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Faculty / Organisational entity
- Kaiserslautern - Fachbereich Mathematik (8)
- Kaiserslautern - Fachbereich Maschinenbau und Verfahrenstechnik (5)
- Kaiserslautern - Fachbereich Informatik (3)
- Kaiserslautern - Fachbereich Chemie (2)
- Kaiserslautern - Fachbereich Elektrotechnik und Informationstechnik (2)
- Kaiserslautern - Fachbereich ARUBI (1)
- Kaiserslautern - Fachbereich Biologie (1)
The main focus of this dissertation is the synthesis and characterization of more recent zeolites with different pore architectures. The unique shape-selective properties of the zeolites are important in various chemical processes and the new zeolites containing novel internal pore architectures are of high interest, since they could lead to further improvement of existing processes or open the way to new applications. This dissertation is organized in the following way: The first part is focused on the synthesis of selected recent zeolites with different pore architectures and their modification to the acidic and bifunctional forms. The second part comprises the characterization of the physicochemical properties of the prepared zeolites by selected physicochemical methods, viz. powder X-ray diffractometry (XRD), N2 adsorption, thermogravimetric analysis (TGA/DTA/MS), ultraviolet-visible (UV-Vis) spectroscopy, atomic absorption spectroscopy (AAS), infrared (IR) spectroscopy, scanning electron microscopy (SEM), 27Al and 29Si magic angle spinning nuclear magnetic resonance (MAS NMR) spectroscopy, temperature-programmed reduction (TPR), temperature-programmed desorption of pyridine (pyridine TPD) and adsorption experiments with hydrocarbon adsorptives. The third part of this work is devoted to the application of test reactions, i.e., the acid catalyzed disproportionation of ethylbenzene and the bifunctional hydroconversion of n-decane, to characterize the pore size and architecture of the prepared zeolites. They are known to be valuable tools for exploring the pore structure of zeolites. Finally, an additional test, viz. the competitive hydrogenation of 1-hexene and 2,4,4-trimethyl-1-pentene, has been applied to probe the location of noble metals in medium pore zeolite. The synthesis of the following zeolite molecular sieves was successfully performed in the frame of this thesis (they are ranked according to the largest window size in the respective structure): • 14-MR pores: UTD-1, CIT-5, SSZ-53 and IM-12 • 12-MR pores: ITQ-21 and MCM-68 • 10-MR pores: SSZ-35 and MCM-71 All of them were obtained as pure phase (except zeolite MCM-71 with a minor impurity phase that is hardly to avoid and also present in samples shown in the patent literature). The synthesis conditions are very critical with respect to the formation of the zeolite with a given structure. In this work, the recommended synthesis recipes are included. Among the 14-MR zeolites, the aluminosilicates UTD-1 (nSi/nAl = 28), CIT-5 (nSi/nAl = 116) and SSZ-53 (nSi/nAl = 55) with unidimensional extra-large pore opening formed from 14-MR rings exhibit promising catalytic properties with high thermal stability and they possess strong Brønsted-acid sites. By contrast, the germanosilicate IM-12 with a structure containing 14-MR channels intersecting with 12-MR channels is unstable toward moisture. It was found that UTD-1 and SSZ-53 zeolites are highly active catalysts for the acid catalyzed disproportionation of ethylbenzene and n-decane hydroconversion due to their high Brønsted acidity. To explore their pore structures, the applied two test reactions suggest that UTD-1, CIT-5 and SSZ-53 zeolites contain a very open pore system (12-MR or larger pore systems) because the product distributions are not hampered by too small pores. ITQ-21, a germanoaluminosilicate zeolite with a three-dimensional pore system and large spherical cages accessible through six 12-MR windows, can be synthesized with nSi/nAl ratios between 27 and >200. It possesses a large amount of Brønsted-acid sites. The aluminosilicate zeolite MCM-68 (nSi/nAl = 9) is an extremely active catalyst in the disproportionation of ethylbenzene and in the n-decane hydroconversion. This is due to the presence of a high density of strong Brønsted-acid sites in its structure. The disproportionation of ethylbenzene suggests that MCM-68 is a large pore (i.e., at least 12-MR) zeolite, in agreement with its crystallographic structure. In the hydroconversion of n-decane, the presence of tribranched and ethylbranched isomers and a high isopentane yield of 58 % in the hydrocracked products suggest the presence of large (12-MR) pores in its structure. By contrast, a relatively high value for CI* (modified constraint index) of 2.9 suggests the presence of medium (10-MR) pores in its structure. As a whole, the results are in-line with the crystallographic structure of MCM-68. SSZ-35, a 10-MR zeolite, can be synthesized in a broad range of nSi/nAl ratios between 11 and >500. This zeolite is interesting in terms of shape selectivity resulting from its unusual pore system having unidimensional channels alternating between 10-MR windows and large 18-MR cages. This thermally very stable zeolite contains both, strong Brønsted- and strong Lewis-acid sites. The disproportionation of ethylbenzene classifies SSZ-35 as a large pore zeolite. In the hydroconversion of n-decane, the suppression of bulky ethyloctanes and propylheptane clearly suggests the presence of 10-MR sections in the pore system. By contrast, the low CI* values of 1.2-2.3 and the high isopentane yields of 56-60 % in the hydrocracked products suggest that SSZ-35 also possesses larger intracystalline voids, i.e., the 18-MR cages. The results from the catalytic characterization are in good agreement with the crystallographic structure of zeolite SSZ-35. It was also found that the nSi/nAl ratio influences the crystallite size and therefore the external surface area. As a consequence, product selectivities are also influenced: The lowest nSi/nAl ratio or the smallest crystallite size sample produces larger amounts of the relatively bulky products. The formation of these products probably results from the higher conversion or they are preferentially formed on the external surface area of the catalyst. Zeolite MCM-71 (nSi/nAl = 8) possesses an extremely thermally stable structure and contains a high concentration of Brønsted-acid sites. Its structure allows for the separation of n-alkanes from branched alkanes by selective adsorption. MCM-71 exhibits unique shape-selective properties towards the product distribution in ethylbenzene disproportionation, which is different to those obtained in the medium pore SSZ-35 zeolite. All reaction parameters are fulfilled to classify MCM-71 as medium pore zeolite and this is in good agreement with its reported structure consisting of two-dimensional network of elliptical 10-MR channels and an orthogonal sinusoidal 8-MR channels. The competitive hydrogenation of 1-hexene and 2,4,4-trimethyl-1-pentene was exploited to probe that the major part of the noble metal is located inside the intracrystalline void volume of the medium pore zeolite SSZ-35.
Wireless Sensor Networks (WSN) are dynamically-arranged networks typically composed of a large number of arbitrarily-distributed sensor nodes with computing capabilities contributing to –at least– one common application. The main characteristic of these networks is that of being functionally constrained due to a scarce availability of resources and strong dependence on uncontrollable environmental factors. These conditions introduce severe restrictions on the applicability of classic real-time methods aiming at guaranteeing time-bounded communications. Existing real-time solutions tend to apply concepts that were originally not conceived for sensor networks, idealizing realistic application scenarios and overlooking at important design limitations. This results in a number of misleading practices contributing to approaches of restricted validity in real-world scenarios. Amending the confrontation between WSNs and real-time objectives starts with a review of the basic fundamentals of existing approaches. In doing so, this thesis presents an alternative approach based on a generalized timeliness notion suitable to the particularities of WSNs. The new conceptual notion allows the definition of feasible real-time objectives opening a new scope of possibilities not constrained to idealized systems. The core of this thesis is based on the definition and application of Quality of Service (QoS) trade-offs between timeliness and other significant QoS metrics. The analysis of local and global trade-offs provides a step-by-step methodology identifying the correlations between these quality metrics. This association enables the definition of alternative trade-off configurations (set points) influencing the quality performance of the network at selected instants of time. With the basic grounds established, the above concepts are embedded in a simple routing protocol constituting a proof of concept for the validity of the presented analysis. Extensive evaluations under realistic scenarios are driven on simulation environments as well as real testbeds, validating the consistency of this approach.
In robotics, information is often regarded as a means to an end. The question of how to structure information and how to bridge the semantic gap between different levels of abstraction in a uniform way is still widely regarded as a technical issue. Ignoring these challenges appears to lead robotics into a similar stasis as experienced in the software industry of the late 1960s. From the beginning of the software crisis until today, numerous methods, techniques, and tools for managing the increasing complexity of software systems have evolved. The attempt to transfer several of these ideas towards applications in robotics yielded various control architectures, frameworks, and process models. These attempts mainly provide modularisation schemata which suggest how to decompose a complex system into less complex subsystems. The schematisation of representation and information flow however is mostly ignored. In this work, a set of design schemata is proposed which is embedded into an action/perception-oriented design methodology to promote thorough abstractions between distinct levels of control. Action-oriented design decomposes control systems top-down and sensor data is extracted from the environment as required. This comes with the problem that information is often condensed in a premature fashion. That way, sensor processing is dependent on the control system design resulting in a monolithical system structure with limited options for reusability. In contrast, perception-oriented design constructs control systems bottom-up starting with the extraction of environment information from sensor data. The extracted entities are placed into structures which evolve with the development of the sensor processing algorithms. In consequence, the control system is strictly dependent on the sensor processing algorithms which again results in a monolithic system. In their particular domain, both design approaches have great advantages but fail to create inherently modular systems. The design approach proposed in this work combines the strengths of action orientation and perception orientation into one coherent methodology without inheriting their weaknesses. More precisely, design schemata for representation, translation, and fusion of environmental information are developed which establish thorough abstraction mechanisms between components. The explicit introduction of abstractions particularly supports extensibility and scalability of robot control systems by design.
A number of natural products are known that contain an enamide as a key structural feature. This functionality is a very important subunit in various biologically active products and pharmaceutical drug lead compounds. In addition, enamides serve as highly versatile synthetic intermediates, particularly in the pericyclic reaction, formation of heterocycles, cross-coupling and in asymmetric synthesis. As a result, several protocols have been devised for the preparation of enamides. Traditional syntheses include condensation of aldehydes and ketones with amides or from hydroxylamines and acetic anhydride, require harsh conditions and yield mixtures of E/Z products. Several metal catalyzed approaches have been also investigated, such as isomerization of N-allylamides and catalytic cross-coupling of amides with vinyl halides or pseudohalides. These protocols proceed under milder conditions but suffer from the limited availability of these starting materials. The research described in this dissertation focuses on efficient and atom-economic preparation of enamides and thioenamides, using readily available starting materials. We developed catalyst systems generated in situ from bis(2-methallyl)-cycloocta-1,5-diene-ruthenium(II), phosphines and Lewis acid or base, efficiently catalyze the addition of primary amides and thioamides to terminal alkynes with exclusive formation of the anti-Markovnikov products in high yield and stereoselectivity under mild reaction conditions. The generality of the newly developed methodologies is demonstrated by common functional group tolerance. Furthermore, Markovnikov products were formed via phosphine-catalyzed addition of cyclic amides to phenylacetylene derivatives. The hydroamidation protocol of primary amides was successfully used in the synthesis of naturally occurring compounds, such as alatamide, lansiumamide A, botryllamides C and E, and the key intermediate in the synthesis of aristolactam. In order to investigate the reaction mechanism, the addition of various amides and carboxylic acids to terminal alkynes was performed using deuterium labeled starting materials and followed by in situ NMR and GC-MS studies.
We tackle the problem of obtaining statistics on content and structure of XML documents by using summaries which may provide cardinality estimations for XML query expressions. Our focus is a data-centric processing scenario in which we use a query engine to process such query expressions. We provide three new summary structures called LESS (Leaf-Element-in-Subtree), LWES (Level-Wide Element Summarization), and EXsum (Element-centered XML Summarization) which are targeted to base an estimation process in an XML query optimizer. Each of these collects structural statistical information of XML documents, and the latter (EXsum) gathers, in addition, statistics on document content. Estimation procedures and/or heuristics for specic types of query expressions of each proposed approach are developed. We have incorporated and implemented our proposals in XTC, a native XML database management system (XDBMS). With this common implementation base, we present an empirical and comparative study in which our proposals are stressed against others published in the literature, which are also incorporated into the XTC. Furthermore, an analysis is made based on criteria pertinent to a query optimizer process.
A classical conjecture in the representation theory of finite groups, the McKay conjecture, states that for any finite group and prime number p the number of complex irreducible characters of degree prime to p is equal to the number of complex irreducible characters of degree prime to p of the normalizer of a p-Sylow subgroup. Recently a reduction theorem was proved by Isaacs, Malle and Navarro: If all simple groups are “good”, then the McKay conjecture holds. In this work we are concerned with the problem of goodness for finite groups of Lie type in their defining characteristic. A simple group is called “good” if certain equivariant bijections between the involved character sets exist. We present a structural approach to the construction of such a bijection by utilizing the so-called “Steinberg-Map”. This yields very natural bijections and we prove most of the desired properties.
This thesis deals with the numerical study of multiscale problems arising in the modelling of processes of the flow of fluid in plain and porous media. Many of these processes, governed by partial differential equations, are relevant in engineering, industry, and environmental studies. The overall task of modelling and simulating the filtration-related multiscale processes becomes interdisciplinary as it employs physics, mathematics and computer programming to reach its aim. Keeping the challenges in mind, the main focus is to overcome the limitations of accuracy, speed and memory and to develop novel efficient numerical algorithms which could, in part or whole, be utilized by those working in the field of porous media. This work has essentially four parts. A single grid basic algorithm and a corresponding parallel algorithm to solve the macroscopic Navier-Stokes-Brinkmann model is discussed. An upscaling subgrid algorithm is derived and numerically tested for the same model. Moving a step further in the line of multiscale methods, an iterative Mutliscale Finite Volume (iMSFV) method is developed for the Stokes-Darcy system. Additionally, the last part of the thesis deals with ways to incorporate changes occurring at different (meso) scale level. The flow equations are coupled with the Convection-Diffusion-Reaction (CDR) equation, which models the transport and capturing of particle concentrations. By employing the numerical method for the coupled flow and transport problem, we understand the interplay between the flow velocity and filtration.
The aim of this study is to describe the consolidation in thermoplastic tape placement
process to obtain high quality structure, making the process viable for automotive
and aerospace industrial applications. The major barrier in this technique is very
short residence time of material under the consolidation roller to accomplished complete
polymer diffusion in the bonded region. Hence investigation is performed to find
out the optimize manufacturing parameters by extensive material, process, product
testing and through process simulation.
Temperature distribution and convective heat transfer under the hot gas torch is experimentally
mapped out. Bonding process inside the laminate is the combine effect
of layers (tapes) intimate contact Dic development and resulting polymer diffusion Dh
at these contacted sections. Three energy levels are identified based on the process
velocity and hot gas flow combinations. For the low energy parameter combinations,
the energy input to the incoming tape and substrate material is limited and result in
incomplete intimate contact which restricts the bonding process. On other hand high
energy input although could increase the bonding degree Db even up to the 97%, but
also activate the thermal degradation phenomena. It is found out that the rate of polymer
healing (diffusion) and polymer crosslinking follows the Arrhenius laws with the
activation energies of 43 KJ/mol and 276 KJ/mol. The polymer crosslinking at high
temperature exposure hinder the polymer diffusion process and reduces the strength
development. So the parameters combination at intermediate energy level provides
the opportunity of continuous interlaminar strength improvement through out the layup
process.
Deformation of tape edges is identified as the dictating factor for the laminate’s transverse
strength. Tape placement with slight overlap reinforced the transverse joint by
more 10 % as compared to pure matrix joint. Finally the simulation tool developed in
this research work is used for identifying the existing limitation to achieve full consolidation.
A parameter study shows that extended consolidation either by mean of additional
pass or by increasing consolidation length widens the high strength (over 90%)
bonding degree Db contour. Thus high lay-up velocity (up to 7 m/min) is viable for industrial
production rate.
Mrázek et al. [25] proposed a unified approach to curve estimation which combines localization and regularization. Franke et al. [10] used that approach to discuss the case of the regularized local least-squares (RLLS) estimate. In this thesis we will use the unified approach of Mrázek et al. to study some asymptotic properties of local smoothers with regularization. In particular, we shall discuss the Huber M-estimate and its limiting cases towards the L2 and the L1 cases. For the regularization part, we will use quadratic regularization. Then, we will define a more general class of regularization functions. Finally, we will do a Monte Carlo simulation study to compare different types of estimates.
This thesis deals with the solution of special problems arising in financial engineering or financial mathematics. The main focus lies on commodity indices. Chapter 1 addresses the important issue for the financial engineering practice of developing well-suited models for certain assets (here: commodity indices). Descriptive analysis of the Dow Jones-UBS commodity index compared to the Standard & Poor 500 stock index provides us with first insights of some features of the corresponding distributions. Statistical tests of normality and mean reversion then helps us in setting up a model for commodity indices. Additionally, chapter 1 encompasses a thorough introduction to commodity investment, history of commodities trading and the most important derivatives, namely futures and European options on futures. Chapter 2 proposes a model for commodity indices and derives fair prices for the most important derivatives in the commodity markets. It is a Heston model supplemented with a stochastic convenience yield. The Heston model belongs to the model class of stochastic volatility models and is currently widely used in stock markets. For the application in the commodity markets the stochastic convenience yield is included in the drift of the instantaneous spot return process. Motivated by the results of chapter 1 it seems reasonable to model the convenience yield by a mean reverting Ornstein-Uhlenbeck process. Since trading desks only apply and consider models with closed form solutions for options I derive such formulas for commodity futures by solving the corresponding partial differential equation. Additionally, semi-closed form formulas for European options on futures are determined. The Cauchy problem with respect to these options is more challenging than the first one. A solution can be provided. Unlike equities, which typically entitle the holder to a continuing stake in a corporation, commodity futures contracts normally specify a certain date for the delivery of the underlying physical commodity. In order to avoid the delivery process and maintain a futures position, nearby contracts must be sold and contracts that have not yet reached the delivery period must be purchased (so called rolling). Optimal trading days for selling and buying futures are determined by applying statistical tests for stochastic dominance. Besides the optimization of the rolling procedure for commodity futures we dedicate ourselves in chapter 3 with the optimization of the weightings of the commodity futures that make up the index. To this end, I apply the Markowitz approach or mean-variance optimization. The mean-variance optimization penalizes up-side and down-side risk equally, whereas most investors do not mind up-side risk. To overcome this, I consider in the next step other risk measures, namely Value-at-Risk and Conditional Value-at-Risk. The Conditional Value-at-Risk is generalized to discontinuous cumulative distribution functions of the loss. For continuous loss distributions, the Conditional Value-at-Risk at a given confidence level is defined as the expected loss exceeding the Value-at-Risk. Loss distributions associated with finite sampling or scenario modeling are, however, discontinuous. Various risk measures involving discontinuous loss distributions shall be introduced and compared. I then apply the theoretical results to the field of portfolio optimization with commodity indices. Furthermore, I uncover graphically the behavior of these risk measures. For this purpose, I consider the risk measures as a function of the confidence level. Based on a special discrete loss distribution, the graphs demonstrate the different properties of these risk measures. The goal of the first section of chapter 4 is to apply the mathematical concept of excursions for the creation of optimal highly automated or algorithmic trading strategies. The idea is to consider the gain of the strategy and the excursion time it takes to realize the gain. In this section I calculate formulas for the Ornstein-Uhlenbeck process. I show that the corresponding formulas can be calculated quite fast since the only function appearing in the formulas is the so called imaginary error function. This function is already implemented in many programs, such as in Maple. My main contribution of this topic is the optimization of the trading strategy for Ornstein-Uhlenbeck processes via the Banach fixed-point theorem. The second section of chapter 4 deals with statistical arbitrage strategies, a long horizon trading opportunity that generates a riskless profit. The results of this section provide an investor with a tool to investigate empirically if some strategies (for example momentum strategies) constitute statistical arbitrage opportunities or not.