Holdups

In a steady state continuous distillation with the assumption of a well mixed liquid and vapour on the plates, the holdup has no effect on the analysis (modelling of such columns does not usually include column holdup) since any quantity of liquid holdup in the system has no effect on the mass flows in the system (Rose, 1985). Batch distillation however is inherently an unsteady state process and the liquid holdup in the system become sinks (accumulators) of material which affect the rate of change of flows and hence the whole dynamic response of the system. 

An extensive literature survey indicates that the role of column holdup on the performance of batch distillation has been the subject of some controversy until recently. The following paragraphs outline briefly the investigations carried out on column holdup since 1950. Most of the investigations were restricted to conventional batch distillation columns and binary mixtures. The readers are directed to the original work to develop further understanding of the topic. 

Rose et al. (1950) and Rose and O Brien (1952) studied the effect of holdup for binary and ternary mixtures in a laboratory batch column. They qualitatively defined the term sharpness of separation as the sharpness in the break between successive components in the graph of instantaneous distillate composition against percentage distilled. They showed that an increase in column holdup enhanced the sharpness of separation at low reflux ratio but did not have any effect at a very high reflux ratio. 

For binary mixtures Converse and Huber (1965) found that in all cases studied, column holdup causes a decrease in the amount of maximum distillate obtained for a fixed time of operation. In another way, for a fixed amount of distillate and purity of the lighter component, higher column holdup increased the batch time. The authors concluded that the presence of significant holdup is bad anyway. 

Using binary mixtures, Luyben (1971) studied the effects of holdup, number of plates, relative volatility, etc. on the capacity (total products/hr). For an arbitrarily assumed constant reflux ratio the author observed both positive and negative effects of tray holdup on the capacity for columns with larger number of plates, while only negative effects were observed for columns with smaller number of plates. It is apparent that these observations are related to the degree of difficulty of separation. 

Xl and Xq may be expressed in tenns of the flow rates Ql and Qg, at a given point in the pipe, as  

The experimental techniques available for measming holdup fall into two categories, namely, direct and indirect methods. The direct method of 

Furthermore, these equations predict values of ai to within 1% at the values of X marking the changeover point between equations. The overall average error is of the order of 7% and the maximiun error is about 15%. 

Because of the widely different types of behaviour exhibited by non-Newtonian fluids, it is convenient to deal with each flow regime separately, depending upon whether the liquid flowing on its own at the same flow rate would be in streamline or turbulent flow. While it is readily conceded that streamline flow does not have as straightforward a meaning in two phase flows as in the flow of single fluids, for the purposes of correlating experimental results, the same criterion is used to delineate the type of flow for non-Newtonian fluids as discussed in Chapter 3 (Section 3.3), and it will be assumed here that the flow will be streamline for ReM/e 2000, prior to the introduction of gas. 

The predictions from equation (4.6) will be compared first with the experimental values of average liquid holdup for cocmrent two-phase flow of a gas and shear-thinning liquids. For a liquid of given rheology (m and n), the pressure gradient (—Api/L) may be calciflated using the methods presented in Chapter 3 but oifly the power-law model will be used here. 

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The column inventory also can be reducdd by the use of low-holdup column internals, including the holdup in the column base. As the design progresses, other features can be included to reduce the inventory. Thermosyphon reboilers have a lower inventory than kettle reboilers. Peripheral equipment such as reboilers can be located inside the column. ... 

At the completion of adsorption, the less selectively adsorbed components have been recovered as product. However, a significant quantity of the weaMy adsorbed species are held up in the bed, especially in the void spaces. A cocurrent depressurization step reduces the bed pressure by allowing dow out of the bed cocurrendy to feed dow and thus reduces the amount of product retained in the voids (holdup), improving product recovery, and increases the concentration of the more strongly adsorbed components in the bed. The purity of the more selectively adsorbed species has been shown to depend strongly on the cocurrent depressurization step for some appHcations (66). A cocurrent depressurization step is optional because a countercurrent one always exists. Criteria have been developed to indicate when the use of both is justified (67). 

To prevent such release, off gases are treated in Charcoal Delay Systems, which delay the release of xenon and krypton, and other radioactive gases, such as iodine and methyl iodide, until sufficient time has elapsed for the short-Hved radioactivity to decay. The delay time is increased by increasing the mass of adsorbent and by lowering the temperature and humidity for a boiling water reactor (BWR), a typical system containing 211 of activated carbon operated at 255 K, at 500 K dewpoint, and 101 kPa (15 psia) would provide about 42 days holdup for xenon and 1.8 days holdup for krypton (88). Humidity reduction is typically provided by a combination of a cooler-condenser and a molecular sieve adsorbent bed. 

In this equation, represents the rate of energy dissipation per unit mass of fluid. In pulsed and reciprocating plate columns the dimensionless proportionahty constant K in equation 38 is on the order of 0.3. In stirred tanks, the proportionaUty constant has been reported as 0.024(1 + 2.5 h) in the holdup range 0 to 0.35 (67). The increase of drop si2e with holdup is attributed to the increasing tendency for coalescence between drops as the concentration of drops increases. A detailed survey of drop si2e correlations is given by the Hterature (65). 

Holdup and Flooding. The volume fraction of the dispersed phase, commonly known as the holdup can be adjusted in a batch extractor by means of the relative volumes of each Hquid phase added. In a continuously operated weU-mixed tank, the holdup is also in proportion to the volume flow rates because the phases become intimately dispersed as soon as they enter the tank. 

However, in a countercurrent column contactor as sketched in Figure 8, the holdup of the dispersed phase is considerably less than this, because the dispersed drops travel quite fast through the continuous phase and therefore have a relatively short residence time in the equipment. The holdup is related to the superficial velocities U of each phase, defined as the flow rate per unit cross section of the contactor, and to a sHp velocity U (71,72) ... 

In the case of a packed column, the terms on the right-hand side should each be divided by the voidage, ie, the volume fraction not occupied by the soHd packing (71). In unpacked columns at low values of the sHp velocity approximates the terminal velocity of an isolated drop, but the sHp velocity decreases with holdup and may also be affected by column internals such as agitators, baffle plates, etc. The sHp velocity can generally be represented by (73) ... 

As the throughput in a contactor represented by the superficial velocities and is increased, the holdup / increases in a nonlinear fashion. A flooding point is reached at which the countercurrent flow of the two Hquid phases cannot be maintained. The flow rates at which flooding occurs depend on system properties, in particular density difference and interfacial tension, and on the equipment design and the amount of agitation suppHed (40,65). 

The nonuniformity of drop dispersions can often be important in extraction. This nonuniformity can lead to axial variation of holdup in a column even though the flow rates and other conditions are held constant. For example, there is a tendency for the smallest drops to remain in a column longer than the larger ones, and thereby to accumulate and lead to a locali2ed increase in holdup. This phenomenon has been studied in reciprocating-plate columns (74). In the process of drop breakup, extremely small secondary drops are often formed (64). These drops, which may be only a few micrometers in diameter, can become entrained in the continuous phase when leaving the contactor. Entrainment can occur weU below the flooding point. 

Coalescence and Phase Separation. Coalescence between adjacent drops and between drops and contactor internals is important for two reasons. It usually plays a part, in combination with breakup, in determining the equiHbrium drop si2e in a dispersion, and it can therefore affect holdup and flooding in a countercurrent extraction column. Secondly, it is an essential step in the disengagement of the phases and the control of entrainment after extraction has been completed. 

The role of coalescence within a contactor is not always obvious. Sometimes the effect of coalescence can be inferred when the holdup is a factor in determining the Sauter mean diameter (67). If mass transfer occurs from the dispersed (d) to the continuous (e) phase, the approach of two drops can lead to the formation of a local surface tension gradient which promotes the drainage of the intervening film of the continuous phase (75) and thereby enhances coalescence. It has been observed that d-X.o-c mass transfer can lead to the formation of much larger drops than for the reverse mass-transfer direction, c to... 

The General Mills mixer—settler (117), shown in Figure 13b, is a pump—mix unit designed for hydrometaHurgical extraction. It has a baffled cylindrical mixer fitted in the base and a turbine that mixes and pumps the incoming Hquids. The dispersion leaves from the top of the mixer and flows into a shallow rectangular settler designed for minimum holdup. 

The sohd can be contacted with the solvent in a number of different ways but traditionally that part of the solvent retained by the sohd is referred to as the underflow or holdup, whereas the sohd-free solute-laden solvent separated from the sohd after extraction is called the overflow. The holdup of bound hquor plays a vital role in the estimation of separation performance. In practice both static and dynamic holdup are measured in a process study, other parameters of importance being the relationship of holdup to drainage time and percolation rate. The results of such studies permit conclusions to be drawn about the feasibihty of extraction by percolation, the holdup of different bed heights of material prepared for extraction, and the relationship between solute content of the hquor and holdup. If the percolation rate is very low (in the case of oilseeds a minimum percolation rate of 3 x 10 m/s is normally required), extraction by immersion may be more effective. Percolation rate measurements and the methods of utilizing the data have been reported (8,9) these indicate that the effect of solute concentration on holdup plays an important part in determining the solute concentration in the hquor leaving the extractor. 

The upward flow of gas and Hquid in a pipe is subject to an interesting and potentially important instabiHty. As gas flow increases, Hquid holdup decreases and frictional losses rise. At low gas velocity the decrease in Hquid holdup and gravity head more than compensates for the increase in frictional losses. Thus an increase in gas velocity is accompanied by a decrease in pressure drop along the pipe, a potentially unstable situation if the flows of gas and Hquid are sensitive to the pressure drop in the pipe. Such a situation can arise in a thermosyphon reboiler, which depends on the difference in density between the Hquid and a Hquid—vapor mixture to produce circulation. The instabiHty is manifested as cycHc surging of the Hquid flow entering the boiler and of the vapor flow leaving it. 

For primary insulation or cable jackets, high production rates are achieved by extmding a tube of resin with a larger internal diameter than the base wke and a thicker wall than the final insulation. The tube is then drawn down to the desked size. An operating temperature of 315—400°C is preferred, depending on holdup time. The surface roughness caused by melt fracture determines the upper limit of production rates under specific extmsion conditions (76). Corrosion-resistant metals should be used for all parts of the extmsion equipment that come in contact with the molten polymer (77). 

At a holdup time longer than 10—15 min at a high temperature, resin degradation is avoided by keeping the rear of the cylinder at a lower temperature than the front. At short holdup times (4—5 min), cylinder temperatures are the same in rear and front. If melt fracture occurs, the injection rate is reduced pressures are in the range of 20.6—55.1 MPa (3000—8000 psi). Low backpressure and screw rotation rates should be used. 

Pressure. Within limits, pressure may have Htfle effect in air-sparged LPO reactors. Consider the case where the pressure is high enough to supply oxygen to the Hquid at a reasonable rate and to maintain the gas holdup relatively low. If pressure is doubled, the concentration of oxygen in the bubbles is approximately doubled and the rate of oxygen deHvery from each bubble is also approximately doubled in the mass-transfer rate-limited zone. The total number of bubbles, however, is approximately halved. The overall effect, therefore, can be small. The optimum pressure is likely to be determined by the permissible maximum gas holdup and/or the desirable maximum vapor load in the vent gas. 

This correlation is valid when turbulent conditions exist in an agitated vessel, drop diameter is significantly bigger than the Kohnogoroff eddy length, and at low dispersed phase holdup. The most commonly reported correlation is based on the Weber number ... 

Gas holdup with Rushton turbine can be estimated from the following correlation ... 

Static mixing of gas—Hquid systems can provide good interphase contacting for mass transfer and heat transfer. Specific interfacial area for the SMV (Koch/Sulzer) mixer is related to gas velocity and gas holdup ( ) by the following ... 

Nonintrusive Instrumentation. Essential to quantitatively enlarging fundamental descriptions of flow patterns and flow regimes are localized nonintmsive measurements. Early investigators used time-averaged pressure traverses for holdups, and pilot tubes for velocity measurements. In the 1990s investigators use laser-Doppler and hot film anemometers, conductivity probes, and optical fibers to capture time-averaged turbulent fluctuations (39). 

The first step in CTO distillation is depitching. A relatively small distillation column is used as a pitch stripper. The vapor from the pitch stripper is fed directiy into the rosin column, where rosin and fatty acids are separated. Rosin is taken from the bottoms of the column and fatty acids as a sidestream near the top. Palmitic acid and light neutrals are removed in the rosin column as heads. The operation is designed to minimize holdup and product decomposition. Care is taken to prevent carryover of some of the heavier neutrals, such as the sterols, from the depitcher to the rosin column (24). 

Examination of equation 42 shows that T is directly proportional to the average stage holdup of process material. Thus, in conjunction with the fact that hquid densities are on the order of a thousand times larger than gas densities at normal conditions, the reason for the widespread use of gas-phase processes in preference to hquid-phase processes in cascades for achieving difficult separations becomes clear. 

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