Trickle bed reactors (TBRs) exhibit complex hydrodynamics and this study is aimed at giving insight into whether liquid-solid mass transfer and wetting are influenced by bed depth in a 5 m trickling column using 4 mm glass spheres as random packing. Measurements were made using the novel electrochemical technique developed by Joubert and Nicol (2013). Using this technique the wetting and mass transfer could be measured simultaneously. The study proves that the liquid-solid mass transfer and wetting efficiency do not stabilise at a minimum bed depth. The parameters were found to continue decreasing until the bottom of the bed. For the upper branch of the hydrodynamic envelope, the rate of decrease for the wetting efficiency was slow at the top of the bed and decreased rapidly closer to the bottom. However, only the wetting efficiency decreased significantly as a function of bed length; the liquid-solid mass transfer exhibited only a slight decrease of 14%. This compared well with the results of Du Toit et al. (2014), who found an 11% decrease in the liquid-solid mass transfer in a column with an x/D value of 29,4. The lower branch of the hydrodynamic envelope showed a linear decrease with respect to bed length for both wetting and mass transfer. The liquid-solid mass transfer decreased by 50% from the top of the bed to the bottom. These results are also in agreement with those of Du Toit et al. (2014)1 who found a decrease of 30% for a 1,6 m column. The wetting efficiency for the Levec mode decreased by 52%, whereas Du Toit et al. (2014)2 found a decrease of 20%. / Dissertation (MEng)--University of Pretoria, 2014. / lk2014 / Chemical Engineering / MEng / 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

Hydrodynamic multiplicity in the trickle flow, or low interaction, regime is a well documented phenomenon. Multiple hydrodynamic states are often presented in the form of hysteresis loops where the hydrodynamic parameter studied are shown as a function of the operating history of the bed, i.e. liquid and gas flow rates. In extreme cases the lower leg, representing an increase in liquid flow rate on a pre-wetted and drained bed, is commonly referred to as the Levec mode. The upper extreme, referred to as the Kan-liquid mode, represents a decrease in liquid flow rate after operation in the high interaction regime. The many reported studies investigating liquid-solid mass transfer in trickle beds have generally used either the dissolution or electrochemical techniques. Numerous researchers have used their data to develop correlations predicting solid-liquid mass transfer coefficients. Most of these studies do not specify the multiplicity mode of operation. Only two studies (Sims et al. (1993) and Van der Merwe, Nicol&Al-Dahhan (2008)) use both the Levec and Kan-liquid operating modes. Both of these studies suggest that solid-liquid mass transfer also exhibit multiplicity behaviour although the trends suggested or speculated differ from each other. Sims et al. (1993) found that a Kan-liquid operated bed will outperform a Levec operated bed; however in contrast to this Van der Merwe et al. (2008) speculated that a Levec operated bed is better suited for liquid limited reactions due to enhanced liquid-solid mass transfer in the Levec mode as a result of faster interstitial velocity. This study showed that solid-liquid mass transfer coefficients, measured with both the dissolution and electrochemical technique, show multiplicity behaviour. Two distinct operating regions were found, which corresponds to the Levec and Kan-liquid modes. Measurements taken using the electrochemical technique yielded solid-liquid mass transfer coefficients larger than those measured using the dissolution method. The experimental results agree with the trend found by Sims et al. (1993) but the mass transfer coefficients in this study were significantly lower. Additionally it was shown that the difference in mass transfer coefficients, in the two modes, cannot be explained by merely compensating for the differences in wetting efficiency and interstitial velocity, suggesting that the Levec mode has a larger percentage of stagnant or poorly irrigated zones. It was also shown that mass transfer coefficients measured at the top of the column is higher than those measured at the bottom, suggesting that the flow structure is changing as a function of axial length. Lastly, with regards to electrochemical measurements of liquid-solid mass transfer, it was shown that measurements using a single particle electrode compared well to that of a multiple packing electrode. / Dissertation (MEng)--University of Pretoria, 2009. / 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