Reflux Ratios

It must be emphasized that it is not worth expending any effort optimizing pressure, feed condition, or reflux ratio until the overall heat-integration picture has been established. These parameters very often change later in the design. 

No attempt should be made to optimize pressure, reflux ratio, or feed condition of distillation in the early stages of design. The optimal values almost certainly will change later once heat integration with the overall process is considered. 

Porter and Momoh have suggested an approximate but simple method of calculating the total vapor rate for a sequence of simple columns. Start by rewriting Eq. (5.3) with the reflux ratio R defined as a proportion relative to the minimum reflux ratio iimin (typically R/ min = 1-D- Defining Rp to be the ratio Eq. (5.3) becomes... 

Consider again the simple process shown in Fig. 4.4d in which FEED is reacted to PRODUCT. If the process usbs a distillation column as separator, there is a tradeofi" between refiux ratio and the number of plates if the feed and products to the distillation column are fixed, as discussed in Chap. 3 (Fig. 3.7). This, of course, assumes that the reboiler and/or condenser are not heat integrated. If the reboiler and/or condenser are heat integrated, the, tradeoff is quite different from that shown in Fig. 3.7, but we shall return to this point later in Chap. 14. The important thing to note for now is that if the reboiler and condenser are using external utilities, then the tradeoff between reflux ratio and the number of plates does not affect other operations in the flowsheet. It is a local tradeoff. 

Distillation capital costs. The classic optimization in distillation is to tradeoff capital cost of the column against energy cost for the distillation, as shown in Fig. 3.7. This wpuld be carried out with distillation columns operating on utilities and not integrated with the rest of the process. Typically, the optimal ratio of actual to minimum reflux ratio lies in the range 1.05 to 1.1. Practical considerations often prevent a ratio of less than 1.1 being used, as discussed in Chap. 3. 

If, however, the column is appropriately integrated, then the reflux ratio often can be increased without changing the overall energy... 

Thus the optimal reflux ratio for an appropriately integrated distillation column will be problem-specific and is likely to be quite different from that for a stand-alone column. 

R distillation column reflux ratio (-) or heat capacity ratio of 1-2 shell-and-tube heat exchanger (-)... 

This is the ASTM D 2892 test method and corresponds to a laboratory technique defined for a distillation column having 15 to 18 theoretical plates and operating with a 5 1 reflux ratio. The test is commonly known as the TBP for True Boiling Point. 

Reflux ratio. This is defined as the ratio between the number of moles of vapour returned as refluxed liquid to the fractionating column and the number of moles of final product (collected as distillate), both per unit time. The reflux ratio should be varied according to the difficulty of fractionation, rather than be maintained constant a high efficiency of separation requires a liigh reflux ratio. ... 

Otherwise expressed, the number of theoretical plates required for a given separation increases when the reflux ratio is decreased, i.e., when the amount of condensed vapour returned to the colunm is decreased and the amount distilled off becomes greater. 

Beyond certain limits increase of the reflux ratio does not appreciably increase the separating power or efficiency of the column. As a rough guide, if the column has an efficiency of n plates at total reflux, the reflux ratio should be between 2>t/3 and 3n/2. 

Improved results are also secured by the use of a short reflux condenser ( cold finger ), Fig. 11, 56, 22, inserted into the top of the column head the simplest type is shown in Fig. 11, 56, 23. The condenser permits con trol of the reflux ratio by adjusting the rate of flow of water through it. 

Fractional distillation. Fig. II, 60, 2 illustrates a set-up for fractional distillation wdth a Hempel-type column and cold finger, the latter to give manual control of the reflux ratio. Any other fractionating colunm, e.g., an all-glass Dufton or a Widmer column may, of course, be used. 

T.eflux Tatio. Generally, the optimum reflux ratio is below 1.15 and often below 1.05 minimum. At this point, excess reflux is a minor contributor to column inefficiency. When designing for this tolerance, correct vapor—Hquid equiUbrium (VLE) and adequate controls are essential. 

Checking Against Optimum Design. This attempts to answer the question whether a balance needs to be as it is. The first thing to compare against is the best current practice. Information is available ia the Hterature (13) for large-volume chemicals such as NH, CH OH, urea, and ethylene. The second step is to look for obvious violations of good practice on iadividual pieces of equipment. Examples of violations are stack temperatures > 150° C process streams > 120° C, cooled by air or water process streams > 65° C, heated by steam t/ urbine 65% reflux ratio > 1.15 times minimum and excess air > 10% on clean fuels. 

The dominance of distiHation-based methods for the separation of Hquid mixtures makes a number of points about RCM and DRD significant. Residue curves trace the Hquid-phase composition of a simple single-stage batch stiHpot as a function of time. Residue curves also approximate the Hquid composition profiles in continuous staged or packed distillation columns operating at infinite reflux and reboil ratios, and are also indicative of many aspects of the behavior of continuous columns operating at practical reflux ratios (12). 

The once-mn tar acids are fractionated in three continuous-vacuum stills heated by superheated steam or circulating hot oil. These stills contain 40—50 bubble trays and operate at reflux ratios between 15 and 20 1. The overhead product from the first column is 90—95% phenol from the second, 90% (9-cresol and from the third, a 40 60 y -cresol—p-cresol mixture. Further fractionation gives the pure products. 

---