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Other Operating Methods A useful control method for difficult industrial or laboratory distillations is cycling operation. The most common form of cycling control is operating the column at total reflux until equilibrium is established, taking off the complete distillate for a short period of time, and then returning to total reflux. An alternative scheme is to interrupt vapor flow to the column periodically by the use of a solenoid-operated butterfly valve in the vapor line from the pot. In both cases, equations necessary to describe the system are very complex, as shown by Schrodt et al. [Chem. Eng. Sci., 22, 759 (1967)]. The most reliable method for establishing the cycle relationships is by experimental trial on an operating column. Several investigators have also proposed that batch distillation can beprogrammed to attain time optimization by proper variation of the reflux ratio. A comprehensive discussion is presented by Coward [Chem. Eng. Sci., 22, 503 (1967)].

The choice of operating mode depends upon characteristics of the specific system, the product specifications, and the engineer's preference in setting up a control sequence. Probably the most direct and most common method is constant reflux. Operation can be regulated by a timed reflux splitter, a ratio controller, or simply a pair of rotame-ters. Since composition is changing with time, some way must be found to estimate the average accumulated-distillate composition in order to define the end point. This is no problem when the specification is not critical or the change in distillate composition is sharply defined. When the composition of the distillate changes slowly with time, the cut point is more difficult to determine. Operating with constant composition (varying reflux), the specification is automatically achieved if control can be linked to concentration or some concentration-sensitive physical variable. The relative advantage, ratewise, of the two systems depends upon the materials being separated and upon the number of theoretical plates in the column. Results of a comparison of distillation rates by using the same initial and final pot composition for the system benzene-toluene are given in Fig. 13-104. Typical control instrumentation is presented in an article by Block [Chem. Eng., 74, 147 (Jan. 16, 1967)]. Control procedures for reflux and vapor-cycling operation and for the time-optimal process are largely a matter of empirical trial.

Effect of Column Holdup When the holdup of liquid on the trays and in the condenser is not negligible compared with the holdup in the pot, the distillate composition at constant-reflux ratio changes with time at a different rate than when the column holdup is negligible because of two separate effects. First, with an appreciable column holdup, composition of the charge to the pot will be higher in the light component than the pot composition at the start of the distillation; the reason for this is that before product takeoff begins, column holdup must be supplied, and its average composition is higher than that of the charge liquid from which it is supplied. Thus, when overhead takeoff begins, the pot composition is lower than it would be if there were no column holdup and separation is more difficult. The second effect of column holdup is to slow the rate of exchange of the components; the holdup exerts an inertia effect, which prevents compositions from changing as rapidly as they would otherwise, and the degree of separation is usually improved. As both these effects occur at the same time and change in importance during the course of distillation, it is difficult, without rigorous calculations, to predict whether the overall effect of holdup will be favorable or detrimental; it is equally difficult to estimate the magnitude of the holdup effect.

Although a number of studies were made and approximate methods developed for predicting the effect of liquid holdup in the period of the 1950s and 1960s, as summarized in the 6th edition of Perry's Chemical Engineers' Handbook, the complexity of the effect of liquid holdup is such that it is now best to use computer-based batch-distillation algorithms to determine the effect of holdup on a case-by-case basis.

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