because the diffusion process did not have jumps. We found self-diffusion coefficient that are 3.10-15 m2.s-1 and 15. 10-15 m2.s-1 at 300 and 400K respectively for the OPLS-AA force-field, and 11.6.10-15 m2.s-1 and 6.68.10-15 m2.s-1 at 300 and 400K respectively for the OPLS-UA force-field. The last result was unexpected as we thought that the self-diffusion coefficient was going to increase with temperature. We believe that running much longer simulations for every molecule that we studied should give more reasonable and reliable results as the self-diffusion coefficients values are very small.

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36

Li, Qinghua. "Crystallization of colloidal TPA-silicalite-1 by a two-stage varying-temperature synthesis." Licentiate thesis, Luleå tekniska universitet, 2000. http://urn.kb.se/resolve?urn=urn:nbn:se:ltu:diva-17472.

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A novel synthesis method called a two-stage varying-temperature synthesis was developed for the investigation of kinetics and mechanism of the crystallization of discrete colloidal crystals of TPA-silicalite-1. Briefly, this method involves a rapid change in treatment temperature at some point during the crystallization. By extending the duration of the period at the initial synthesis temperature, the crystal concentration and final crystal size varied until they were approximately equal to those obtained for a complete synthesis at the initial temperature. At this point in the crystallization, it was concluded that the nucleation stage was completed. In the TPAOH-TEOS-H2O system, the nucleation was a continuous process and the rate of nucleation was initially high immediately after the start of hydrothermal treatment, but then exponentially declined throughout the nucleation period. In the TPAOH-SiO2-H2O-ethanol system, where SiO2 was colloidal amorphous silica, the nucleation was still a successive process, whereas the nucleation profile was more similar to that usually considered to occur during zeolite syntheses with an autocatalytic increase in the nucleation rate. When the synthesis conditions were identical, except for the silica source in the above two systems, the nucleation period for the TPAOH-SiO2-H2O-ethanol system was longer than that for the TPAOH-TEOS-H2O system. This was presumably due to the fact that the colloidal silica particles needed to depolymerize to reach a supersaturation concentration in order for nucleation and crystal growth to occur. Also, it was found that irrespective of silica sources, the vast majority of nucleation occurred during an induction period before linear crystal growth started. The two-stage synthesis method could also be used to produce particularly small colloidal crystals of TPA-siliclaite-1 with reduced synthesis times and high yields. Using this method involves starting a synthesis at a lower temperature and ending the synthesis at a higher temperature. After determining the nucleation stage, an elevated temperature can be used to accelerate the crystal growth and reach higher equilibrium yields controlled by the final temperature. The effects of temperature, dilution and alkalinity on the synthesis were studied to optimize syntheses. The effect of aging on the kinetics and mechanism for crystallization of colloidal TPA-silicalite-1 with varying silica source was also investigated with the two-stage synthesis procedure. With the TEOS silica source, aging for up to 15 days at room temperature had no significant effect on the nucleation and crystallization at a low synthesis temperature. Whereas with amorphous silica, aging caused the nucleation kinetics to become increasingly similar to those for syntheses with TEOS. Thus, with sufficient aging of more economical amorphous silica sources, the properties of the final products approached that with the more exotic TEOS silica source, viz., small colloidal crystals with a narrow crystal size distribution.
Godkänd; 2000; 20070318 (ysko)

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37

Gueudré, Laurent, Christian Chmelik, and Jörg Kärger. "Diffusion anisotropy in a single crystal of silicalite-1 studied by interference microscopy." Diffusion fundamentals 16 (2011) 45, S. 1-2, 2011. https://ul.qucosa.de/id/qucosa%3A13781.

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38

Petry, David P. "Silicalite Clear Sol Precursors Studied by NMR, Mass Spectrometry and Dynamic Light Scattering." Thesis, University of Manchester, 2010. http://ethos.bl.uk/OrderDetails.do?uin=uk.bl.ethos.525295.

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39

Gueudré, Laurent, Christian Chmelik, and Jörg Kärger. "Diffusion anisotropy in a single crystal of silicalite-1 studied by interference microscopy." Universitätsbibliothek Leipzig, 2015. http://nbn-resolving.de/urn:nbn:de:bsz:15-qucosa-185041.

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40

Chmelik, Christian, Lars Heinke, Jörg Kärger, Baten Jasper M. van, and Rajamani Krishna. "Diffusion of n-butane/iso-butane mixtures in silicalite-1 investigated using infrared microscopy." Universitätsbibliothek Leipzig, 2015. http://nbn-resolving.de/urn:nbn:de:bsz:15-qucosa-189481.

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41

Shin, Sang Baek. "Catalytic reaction engineering of propene epoxidation with hydrogen peroxide over titanium silicalite (TS-1)." Thesis, Imperial College London, 2011. http://hdl.handle.net/10044/1/6951.

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Propene oxide is an important chemical intermediate in the chemical industry. The propene oxide industry has employed two different types of commercial processes for several decades: the chlorohydrin process and the hydroperoxidation process. However, direct epoxidation of propene with hydrogen peroxide has recently attracted much attention as a more environmentally benign and profitable process. This thesis presents the catalytic reaction engineering of the epoxidation of propene to propene oxide using hydrogen peroxide as the oxidant and titanium silicalite (TS-1) as the catalyst under mild conditions. The kinetics of the heterogeneous catalytic epoxidation was studied in an autoclave reactor using methanol/water mixtures as the solvent. The effects of stirring speed, catalyst loading, reactant concentration, reaction temperature, solvent composition and solvent variation on the propene oxidation are presented and discussed. The catalytic performance of TS-1 impregnated with precious metal nanoparticles such as gold and palladium for the propene epoxidation was also investigated. The influences of the kind of precious metal and treatment process adopted in the catalyst preparation on the propene epoxidation and the hydrogen peroxide decomposition were explored. One of the key objectives of this research was to evaluate a new continuous reactor concept for propene epoxidation and other liquid-phase selective oxidation reactions. A conventional monolith and a confined Taylor flow (CTF) reactor were studied for the propene epoxidation. The influences of gas and liquid flow rates on the hydrodynamics of the structured reactors were investigated under Taylor flow regime at atmospheric pressure. It was found that the variation of hydrodynamics had a significant impact on the production of propene oxide. The effect of operating pressure on the propene oxide production was studied in a pressurised system. In addition, the performances of various structures of reactor column were examined to compare.

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42

Yip, Chi Kin. "A catalytic architecture composed of titanium silicalite-1 and nanostructured support for oxime synthesis /." View abstract or full-text, 2009. http://library.ust.hk/cgi/db/thesis.pl?CBME%202009%20YIP.

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43

Gueudré, Laurent. "Diffusion du cyclohexane dans la Silicalite-1 : Origine et caractérisation de la résistance de surface." Lyon, Ecole normale supérieure, 2010. http://www.theses.fr/2010ENSL0580.

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L’objectif de ce travail est d’étudier plus en détail la résistance au transfert de matière à la surface des solides microporeux, en mesurant les cinétiques d’adsorption sur le système cyclohexane/Silicalite-1 par thermogravimétrie. Afin de réaliser cette thèse, un soin particulier a été accordé à la synthèse de cristaux de Silicalite-1 de différentes tailles afin de dissocier la résistance de surface de la résistance diffusionnelle intracristalline. Ces synthèses ont été réalisées de manière à obtenir des cristaux de géométrie quasi sphérique et possédant une répartition de taille homogène. Le montage expérimental utilisé lors de ces travaux nous a permis d’obtenir des courbes de cinétiques de prise et de perte de masse dans différentes conditions de température, de pression partielle et pour ces cristaux de tailles différentes. Celui-ci est principalement constitué d’un saturateur permettant de vaporiser un adsorbat liquide à une pression partielle déterminée et d’une thermobalance composée de deux fours, l’un servant de référence et l’autre accueillant les échantillons. Bien que cette méthode expérimentale soit simple de part son principe, son utilisation s’est montrée particulièrement délicate du fait des très faibles variations de masse mesurées. Les résultats ont ensuite été exploités à l'aide d’un modèle tenant compte de la variation de diffusivité intracristalline avec le taux de remplissage et d’une résistance de surface représentée par un modèle de film situé dans le cristal. Les résultats expérimentaux nous ont permis de définir deux types de résistance de surface distincts, que nous avons nommée "résistance native" et "résistance évolutive". La première est présente dès la synthèse des cristaux, tandis que l’autre est dépendante de l’historique et de la méthode de synthèse des échantillons. La résistance évolutive peut être fortement réduite en lavant la surface des cristaux avec des solutions d'acide fluorhydrique, ce qui n'est pas le cas pour la surface native. En étudiant l'influence de différentes conditions opératoires (température, concentration, comparaison adsorption/désorption), nous avons pu proposer un mécanisme pour le transfert de matière à la surface des cristaux : les molécules s’adsorberaient sur la surface des cristaux depuis la phase fluide en suivant une isotherme d’adsorption favorable. L’adsorbat serait ensuite libre de diffuser sur la surface, avant de pénétrer dans les pores
The aim of this work is to study cyclohexane transfer resistance at the surface of Silicalite-1 crystals. To do so, cyclohexane uptake curves were performed on Silicalite-1 crystals using a classical gravimetric technique. In order to dissociate surface and microporous resistances, the experiments were performed on a wide range of crystals sizes. First of all, Silicalite-1 crystals of different sizes were synthesized. The synthesis conditions were optimized so as to obtain crystals of different sizes, quasi spherical, homogeneous in size. Next, uptake curves were recorded in different operating conditions, such as temperature and partial pressure. The results were interpreted using a simplified model, taking into account both the variation of the effective intracristalline diffusion with the adsorbent loading and the surface resistance, represented by a solid film. The results show that two different types of resistances can be found on the crystals surfaces. The first resistance, called "native resistance" is present as soon as the crystal is synthesised, whereas the other one, called "evolving resistance" is generated during the sample storage or during the adsorption experiments. The evolving resistance can be strongly reduced by washing the crystal surface with fluorhydric acid, which is not the case for the native resistance. It is therefore probable that the evolving resistance is due to a partial blockage of the pores due to an amorphization of the first crystal layers. By studying the influence of the different operating conditions (temperature, fluid phase concentration, adsorption vs. Desorption), we were able to propose a mechanism for the native resistance. Fluid phase molecules are first strongly adsorbed on the surface, as the surface adsorption isotherm is very favourable. The adsorbate then diffuses on the surface until it eventually penetrates into the microporosity

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44

Cheng, Chil-Hung. "High-silica zeolite nucleation from clear solutions." Texas A&M University, 2005. http://hdl.handle.net/1969.1/3273.

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Understanding the mechanism of zeolite nucleation and crystallization will enable the zeolite science community to tune zeolite properties during synthesis in order to accommodate the purposes of various applications. Thus there has been considerable research effort in "deciphering" the mechanism by studying the growth course of tetrapropylammonium (TPA)-mediated silicalite-1 using several techniques, such as dynamic light scattering (DLS), small-angle X-ray/neutron scattering (SAXS/SANS), and nuclear magnetic resonance (NMR). While these studies have generated a more comprehensive picture on the silicalite-1 growth mechanism, the general application of the mechanism and how it could be applied to other zeolite systems have not been addressed. This work initially tried to apply the insights developed from the TPAsilicalite- 1 clear solution synthesis by investigating the nanoparticles formation and zeolite growth in several tetraethyl orthosilicate (TEOS)-organocation-water solutions heated at 368 K using SAXS. The results are in contrast to TEOS-TPAOH-water mixtures that rapidly form silicalite-1 at 368 K. These results imply that the developed TPA-silicalite-1 nucleation and crystallization mechanism is not universally applicable to other zeolite systems and TPA-silicalite-1 itself could be a special case. With this in mind, the next goal of this work uses in situ SAXS to revisit silicalite-1 growth kinetics prepared by using several TPA-mimic organocations and some asymmetric geometry organocations. The results clearly show the TPA cation is an extraordinarily efficient structure-directing agent (SDA) due to its moderate hydrophobicity and perfect symmetric geometry. Any perturbation of the hydrophobicity and symmetry of SDA leads to a deterioration of zeolite growth. This work further investigates the influences of alcohol identity and content on silicalite-1 growth from clear solutions at 368 K using in situ SAXS. Several tetraalkyl orthosilicates (Si(OR)4, R = Me, Pr, and Bu) are used as the alternative silica sources to TEOS in synthesizing silicalite-1. Increasing the alcohol identity hydrophobicity or lowering the alcohol content enhances silicalite-1 growth kinetics. This implies that the alcohol identity and content do affect the strength of 1) hydrophobic hydration of the SDA and 2) the water-alcohol interaction, through changing the efficiency of the interchanges between clathrated water molecules and solvated silicate species.

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Huve, Joffrey. "Highly selective, active and stable Fischer-Tropsch catalyst using entrapped iron nanoparticles in silicalite-1." Thesis, Lyon, 2017. http://www.theses.fr/2017LYSE1042/document.

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L'intérêt pour la synthèse de Fischer-Tropsch (FTS) est d'actualité. Elle permet la conversion de matière première (biomasse) en combustible liquide. Comparés aux catalyseurs à base de cobalt, ceux à base de fer présentent une désactivation rapide, une activité et une sélectivité faibles en produisant une quantité non désirable de CO2. Après plusieurs décennies d'études, l'origine de ces défauts reste méconnue. Les catalyseurs classiques sont généralement fortement chargés en fer (>70 wt.%) et composés de nombreuses phases empêchant l'établissement d'une relation structure-activité. Il est nécessaire de développer des catalyseurs contenant du fer plus actifs, plus sélectifs et plus stables par une approche rationnelle. La synthèse de nanoparticules de taille contrôlée (3.5 nm) encapsulées dans les murs d'une silicalite-1 creuse (Fe@hollow-silicalite-1) est présentée. L'encapsulation empêche le frittage pendant la synthèse de Fischer-Tropsch, permettant de garder une bonne dispersion du fer. Contrairement aux autres catalyseurs, le catalyseur Fe@hollow-silicalite-1actif ne produit pas de CO2. L'hydrophobicité de la silicalite-1 est très certainement à l'origine de la non-production de CO2 par inhibition de la réaction directe du gaz à l'eau. On démontre que le catalyseur Fe@hollow-silicalite-1convertit le CO2 en CO par réaction du gaz à l'eau inversée (R-WGS). Afin d'établir une relation structure-activité, des catalyseurs à base de fer de taille bien contrôlée sont synthétisés et caractérisés (MET, in-situ XANES, in-situ Mössbauer). Deux catégories de TOF suivant la taille des particules, ~10-2 s-1 pour les plus larges (>20 nm) et ~10-3 s-1 pour les plus petites, sont observées
Fischer-Tropsch synthesis (FTS) is gaining renewed interests as it allows converting alternative feedstocks (biomass) into liquid fuels. Compared to Co-based catalysts, state of the art Fe catalysts show lower activity, faster deactivation and lower selectivity as it produces an undesirable amount of CO2. Despite decades of studies, the origins of low activity and selectivity and fast deactivation are still unclear. Typical Fe based catalysts are highly metal loaded (>70 wt.%) and composed of many different phases, which strongly impedes the establishment of structure-activity relationships. There is a need to develop more active, more selective and more stable iron FTS catalysts by rational approaches.The synthesis of well-controlled 3.5 nm iron nanoparticles encapsulated in the walls of a hollow-silicalite-1 zeolite (Fe@hollow-silicalite-1) is presented. The encapsulation prevents particle sintering under FTS conditions leading to a high and stable Fe dispersion. The catalyst Fe@hollow-silicalite-1 is active and highly selective in FTS. Most importantly, Fe@hollow-silicalite-1 does not produce CO2 in contrast to all other Fe-based catalysts. The strong hydrophobicity of the silicalite-1 is likely the origin of the lack of CO2 production by inhibition of the forward WGS reaction. We demonstrated that Fe@hollow-silicalite-1converts CO2 into CO by the reverse WGS reaction. In order to establish a structure-activity relationship, a series of Fe-based catalysts with well-controlled particle sizes were synthesized and characterized (TEM, in-situ XANES, in-situ Mössbauer, XRD). We observed two distinct categories of TOFs depending on the particle size, ~10-2 s-1 for larger (>20 nm) and ~10-3 s-1 for smaller ones

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46

Rimer, Jeffrey D. "Self-assembly of silica nanoparticles and their role in the mechanism of silicalite-1 crystallization." Access to citation, abstract and download form provided by ProQuest Information and Learning Company; downloadable PDF file, 302 p, 2007. http://proquest.umi.com/pqdlink?did=1253510461&Fmt=7&clientId=79356&RQT=309&VName=PQD.

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47

Chalhoub, Elie, and Dhananjai B. Shah. "Measurement of diffusivities of helium and argon in silicalite by static single crystal membrane technique." Universitätsbibliothek Leipzig, 2016. http://nbn-resolving.de/urn:nbn:de:bsz:15-qucosa-196430.

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48

Laloué, Nicolas, Catherine Laroche, and Hervé Jobic. "Concentration dependence of transport and corrected diffusivities of n-Hexane in silicalite measured by QENS." Universitätsbibliothek Leipzig, 2016. http://nbn-resolving.de/urn:nbn:de:bsz:15-qucosa-196598.

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49

Chalhoub, Elie, and Dhananjai B. Shah. "Measurement of diffusivities of helium and argon in silicalite by static single crystal membrane technique." Diffusion fundamentals 2 (2005) 85, S. 1-2, 2005. https://ul.qucosa.de/id/qucosa%3A14422.

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50

Laloué, Nicolas, Catherine Laroche, and Hervé Jobic. "Concentration dependence of transport and corrected diffusivities of n-Hexane in silicalite measured by QENS." Diffusion fundamentals 2 (2005) 98, S. 1-2, 2005. https://ul.qucosa.de/id/qucosa%3A14436.

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