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Selective hydrogenation/Oxidation of CVD graphene using AFM
Přikryl, Vojtěch ; Švarc, Vojtěch (referee) ; Bartošík, Miroslav (advisor)
Graphene is a perspective material for utilization in electronics due to its high charge carrier mobility. However, in order to be applicable in practice the bandgap opening is necessary. One way of achieving this is modification of graphene by hydrogenation or oxidation. This work concerns the possibility of using AFM for local hydrogenation/oxidation of graphene depending on the bias voltage between the tip and the sample. The presence of hydrogenation/oxidation was examined by Kelvin probe force microscopy and Raman spectroscopy. The possibility of oxidation was proved but hydrogenation was not proved.
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The optimization the production of selected medicinal substances
Fránek, Jan ; Ing.Oldrřich Smékal (referee) ; Omelková, Jiřina (advisor)
Mgr. Jan Fránek 2011: The optimization the production of selected medicinal substances The diploma thesis dealt with optimization of production of fingolimod by hydrogenation. During the optimization of production, there was reduction of benzylic hydroxygroup and nitrogroup of nitrofingotriol. Reduction of two different groups caused dividing process of hydrogenation into two phases. The original intention was to optimize production only in the autoclave, but the need of using acidic catalytical medium in first phase led to dividing the production into reduction in the reactor and following catalyzed hydrogenation, already in neutral conditions, in the autoclave. The way of preparation of active substance by using an autoclave had not been explored in detail before. Evaluation of optimization is a part of results. There are also production charges on pilot plant included in results. Because the results of procedure of the pilot unit were not uniform, it was necessary to continue in optimization even after finishing the production in pilot plant. Following procedure modified according to the latest experiments was passed to the operating process.
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Study of selective hydrogenation using KPFM
Zeman, Filip ; Konečný, Martin (referee) ; Bartošík, Miroslav (advisor)
The bachelor thesis deals with the possibilities of selective hydrogenation of graphene and their analysis. The theoretical part deals with the properties of carbon materials and different hydrogenation methods. Furthermore, it thoroughly describes the raster probe microscopy AFM and KPFM. The last part of the theory discusses a suitable method to analyze hydrogenated graphene, namely Raman spectroscopy. The results that have already been observed in previous research are discussed. In the experimental part, three methods for producing hydrogenated graphene samples are described, which are measured using KPFM and Raman spectroscopy. Finally, their results are compared.
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Synthesis of ligands and reductive coupling catalysts
Žáková, Andrea ; Hulla, Martin (advisor) ; Schulz, Jiří (referee)
This thesis investigates Frustrated Lewis pair hydrogenation catalysts for the use in reductive amination reactions. A series of tin complexes using Schiff base ligands was synthetized. Their ability to act as Lewis acids in Frustrated Lewis pair catalysis was disclosed by series of experiment including Gutmann Beckett method, H2 activation using high pressure NMR measurements and hydrogenation catalytic testing. Synthetized ditriflate and monotriflate complexes were proven to reversibly activate H2 at room temperature and 60 řC respectively. All of the synthetized compounds successfully mediated imine hydrogenation confirming Frustrated Lewis pairs catalysis.
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Aplications of hydrogenation catalysts prepared by reductive demetalation of zeolites
Kurucová, Svetlana ; Přech, Jan (advisor) ; Vyskočilová, Eliška (referee)
Hydrogenation reactions belong to the most important reactions in the chemical industry. They are needed for crude oil processing, production of pharmaceutical, polymers, chemical specialties, etc. Supported noble metal catalysts are commonly used industrial catalysts due to their high activity and selectivity. However, the high cost of production and recovery of noble metal catalysts is one of the disadvantages of their use. The application of transition metal catalysts containing Cu, Fe or Zn presents a more environmentally friendly alternative to currently used catalysts. In this work, we studied the catalytic activity of metal@zeolite composite catalysts containing CuFe and CuZn bimetallic nanoparticles, prepared by reductive demetallation in hydrogenation of -NO2, -C≡C-, -C=C- and -C=O groups. Reductive demetallation is a novel method for the synthesis of bimetallic nanoparticles encapsulated inside zeolite pores. The catalytic activity of the metal@zeolite composites prepared by reductive demetallation was compared with analogues synthesised by impregnation and ion exchange in the hydrogenation of p-nitrotoluene, 3-ethynylanisole and cinnamaldehyde. Metal@zeolite catalysts synthesised by reductive demetallation were active in the hydrogenation of all the cited groups: -NO2, -C≡C-, -C=C- and...
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Preparation of organocatalysts derived from monosaccharides
Nekvinda, Jan ; Veselý, Jan (advisor) ; Trnka, Tomáš (referee)
This bachelor thesis is focused on the synthesis of organocatalysts derived from monosaccharides, in particular D-glucose and D-glucosamine, with various protecting groups. Synthesis of various thiourea catalysts and the attempt to prepare new squaramide catalysts is described. ABSTRAKT Tato bakalářská práce je zaměřena na syntézu organokatalyzátorů odvozených od monosacharidů, zejména z D-glukózy a D-glukosaminu, s různými chránícími skupinami. Dále je popsána syntéza různých thiomočovinových katalyzátorů a pokus o přípravu katalyzátoru obsahující derivát kyseliny čtvercové.
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Preparation and properties of building blocks of specialty polymers
Šichová, Kristýna
This Diploma Thesis presents results obtained by solution of two partial projects: a) Preparation of monomers from renewable sources using metathesis and tandem hydrogenation catalyzed with ruthenium compounds - project solved during my Erasmus stay at the Université de Rennes 1 in France; b) Preparation and properties of ,-bis(tpy)quarterthiophene oligomers carrying ionic side groups as oligomonomers for polyelectrolyte conjugated dynamers - project solved at the Department of Physical and Macromolecular Chemistry, Faculty of Science, Charles University in Prague. Project a): Self-metathesis of 1,2-epoxyhex-5-ene (but-3-enyloxirane) and its cross-metathesis with methyl acrylate and acrylonitrile catalyzed with ruthenium compounds as well as tandem design of these metatheses and consecutive hydrogenation of their products by gaseous hydrogen have been optimized. The following influences have been studied and tuned: (i) type of the catalyst (Grubbs, Hoveyda, Zhan) and its concentration and method of dosing, (ii) concentration of reactants and additives, (iii) type of solvent, and (iv) reaction temperature. Reactions were monitored by the GC, GC and MS methods and the products were characterized by the NMR method. Methyl 6,7-epoxyheptanoate (methyl 5-oxiranylpentanoate) obtained by the tandem...
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Preparation of optically pure compounds by stereoslective hydrogenation in a microreactor
Jaklová, Natalie ; Klusoň, Petr (advisor) ; Paterová, Iva (referee)
This bachelor Thesis is introducing an alternative approach to the synthesis of the pharmaceutically important compound (R)-4-chloro-3-hydroxybutyrate ((R)-CHBE). This compound is used as a precursor in the production of pharmaceutically valuable products, such as L-carnitine, (R)-4-amino-3-hydroxybutyric acid and (R)-4-hydroxy-pyrrolidone. At present time these chemicals are predominantly produced by using biochemical methods largely based on enyzmatic reactions in the presence of stereoselective carbonyl reductases. In this Thesis a new approach is described, which is based on stereoselective hydrogenation of ethyl-4-chloracetoacetate catalyzed by an optically pure ruthenium bis(phosphine) complex. The whole process was carried out in a microfluidic reactor system. This assembly is highly promising for a potential scale-up, studies of reaction kitetics, optimization of reaction and process conditions etc. For the reaction described above the optimal reaction conditions, such as temperature, pressure, solvent phase composition and flow rates of gas and liquid phases, were determined. Furthermore, the use of a suitable ionic liquid preserving the catalyst's chiral selectivity was described. Key words: (R)-4-chloro-3-hydroxybutyrate, L-carnitine, microfluid chip reactor, hydrogenation
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Preparation and properties of building blocks of specialty polymers
Šichová, Kristýna
This Diploma Thesis presents results obtained by solution of two partial projects: a) Preparation of monomers from renewable sources using metathesis and tandem hydrogenation catalyzed with ruthenium compounds - project solved during my Erasmus stay at the Université de Rennes 1 in France; b) Preparation and properties of ,-bis(tpy)quarterthiophene oligomers carrying ionic side groups as oligomonomers for polyelectrolyte conjugated dynamers - project solved at the Department of Physical and Macromolecular Chemistry, Faculty of Science, Charles University in Prague. Project a): Self-metathesis of 1,2-epoxyhex-5-ene (but-3-enyloxirane) and its cross-metathesis with methyl acrylate and acrylonitrile catalyzed with ruthenium compounds as well as tandem design of these metatheses and consecutive hydrogenation of their products by gaseous hydrogen have been optimized. The following influences have been studied and tuned: (i) type of the catalyst (Grubbs, Hoveyda, Zhan) and its concentration and method of dosing, (ii) concentration of reactants and additives, (iii) type of solvent, and (iv) reaction temperature. Reactions were monitored by the GC, GC and MS methods and the products were characterized by the NMR method. Methyl 6,7-epoxyheptanoate (methyl 5-oxiranylpentanoate) obtained by the tandem...
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Preparation and properties of building blocks of specialty polymers
Šichová, Kristýna ; Svoboda, Jan (advisor) ; Sedláček, Jan (referee)
This Diploma Thesis presents results obtained by solution of two partial projects: a) Preparation of monomers from renewable sources using metathesis and tandem hydrogenation catalyzed with ruthenium compounds - project solved during my Erasmus stay at the Université de Rennes 1 in France; b) Preparation and properties of ,-bis(tpy)quarterthiophene oligomers carrying ionic side groups as oligomonomers for polyelectrolyte conjugated dynamers - project solved at the Department of Physical and Macromolecular Chemistry, Faculty of Science, Charles University in Prague. Project a): Self-metathesis of 1,2-epoxyhex-5-ene (but-3-enyloxirane) and its cross-metathesis with methyl acrylate and acrylonitrile catalyzed with ruthenium compounds as well as tandem design of these metatheses and consecutive hydrogenation of their products by gaseous hydrogen have been optimized. The following influences have been studied and tuned: (i) type of the catalyst (Grubbs, Hoveyda, Zhan) and its concentration and method of dosing, (ii) concentration of reactants and additives, (iii) type of solvent, and (iv) reaction temperature. Reactions were monitored by the GC, GC and MS methods and the products were characterized by the NMR method. Methyl 6,7-epoxyheptanoate (methyl 5-oxiranylpentanoate) obtained by the tandem...
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