Gravity driven trickle flow of a liquid over a fixed bed in the presence of a gaseous phase is widely encountered throughout the process industry. It is one of the most common ways of contacting multi-phase fluids for reaction or mass transfer purposes. The presence of three phases greatly complicates the mathematical modelling of trickle-bed reactors and makes a description from first principles difficult. Trickle flow performance is usually characterized in terms of hydrodynamic parameters. One such parameter is the liquid holdup. The value and morphology (shape or texture) of the holdup influences the catalyst contacting, wetting, mass transfer characteristics and ultimately the performance of the trickle flow unit. This study is limited to the air-water-glass spheres system with no gas flow. It is partitioned into three sections. An investigation into the nature of the residual liquid holdup in beds of spherical particles revealed that the general assumption that all residual liquid is held in the form of pendular rings at particle contact points proves to be untrue. Instead, indication is that 48 % of the residual holdup is present in the form of agglomerated liquid globules in interstices of low local porosity. Theoretical residual liquid holdup models and residual liquid holdup-based mass transfer models should include this phenomenon. In a subsequent section, the influence of the prewetting procedure on the operating holdup is investigated. Three distinct limiting cases are identified: Kan-wetted, Levec-wetted and non-wetted. A volumetric utilization coefficient that describes the extent to which the bed is irrigated is developed. It indicates that large fractions of the bed remain non-irrigated in the Levec- and non-wetted modes. A momentum balance-based model is adopted to predict the Kan-wetted mode holdup. This model was successfully extended to predicting the holdup in the Levec- and non-wetted modes by simple incorporation of the volumetric utilization coefficient. The predictive capability of this model is highly satisfactory, especially in light of it using only the classical Ergun constants and no fitted parameters (AARE = 9.6 %). The differences in the hysteresis behaviour of holdup and pressure drop in the different modes are attributed to differences in the morphology of the operating holdup. The existence of the three limiting prewetted modes is confirmed by residence time distribution (RTD) analysis of the stimulus-response behaviour of the system. This behaviour was quantified using a NaCl tracer and conductivity measurements at both the inlet and outlet of a bench scale bed. The analyses show that: · There are large fractions of the holdup that is inaccessible to the tracer in the Levec-wetted and non-wetted modes. · The mixedness in the three prewetted modes differ appreciably, with the Kan-wetted mode clearly less mixed than the Levec-wetted mode. The RTD analyses also confirm the existence of the three prewetting modes in a porous system (spherical a-alumina), with a large fraction of the holdup being inaccessible to the tracer in the Levec-wetted mode. This study emphasizes the role of the morphology of the various types of liquid holdup on the hydrodynamic performance of a trickle flow unit. It is apparent that aspects of the morphology depend strongly on phenomena like globule formation, hysteresis and flow and prewetting history that have not been adequately recognized to date. The visualization of the various modes of trickle flow is an intellectual platform from which future studies may be directed. / Dissertation (MEng)--University of Pretoria, 2004. / Chemical Engineering / Unrestricted

The prewetting of a trickle-bed reactor has important implications in the design and operation of these reactors. This is because the prewetting changes the flow morphology (shape and texture) of the liquid flowing through the bed and leads to the existence of multiple hydrodynamic states. The extent of this change in flow morphology can be seen in the effect the prewetting of the reactor has on the pressure drop, liquid holdup and gas-liquid mass transfer. The following prewetting procedures were used: -- Levec-wetted: the bed is flooded and drained and after residual holdup stabilisation the gas and liquid flow is reintroduced -- Kan-wetted: the bed is operated in the pulse flow regime and liquid and gas flow rates are reduced to the desired set point -- Super-wetted: the bed is flooded and gas and liquid flow are introduced once draining commences For the pressure drop: -- The different prewetting procedures resulted in two distinct regions (Upper region Kan and Super-wetted, Lower region Dry and Levec-wetted) -- There was no significant difference between the Dry and Levec-wetted beds -- The pressure drop in the Kan and Super-wetted beds can be as much as seven times greater than the pressure drop in the Dry and Levec-wetted beds For the liquid holdup: -- The different prewetting procedures resulted in four distinct regions (Kan-wetted, Super-wetted, Levec-wetted, Dry bed) -- The liquid holdup in the Kan-wetted bed can be as much as four times greater than the liquid holdup in the Dry bed -- The liquid holdup in the Levec-wetted can be as much as thirty percent lower than the liquid holdup in the Kan-wetted bed For the gas-liquid mass transfer: -- The different prewetting procedures resulted in three distinct regions (Kan and Super-wetted, Levec-wetted, Dry bed) -- The volumetric gas-liquid mass transfer coefficient in the Kan and Super-wetted beds can be as much as six times greater than the mass transfer coefficient in the Dry bed -- The volumetric gas-liquid mass transfer coefficient in the Kan and Super-wetted beds can be as much as two and a half times greater than the mass transfer coefficient in the Levec-wetted bed While an increase in the liquid flow rate results in an increase in the pressure drop, liquid holdup and gas-liquid mass transfer for all of the experiments, the effect of increasing gas flow on the measured variables were more pronounced for the prewetted beds. In a prewetted bed (Kan, Super and Levec-wetted) an increase in the gas flow rate causes an increase in the volumetric gas-liquid mass transfer coefficient and a decrease in the liquid holdup. The decrease in the liquid holdup is due to the fact that the increased gas flow rate causes the films around the particles to thin and spread out. In the dry bed the flow is predominantly in the form of rivulets and the increase in gas flow rate does not affect the liquid holdup. In the case of the volumetric gas-liquid mass transfer coefficient the increased gas flow rate causes an increase in the mass transfer coefficient regardless of the prewetting procedure. This increase is due to the effect that the gas flow rate has on the liquid holdup as well as the increase in the gas-liquid interfacial area due to the increased gas-liquid interaction. If the pulsing in the Kan-wetted bed is induced by increasing the gas flow rate and keeping the liquid flow rate constant the results are significantly different. The pressure drop in the gas-pulsing experiments was lower than the pressure drop in the recorded in the Kan and Super-wetted beds, but higher than the pressure drop in the dry and Levec-wetted beds. However, the liquid holdup in the gas-pulsing experiments was higher than the liquid holdup in any of the other beds. The volumetric gas-liquid mass transfer coefficient in the gas-pulsing experiments was lower than the mass transfer coefficients of the Kan and Super-wetted beds, but higher than the mass transfer coefficients in the dry and Levec-wetted beds. The multiple operating points obtained from the different prewetting procedures are by no means the only possible operating points. By simply decreasing the draining time in the Levec-wetted bed steady state operating points can be found between those of the Super and Levec-wetted beds. This alludes to the fact that the operating conditions determined from the different prewetting modes are only boundaries and that the actual operating point can lie anywhere between these boundaries. The existence of these multiple hydrodynamic states complicates things further when a correlation is developed to determine the pressure drop, liquid holdup or the volumetric gas-liquid mass transfer coefficient. No correlation tested was able to accurately predict the pressure drop, liquid holdup or volumetric gas-liquid mass transfer coefficient in the dry or prewetted beds. / Dissertation (MEng (Chemical Engineering))--University of Pretoria, 2007. / Chemical Engineering / unrestricted

Trickle-flow is traditionally modeled by means of hydrodynamic parameters such as liquid holdup, two-phase pressure drop and wetting efficiency. Several studies showed that these parameters are not only a function of flow conditions and bed properties, but also of the flow history and morphology of flow. These can have a major influence on the distribution in the bed. The effect of flow morphology on liquid holdup and pressure drop is widely discussed in literature, but little attention is paid to its effect on wetting efficiency. Trickle-bed reactor models suggest that not a only bed-averaged but also the distribution of wetting efficiency may be of importance for reactor performance. Both the average wetting efficiency and the distribution of wetting are probably a function flow history and morphology. The distribution of wetting efficiency for different flow morphologies were investigated by means of a colorometric method that was developed for this purpose. Representative wetting distributions could be obtained. Flow morphologies and liquid distributions were manipulated by means of the pre-wetting procedure that was performed prior to flow. Pulse and Levec pre-wetted beds were investigated. These distributions were explained in detail in terms of flow morphology. It was found that the average wetting efficiency in pulse pre-wetted beds are much higher than in Levec pre-wetted beds. All particles in the pulse pre-wetted beds at all investigated flow conditions were contacted by the flowing liquid. This was not the case for the Levec pre-wetted beds. It was found that the flow in Levec pre-wetted beds become similar to that in pulse pre-wetted beds at high liquid flow rates. It was investigated how these distributions can affect reactor modeling, based on popular particle-scale models that relate reactor efficiency to wetting efficiency. According to these models, the wetting efficiency distribution in pulse pre-wetted beds can be characterised by means of only its average value. This is not the case for Levec pre-wetted beds. These results are however a strong function of the models that were employed. Finally, some recommendations are made in terms of the preferred pre-wetting method or flow morphology for different types of reactions. These recommendations are also based on models and have not been verified with experiments. / Dissertation (MEng (Chemical Engineering))--University of Pretoria, 2007. / Chemical Engineering / unrestricted

Trickle flow is encountered in a variety of process engineering applications where gas and liquid flow through a packed bed of stationary solid. Owing to the complexities of three interacting phases, a fundamentally exhaustive description of trickle flow hydrodynamics has not been achieved. A complicating factor in describing the hydrodynamics is the fact that the hydrodynamic state is dependent not only on the present operating conditions but also on their entire history, including fluid flow rate changes and pre-wetting procedures. This phenomenon is termed hydrodynamic multiplicity and is the subject of this work. Hydrodynamic multiplicity greatly complicates both the experimental investigation into the behaviour of a trickle flow column and the theoretical modelling of the observed behaviour. Broadly speaking, this study addresses hydrodynamic multiplicity on three levels. First, a conceptual framework is proposed that can be used to study hydrodynamic multiplicity with limited resources. It is based on the absolute limiting values that the hydrodynamic parameters can adopt for a certain set of conditions, and encompasses both flow rate hysteresis loops and pre-wetting procedures. There are 5 such hydrodynamic modes. When the existing literature is critically evaluated in light of this framework, it is established that the reported experimental studies have not addressed all the issues. Previous modelling attempts are also shown to be unable to qualitative explain all the existing data. Moreover, authors have suggested different (and often contradictory) physical mechanisms responsible for hydrodynamic multiplicity. Secondly, an experimental investigation intended to supplement the existing literature and illustrate the utility of the proposed framework is launched. This includes bed-scale measurements of liquid holdup, pressure drop and gas-liquid mass transfer for a variety of conditions including different flow rates, pressures, particle shapes, particle porosity and surface tension. The second part of the experimental effort uses radiography and tomography in new ways to visualise the temporal and spatial characteristics of the different hydrodynamic modes. The tomographic investigation incorporates advanced image processing techniques in order to culminate in a pore-level evaluation of the hydrodynamic modes that reveals additional features of hydrodynamic multiplicity. Thirdly, the experimental insights are condensed into a set of characteristic trends that highlight the features of hydrodynamic multiplicity. A pore-level capillary mechanism is then introduced to qualitatively explain the observed behaviour. The mechanism shows how the differences in advancing and receding contact angles and the characteristics of the packed structure (or pore geometries) are ultimately responsible for the observed hydrodynamic multiplicity behaviour. Lastly, the effect of hydrodynamic multiplicity on trickle bed reactor performance is discussed. It is established experimentally that depending on the reaction conditions, different modes yield optimal performance. The idea of optimizing the performance by manipulating the hydrodynamic state is introduced. In totality, this work advances the understanding of trickle flow hydrodynamics in general and hydrodynamic multiplicity in particular. / Thesis (PhD (Chemical Engineering))--University of Pretoria, 2008. / Chemical Engineering / unrestricted

Please read the abstract in the dissertation. Copyright / Dissertation (MEng)--University of Pretoria, 2011. / Chemical Engineering / unrestricted

Residence time distributions have become an important analytical tool in the analysis of many types of flow systems. Residence time distributions have proven to be effective for analysing trickle bed reactors, as it allows determination of parameters under operating conditions allowing no interference of these conditions. By studying the residence time distribution a great amount of information can be obtained and therefore used to determine a number of hydrodynamic parameters. Due to recent findings that prewetting has a tremendous effect on a number of hydrodynamic parameters such as holdup, wetting efficiency and pressure drop, it is therefore the aim of this study to investigate the effect of trickle flow morphology or prewetting on a trickle bed reactor. The residence time distribution is obtained whereby hydrodynamic parameters are determined and therefore the effect the flow morphology has on various hydrodynamic parameters is highlighted. A number of methods were used to determine these parameters, namely that of the best-fit method, whereby the PDE model was used, and the method of moments. Operating conditions included varying gas and liquid flow rates for porous and non-porous catalyst particles at atmospheric pressure. The different prewetting procedures used during this work included the following: <ul><li>Non-wetted </li> <li>Levec-wetted </li> <li>Super-wetted</li></ul> From this investigation the following conclusions were made: <li>Prewetting has a great effect on the hydrodynamic parameters of trickle bed reactors</li> <li>The differences in prewetting can be attributed to differing flow morphologies for the different prewetted beds i.e. the dominant flow morphology for a non-wetted bed is that of rivulets and for prewetted beds that of film flow</li> <li>It was also found that at low liquid flow rates the flow morphology in prewetted beds changes from film flow to a combination of rivulet and film flow</li> <li>The different flow morphologies for prewetted and non prewetted beds was confirmed by the residence time distributions and various parameters obtained there from</li> <li>At low liquid flow rates the flow morphology becomes a more predominant factor in creating the tailing effect present in residence time distribution for prewetted beds</li> <li>The tailing effect in residence time distributions is a result of both internal diffusion and liquid flow morphology, where the liquid flow morphology is the more dominant factor</li> <li>The use of residence time distributions to determine a number of hydrodynamic parameters proved to be very useful and accurate by means of different methods, i.e. method of moments and best-fit method</li> <li>Differences in the liquid holdup determined from the method of moments and the weighing method confirmed that different flow morphologies exist for different prewetted beds</li> <li>An increase in the dispersion coefficient with prewetting was observed indicating that the amount of micro mixing is different for the different prewetted beds</li> <li>Differences in residence times and high values for the dynamic holdup, for the porous packing, confirmed that the PDE model does not model well the porous packing response curves due to the lack of internal diffusion and internal holdup in this model</li> <li>The dynamic-static mass transfer showed that film flow, as in prewetted beds, results in slower mass transfer as opposed to rivulet flow and therefore it is concluded that prewetting results in different flow morphologies.</li></ul> Following this study it is recommended that a residence time distribution model be used or developed that incorporates the effects of internal diffusion and internal holdup as present in porous catalyst particles. In addition, it was found that very few correlations could accurately predict hydrodynamic parameters due to the absence of the effect of prewetting and therefore it is recommended that correlations be developed that incorporate the effect of prewetting. / Dissertation (MEng)--University of Pretoria, 2008. / Chemical Engineering / unrestricted

Several types of reactors are encountered in industry where reagents in a gas and a liquid phase need to be catalysed by a solid catalyst. Common reactors that are used to this end, are trickle-bed reactors, where gas and liquid flow cocurrently down a packed bed of catalyst. Apart from the catalytic process itself, several mass transfer steps can influence the rate and/or selectivity of a solid catalysed gas-liquid reaction. In trickle-bed reactors, flow morphology can have a major effect on these mass transfer steps. This study investigates the interaction between liquid flow morphology and mass transfer in trickle-bed reactors from three different angles. The primary focus is on liquid-solid mass transfer and internal diffusion as affected by the contacting between the liquid and the catalyst. First, the contacting between the liquid and the solid in trickleflow, or wetting efficiency, is characterised using colorimetry. Though this investigation is limited to the flow of nitrogen and water over a packed bed at ambient conditions, it provides useful information regarding liquid flow multiplicity behaviour and its influence on the distribution of fractional wetting on a particle scale. The colorimetric study also provides descriptions of the geometry of the liquid-solid contacting on partially wetted particles. These are used in a second investigation, for the numerical simulation of reaction and diffusion in partially wetted catalysts. This second investigation uses numerical simulations to evaluate and develop simple theoretical descriptions of liquid-solid contacting effects on catalyst particle efficiency. Special attention is given to the case where external and intraparticle mass transfer rates of both a volatile and non-volatile reagent affect the overall rate of reaction. Also, since these are not often considered in theoretical studies, some suggestions are made for the evaluation of the particle efficiency of eggshell catalyst. Finally, liquid-solid contacting is investigated in a high-pressure pilot reactor. Wetting efficiency is measured with a useful technique that does not rely on descriptions of particle kinetics or liquid-solid mass transfer rates. Liquid-solid mass transfer coefficients are also measured and results agree well with the colorimetric investigation, suggesting the existence of different types of flow within in the hydrodynamic multiplicity envelope of trickle-flow. Since it consists of different investigations of liquid-solid contacting from different angles, the study highlights several aspects of liquid-solid contacting and how it can be expected to influence trickle-bed reactor performance. / Thesis (PhD)--University of Pretoria, 2009. / Chemical Engineering / unrestricted