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Sustainable processing of materials using supercritical fluids : doktorska disertacija
Dragana Borjan, 2022, doktorska disertacija

Opis: Supercritical fluids (SCFs) are powerful solvents with many unique properties. They have great potential for many processes, from extraction to chemical reactions and recycling. Accordingly, phase equilibrium data and thermodynamic and transport properties measurements in systems with a supercritical phase, as well as reliable and versatile mathematical models of the phase equilibrium thermodynamics, are needed for the process design and economic feasibility studies. The dissertation focuses on the benefits of supercritical fluid technology and consists of three main sections. The first section includes studies of the phase equilibria of the binary gas-alcohol and gas-urea derivatives. The influence of pressure and temperature on the system behaviour (solubility, viscosity, density, interfacial tension, melting point curve) was investigated. Most of the experiments were carried out with a high-pressure optical view cell, with minor modifications of the apparatus and measurement principle to determine mentioned thermodynamic and transport properties. The second part of the dissertation deals with the recovery of extracts from natural materials. Special interest is oriented towards supercritical fluid extracts, characterised by strong biological activities, especially antimicrobial and antioxidant properties. Supercritical fluid extraction has been performed on a semi-continuous apparatus (at pressures of 150 bar and 250 bar and temperatures of 313.15 K and 333.15 K for oregano extraction; and at pressures of 100 bar and 300 bar and temperatures of 313.15 K and 333.15 K for red beetroot extraction) and various methods such as the microdilution method and the DPPH method were used to determine antimicrobial and antioxidant activity. In the third part, an overview of different methods for recycling carbon fibre reinforced composites is given, including chemical recycling with supercritical fluids. This field has not been well explored, and the approach is relatively new but very interesting from a sustainable point of view. For an economically feasible process design, the thermodynamic and mass transfer data have to be determined. The principles of the future lab- and pilot-scale operations demand these supporting data be known. The results obtained in the frame of this study represent the high added value in the scientific field. They are essential to design and modify processes that yield products that cannot be achieved with conventional production processes.
Ključne besede: supercritical fluids, alcohols, urea, phase equilibria, viscosity, density, interfacial tension, modified capillary method, isolation methods, supercritical fluid extraction, pharmacological activity, carbon fiber reinforced composites, recycling techniques
Objavljeno v DKUM: 11.10.2022; Ogledov: 304; Prenosov: 63
.pdf Celotno besedilo (4,64 MB)

Muhammad Ali, 2021, doktorska disertacija

Opis: In this thesis, we study the structure and optical transmission properties of the twist-bend nematic liquid crystalline phase, made of bent dimers, confined in thin planar cells. Confinement leads to the formation of a periodic modulated structure, the formation of which is explained as follows. The twist-bend nematic phase is characterized by a heliconical modulation of the molecular long axes. Due to a short pitch of modulation (approximately 10 nm), the twist-bend nematic phase behaves as a pseudo-layered medium. At temperatures below the nematic – twist-bend nematic phase transition, the heliconical pitch and thus the thickness of the pseudo-layers reduces, which leads to a two-dimensional undulation of pseudo-layers in the direction perpendicular to the cell surfaces and along the surfaces. The undulated structure is responsible for a stripe texture observed under a polarizing microscope and acts as a diffraction grating. We constructed theoretical models to predict the pseudo-layer structure of a confined twist-bend nematic phase and to describe the properties of light diffracted on such cells. The free energy of the two-dimensional pseudo-layer structure of the twist-bend nematic phase is expressed in terms of the nematic director field, by which we describe the direction of the heliconical axis, and a complex smectic order parameter, the gradient of which gives the direction of the layer normal. At first, we assume that pseudo-layers are perpendicular to the surfaces (bookshelf geometry) and find a stable structure by assuming an ansatz for the pseudo-layer displacement from the bookshelf geometry and then minimizing the free energy at a very strong and very weak surface anchoring. In this way a threshold condition for the onset of the modulated structure is obtained, as well as the amplitude and period of modulation. Next, we assume that, at the onset of the twist-bend nematic phase, pseudo-layers are formed at some angle (pre-tilt) with respect to the surface. We find that in both cases, the bookshelf and pre-tilted one, the calculated period of modulation far from the phase transition is always approximately twice the cell thickness, which agrees with experimental observations. The properties of light diffracted by the spontaneously formed grating were studied both experimentally and theoretically. We measured the intensity and polarization properties of the first two orders of the diffracted light and the temperature dependence of the polarization of the second order diffraction peaks. To predict the observed properties of the diffracted light and to simplify the description of such gratings, we consider different preliminary models of a one-dimensional spatial variation of the optic axis, the direction of which is given by two angles. A transfer matrix method is used and a good agreement between the experimental and theoretical results is obtained. In a more comprehensive approach, we determine the spatial variation of the optic axis direction from the modeled structure. The electric field in the diffracted light is obtained by using the transfer matrix method and beam propagation method. In the case of a pre-tilt of the pseudo-layers and very strong surface anchoring both methods give good qualitative agreement with experimental results, only in the case of the temperature dependence of the second order diffraction peaks, a more complex beam propagation method is superior to the transfer matrix method. The thesis is divided into three parts. In the first part, we focus on the physical properties of the twist-bend nematic phase and its structure in thin planar cells. In the second part, a continuum model is proposed and finally, the properties of diffracted light are discussed and theoretically predicted by using the beam propagation method and transfer matrix method.
Ključne besede: Bent-dimer liquid crystals, twist-bend nematic phase, undulation of pseudo-layers, polarization, diffraction grating, beam propagation method, transfer matrix method.
Objavljeno v DKUM: 21.10.2021; Ogledov: 670; Prenosov: 61
.pdf Celotno besedilo (10,65 MB)

Lagrangian particle tracking in velocity-vorticity resolved viscous flows by subdomain BEM
Jure Ravnik, Matjaž Hriberšek, Janez Lupše, 2016, izvirni znanstveni članek

Opis: A numerical study of particle motion in a cubic lid driven cavity is presented. As a computational tool, a boundary element based flow solver with a Lagrangian particle tracking algorithm is derived. Flow simulations were performed using an in-house boundary element based 3D viscous flow solver. The Lagrangian particle tracking algorithm is capable of simulation of dilute suspensions of particles in viscous flows taking into account gravity, buoyancy, drag, pressure gradient and added mass. The derived algorithm is used to simulate particle behaviour in a cellular flow field and in a lid driven cavity flow. Simulations of particle movement in a cellular flow field were used to validate the algorithm. The main goal of the paper was to numerically simulate the flow behaviour of spheres of different densities and different diameters, as experimentally observed in work of Tsorng et al.The study of slightly buoyant and non-buoyant particles in a lid driven cavity was aimed at discovering cases when particles leave the primary vortex and enter into secondary vortices, a phenomenon described in the work of Tsorng et al. A parametric study of this phenomenon was preformed. The presented computational results show excellent agreement with experiments, confirming the accuracy of the developed computational method.
Ključne besede: dispersed two phase flow, Lagrangian particle tracking, cellular flow, lid driven cavity, boundary element method
Objavljeno v DKUM: 04.08.2017; Ogledov: 883; Prenosov: 364
.pdf Celotno besedilo (13,57 MB)
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Qualitative Studies of Some Polynomial Systems of Ordinary Differential Equations
Maša Dukarić, 2016, doktorska disertacija

Opis: This doctoral dissertation is devoted to the studies of some qualitative properties of certain polynomial systems of ordinary differential equations. The main problems that are considered in this thesis are the problems of integrability and cyclicity. Some results on the classification of the global phase portraits of a family of cubic systems are presented as well. In the first chapter basic notions and results of the qualitative theory of systems of ODE's are introduced. Since one of important tools for our study of these problems is the commutative computational algebra, some main notions and properties of polynomial ideals and their varieties, including various algorithms related to them, are also presented in the introduction. In the second chapter methods for investigation of trajectories near degenerated singularities are presented. They are further used for the classification of global phase portraits of a family of cubic systems with the nilpotent center at the origin. In the third chapter the main problem of these thesis is studied, the problem of integrability. The problem of integrability which is connected to the problem of distinguishing between a center and a focus is studied for two different families of cubic polynomial systems of ODE's. With the computational algebra approach the necessary conditions for the existence of the first integral of these systems were obtained. For all but one condition was proven, using various approaches, the existence of the first integrals. The center problem for the real systems can be generalized to the complex systems. The origin of the system obtained after the complexification of the real system is the so-called 1:-1 resonant singular point, from which one additional generalization follows. This is the generalization to the p:-q resonant center. In the third chapter the :-3 resonant singular point of a quadratic family of complex systems is studied. The fourth chapter is devoted to the study of the problem of integrability of a three dimensional polynomial system with quadratic nonlinearities. The problem of existence of two independent first integrals and the existence of one first integral in the system was investigated. In the last chapter local bifurcations of limit cycles of a family of cubic systems are studied. Estimations for the number of limit cycles bifurcated from each components of the center variety are obtained.
Ključne besede: planar systems of ODE's, higher dimensional systems of ODE's, phase portrait, nilpotent center, limit cylces, Poincaré compactification, center problem, Bautin ideal, focus quantities, time-reversibility, integrability problem, Darboux method, linearizability, limit cycle, cyclicity
Objavljeno v DKUM: 19.07.2016; Ogledov: 1592; Prenosov: 247
.pdf Celotno besedilo (12,26 MB)

Unobtrusive monitoring of human vital functions based on speckle interferometry with plastic optical fiber
Peter Podbreznik, Denis Đonlagić, Dejan Lešnik, Boris Cigale, Damjan Zazula, 2013, izvirni znanstveni članek

Opis: In this paper, a speckle interferometer with a plastic optical fiber system is reported for unobtrusive monitoring of heartbeat and respiration. The sensor consists of a laser diode butt-coupled to the plastic optical fiber, whose exit face projects speckle patterns onto a linear optical sensor array, which leads to a simple and cost-effective construction. Speckle images are acquired in a sequence and transformed into a 1D signal by using a phase-shifting method. Band-pass filtering and Morlet-wavelet-based multiresolutional approaches were used to analyze signals for the detection of cardiac and respiratory activities, respectively. Ten young, healthy persons participated in system testing, by lying supine on a mattress with embedded plastic optical fiber. Experimental results show the proposed system and detection algorithms are highly efficient. Sensitivities of 99.4 0.6% and 95.3 3%, precisions of 98.8 1.5% and 97.9 2.3%, and mean delays between interferometric detections and corresponding referential signals of 116.6 55.5ms and 1299.2 437.3 ms were computed for heartbeat and respiration, respectively.
Ključne besede: plastic optical fiber, speckle interferometry, unobtrusive monitoring, heartbeat detection, respiration detection, phase-shift method, wavelet transform
Objavljeno v DKUM: 10.07.2015; Ogledov: 1246; Prenosov: 16
URL Povezava na celotno besedilo

“Thermodynamic and physical properties for high pressure process design”
Maša Knez Marevci, 2014, doktorska disertacija

Opis: The thesis is comprised of three main categories. The first part of dissertation covers investigations of phase equilibria of compounds from natural materials in conventional and also non conventional supercritical fluids. In details, the impact of pressure and/or temperature on the system behaviour (miscibility, solubility, phase inversion) is investigated, quantitative and qualitative analyses to evaluate and identify compounds contained after performing preliminary extraction experiments from different natural tissues are presented. The impact of operating parameters (pre-treatment of the raw material with SFE; different extraction solvents: propane, CO2, non conventional SCFs; different extraction temperatures and pressures) on extraction kinetics is observed. Following substances were taken into consideration: vanillins, caffeine, carnosoic acid extract and lecithin. Second part of dissertation covers studies of phase equilibria of the systems bio oil/gas, which is crucial in biorefinery process design. In this part of dissertation, which covers studies of phase equilibria of binary and ternary systems, the impact of pressure and/or temperature on the system behaviour (miscibility, solubility, phase inversion) for binary system bio oil/supercritical fluid (bio oil/CO2) and (bio oil/H2) was studied. Additionally, phase behaviour of ternary systems of (bio oil/diesel/CO2) and (bio oil/tail water/CO2) under the impact of pressure and/or temperature is observed. These data are of a high importance for bio refineries as an important part of necessary sustainable development. In recent years, studies on biodiesel synthesis have focused on development of process intensification technologies to resolve some of these issues. Fundamental data to design fractionation process of components of bio oil are crucial for an efficient hydrogenation process of bio oil. In the third part of dissertation observation of phase equilibria and determination of the parameters like diffusion coefficient, density and viscosity for the systems polymer/CO2 at elevated pressures is investigated. An overview of different methods applied to determine the parameters like diffusion coefficient, density and viscosity of the systems polymer (PEG)/CO2 at elevated pressures is offered. Observation of phase equilibria of the binary system PEG/CO2, determination of the impact of pressure and/or temperature on the system behaviour (miscibility, solubility, phase inversion), determination of thermodynamically and physically properties of the system with new applicative methods and finally, comparison of the results obtained by different methods is provided. The interfacial tension (IFT) at the (PEG)/CO2 interface has been determined by using an experimental technique developed to study the interfacial interactions of the liquids in equilibrium with gas in a glass-windowed equilibrium cell by the means of Capillary Rise (CR) method. Advantages and disadvantages of methods that were applied are exposed and discussed.
Ključne besede: phase equilibria, natural materials, conventional and non conventional supercritical fluids, extraction, bio oil, data for biorefinery process design, systems polymer (PEG)/CO2, diffusion coefficient, density, viscosity, surface tension, Capillary Rise (CR) method.
Objavljeno v DKUM: 28.10.2014; Ogledov: 2377; Prenosov: 338
.pdf Celotno besedilo (4,46 MB)

Weakly coupled analysis of a blade in multiphase mixing vessel
Matej Vesenjak, Zoran Ren, Matjaž Hriberšek, 2004, kratki znanstveni prispevek

Opis: Two or more physical systems frequently interact with each other, where the independent solution of one system is impossible without a simultaneous solution of the others. An obvious coupled system is that of a dynamic fluid-structure interaction. š8đ In this paper a computational analysis of thefluid-structure interaction in a mixing vessel is presented. In mixing vessels the fluid can have a significant influence on the deformation of blades during mixing, depending on speed of mixing blades and fluid viscosity.For this purpose a computational weakly coupled analysis has been performed to determine the multiphase fluid influences on the mixing vessel structure. The multiphase fluid field in the mixing vessel was first analyzed with the computational fluid dynamics (CFD) code CFX. The results in the form of pressure were then applied to the blade model, which was the analysed with the structural code MSC.visualNastran forWindows, which is based on the finiteelement method (FEM).
Ključne besede: fluid mechanics, solid mechanics, coupled problems, computational analysis, two-phase fluid, mixing blade, pressure distribution, finite volume method, finite element method
Objavljeno v DKUM: 01.06.2012; Ogledov: 1434; Prenosov: 88
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