ChE 448 Chemical Engineering Design, Spring 2007

MultiComponent Distillation: Notes, Equations and Problem Statements You know how to calculate the minimum reux ratio for a binary distillation problem (and the minimum number of stages at maximum reux). When distilling a multicomponent system, you cannot operate at less than some minimum value of the reux ratio. For multicomponent systems, the minimum reux ratio is calculated on the basis of separation of two key components, called the light and the heavy key. (You have to choose these two key components) In binary systems, purity is dened by specifying xD , xB . (D stands for Distillate while B is Bottoms, x usually refers to the liquid phases, y is used to represent the gaseous phase). This then xes D and B for a given F. Once the reux ratio is chosen, we can then calculate the number of stages. For multicomponent systems, specifying one concentration in D and B is not sucient. In general, the designer (that is you) will choose two components whose concentrations or fractional recoveries in D and B are good indicators of the separation required. These are the keys; one is the light key (L) and the other is the heavy key (H). The designer assigns small values to xDH and xBL ; i.e. most of the light key should be found in D (the Distillate) while most of the heavy key should be in the B (the Bottoms). (In programs such as ChemCAD, these values may have to be given as percent recoveries of the light and the heavy keys in the distillate when compared to the values in the feed stream - read the manual.) Any two components can be chosen as the keys - if they are adjacent in the rank order or volatility, such a choice will lead to what is called a sharp separation. Ofcourse what you choose as keys will aect the actual separation of the other components (right?) Fenskes equation applies to any two components at reux. log Nmin =
xDi /xBi xDj /xBj

log( ) ij

(1)

i is more volatile than j (i.e. i is light and j is the heavy key) and ij is dened by
1/3

ij = Dij F ij Bij

(2)

i.e. ij is the geometric mean of the s at the temperature of the feed, distillate and the bottoms. Unlike binary systems, in multicomponent systems there are two pinch regions - one above the feed and one below the feed (for minimum reux). An approximate (but fairly accurate) method for calculating Rmin is given by Underwood. Two equations must be solved. i xF i 1q = (3) i 1

Rmin + 1 =

i xDi i

(4)

Ki where i is equal to Kref where Kref is the K value for the heavy key. The correct value of lies between the values of for the keys; i.e. solve the rst equation for , use this value to get Rmin . Notice that while all components of feed are in the rst equation, the second equation contains only those found in the distillate. If there are more than one or more compounds in the feed between the light and the heavy keys, there are 2 or more values of between the s (of the keys) that will satisfy the rst equation. The correct value is found by solving the equations 3 and 4 simultaneously. What about Number of Stages? Precise methods are best done using the computer using rather involved methods. There are a number of techniques which can be used for preliminary estimates. Gillilands correlation requires minimum number of plates at reux by Fenskes method and the minimum reux ratio from Underwoods equation. The correlation is presented as a log-log plot of N N min (call it Y) vs RRmin (call it X). When N +1 R+1 R = Rmin , X = 0 and Y = , when N = Nmin Y = 0 and X 1. There are a number of equations that can be used to represent the plot. The Eduljee Equation is: (5) Y = 0.75(1 X 0.5668 )

and it applies for 0.01 < X < 1, values of X below 0.01 are of little practical importance. The Chung Equation is Y = 1 exp 1.490 + 0.315X Molkanovs Equation is Y = 1 exp (1 + 54.4X)(X 1) (11 + 117.2X)(X 0.5 ) (7) 1.805 X 0.1 (6)

R N When Rmin is 1.3, Gillilands correlation shows that Nmin is 2.0. The Gilliland correlation is OK for preliminary estimates, but has some restrictions:

Number of components must be between 2 through 11 q value must be between 0.28 and 1.42 Pressure must be from vacuum to 600 psig must be between 1.11 and 4.05 Rmin must be between 0.53 and 9.09 Nmin must be from 3.4 to 60.3

More accurate correlations must use q as a parameter, the simple Gilliland correlation appears to be conservative for feeds with low qs. If stripping is more important that rectifying then the Gillilands correlation does not work very well! The most popular method for determining the best feed locations are done using Fenskes equation and the Kirkbridge equation which is given below NR = NS zHK xB,LK B zLK xD,HK D
0.206

(8)

where NR is the number of stages above the feed, while NS is the number of stages below the feed. Since NR + NS = N where N is the total number of stages, we can easily calculate the location of the feed plate. The Fenske equation can be turned inside-out to help estimate the splits of other components, if the split of one is specied. You can show that xDj xDi = (ij Nmin ) (9) xBi xBj The estimated splits are close to being correct even though N is not at minimum. If you multiply the equation by D i.e. Distillate then you get B Bottoms di dj = (ij Nmin ) bi bj If j is the heavy key, the fi = bi + di (material balance on the column) We can show that j fi (ij Nmin ) dj b di = j 1 + (ij Nmin ) dj b (10)

(11)

Notice that in this equation, 11, the i refers to a non-key component while the j is the heavy key component. When you calculate the minimum number of stages, the i was the heavy key, in this equation the i is a non-key component (i.e. its everything other than the heavy key component). D= di (12)

Do the following problems using a Spreadsheet (or MathCAD or Maple or ...) and ChemCAD. 1. A distillation column is to separate 4750 moles of feed composed of 37 mole% nbutane, 32 mole% isopentane, 21 mole% n-pentane and 10 mole% n-hexane. The feed is supplied as a mixture of 75 % liquid, 25 % vapor (i.e. q value is 0.75) The column operates at an average pressure of 2 atm and is required to produce a distillate product containing 95 mole% n-butane. The bottoms should not contain more than 570 moles of n-butane. Use Underwoods method to calculate the minimum reux required Determine the minimum number of stages by Fenskes equation Determine the number of theoretical stages required if the actual reux is 1.2 times the minimum reux. Use the Eduljee Equation 5, the Chung Equation 6 and the Molkanov Equation 7. Are the results dierent? How does it compare with what you get using ChemCAD? Prepare a table comparing the dierent calculations. The approach just described assumes optimal location of the feed stream, and the column is assumed to have one feed and a total condenser. If the splits of the keys are not specied, a key split must be assumed to commence the procedure for determining the number of stages. The column can then be sized according to the technique described below, known as the short-cut method: (Do the problem described above using the shortcut method) (a) Choose the split between the top and bottom for all components not specied, the split must be consistent with purity requirements. (b) Estimate column temperatures: do a dew point temperature for the top from the assumed concentrations, do a bubble point calculation for the bottom, use the temperature of the feed for the middle of the column. Locate K values for the components as a function of temperature at 2.0 atm or use Antoines equation with appropriate constants to calculate saturation vapor pressure. For light hydrocarbon systems, K values are in general not a strong function of composition. How close are the K values calculated using Antoines equation and tabulated values? (if you can locate them) (c) Calculate the geometric mean of the relative volatilities for each component relative to the heavy key, equation 2. (d) Use Fenskes equation to calculate Nmin , equation 1 (e) Using Nmin , calculate the splits of the non-keys using the equation for dii , this is b equation 10. By knowing the total moles of that component entering the column, the amounts in the top and the bottom products may also be determined, using equation 11. The amounts in the bottom products may then be determined from the equation for bi = fi di . 4

(f) If the compositions determined are such that they change the average value of then repeat steps 2 through 5 till you see no change in . (g) With the nal values of the top-product compositon, Underwoods method is used to determine minimum reux. (h) Calculate actual stages from assumed value of reux ratio and Gillilands correlation, use any of the ones given, equations 5, 6 or 7. (i) Use Kirkbridge correlation to calculate feed point, equation 8 2. 100 moles/hour of a saturated liquid feed with the following composition: n-butane (mole fraction 0.40), n-pentane (0.25), n-hexane (0.25) and n-heptane (0.15) is fed to a distillation tower at 405.3 kPa abs. This liquid is to be fractionated so that 90% of the n-pentane is recovered in the distillate and 90% of the n-hexane is recovered in the bottoms. Use Aspenplus or other sources for thermodynamic property calculations. Calculate the temperature of the feed. Calculate the composition of the vapor that would be in equilibrium with this feed Calculate the moles per hour and the composition of the distillate and the bottoms Calculate the temperature at the top (dew point) and the bottom (bubble point) of the tower Calculate the minimum number of stages for total (i.e. ) reux and the distribution of the other components in the distillate and the bottoms. Calculate the minimum reux ratio using Underwoods equation Assuming an actual reux ratio of 1.5 times the minimum, calculate the actual number of theoretical stages using any one of the equations. On which stage is the feed to be introduced?