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Distillation Notes PartIV

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521 views

Distillation Notes PartIV

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Immanuel Reji
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286 Mass Transfer—Theory and Practice WORKED EXAMPLES 1, Compute the equilibrium data from the following data at 760 mm Hg pressure and calculate the relative volatility. ‘VP of A, mm Hg | 760 | 830) 920 | 1060 | 1200] 1360 ‘VP of B,mm Hg | 200 | 350 | 420] 550| 690) 760 Pr = 760 mm Hg Solution. P,,mmHg | 760 | 830 | 920 | 1060 | 1200 | 1360 Ps,mmHg | 200 | 350 | 420 | 550 | 690 | 760 P,P, P, We know that »-[2-2 ana, = [20] x, =| S- 1.0 }0.854| 0.68 | 0.412] 0.137/0 4 La Pa) ° ° - “ " P, va -[%e2] 1.0 | 0.933 | 0.823 | 0.575 | 0.216 | 0 @,, = VP of A/VP of B} 3.80 | 2.37 |2.19 | 1.93 | 1.74 | 1.79 Average relative volatility: 2.303 2. The vapour pressure data for n-Hexane ~n-Octane system is given below. Compute the equilibrium data and relative volatility for the system at a total pressure of 101.32 kPa. TPC n-Hexane n-Octane P, kPa (A) P,kPa (B) 68.7 101.32 16.1 79.4 136.7 23.1 93.3 197.3 37.1 107.2 284.0 57.9 125.7 456.0 101.32 Distillation 287 Solution. Te | n= Oclane RP Pika Hexane | PokPa(B) | P4/Pe| *4~(P,—P5)| 4" |?” te@=Dal Pa kPa a) 7 [ 10132 | 161 629 | __ 1000 1.00 1.000 794 | 1367 | 230 592 | 0.689 0.930 0923 933 1973 | 371 332] 0401 O7a1 0783 1072 | 2840 | 579 491] 0.192 0538 0562 1257 | 4560 | 10132_| 450 0 0 0 3. Compute x-y data at 1 atm, Pressure from the following data: i: 80.1 85 90} 95} 100} 105] 110.6 VP, | 760} 877| 1016| 1168] 1344] 1532] 1800 VPa -| 345| 405] 475] 577| 645| 760 Solution. zi 80.1} 85 | 90 | 95 | 100 | 105 | 110.6 VPA 760 | 877 | 1016 | 1168 | 1344 | 1532 | 1800 vP, | — | 345 | 405 | 475 | 577 | 645 | 760 _ VP, a= 74 | — | 254] 251 | 2.46 | 2.33 | 2.38 | 2.37 VP, (P,P, x, =| 42 | | 1.0] 0.78 | 0.58 | 0.411 | 0.239 | 0.13 | 0 (Px - Pa) : ve 4. A solution of methanol and ethanol are substantially ideal. Compute the VLE for this system at 1 atm pressure and relative volatility. .0 | 0.9 | 0.777 | 0.632 | 0.423 | 0.26 | 0 1473.11 Jog [P, mm] senart = 7.84863 - G55 ey 1554.3 log [P, mm] spans = 804494 — G9 Te sey Solution. In this problem one has to compute the vapour pressure values at different temperatures. ‘The temperature range is fixed by keeping the pressure as 288 Mass Transfer—Theory and Practice 760 mm Hg for each component. Thus, in the following equation for Methanol, 1473.11 (230+ °C) Setting the vapour pressure as 760 mm Hg (at BP, vapour pressure equals the prevailing pressure), we get the temperature as 66.53°C, which is the boiling point of Methanol. Similarly, by setting P as 760 mm Hg in the equation for ethanol, log [P, mm] settanat = 7.84863 ~ 1554.3 (222.65 + t°C) we get the boiling point of Ethanol as 78.33°C. This fixes the range of. temperature. Jog [P, mm] pinanoi = 8.04494 — eC 66.53 | 70 | 72 4 76 | 78 78.3: V.P. of Methanol, Pymm 760 | 867.5 | 934.94 |1006.6 [1082.79 [1163.6 [1177.4 V.P. of Ethanol, P,mm 467.8 | $41.77 | 588.66 | 638.9 | 692.66 | 750.14 | 760 Relative volatility, P R 1.625] 1.601] 1.588] 1.576] 1.563, 1.551 | 1.549, 10 | 067 | 0.495] 0.329} 0.173, 0.024] 00 1.0 | 0.765} 0.609 0.436] 0.244 0.0365) 0.0 Average relative volatility = 1.579 Methanol and Ethanol form an ideal solution. Compute the VLE data at 760 mm Hg pressure, Vapour pressure Data: Vapour pressure, mm Hg | 200 | 400 | 760 | 1520 ‘Temperature,°C, Ethanol | 48.4 | 62.5 | 78.4| 97.5 Temperature,°C, Methanol | 34.8 | 49.9 | 64.7| 84.0 Plot vapour pressure vs temperature for both the components and compute T vs. VP for Methanol and T vs. VP for Ethanol as shown in Fig. 9.34. 289 Solution. 100 90 Ethanol 80 £ ie Methanol ae an 50 40 30 200 400 600 800 1000 +1200 +1400 1600 Vapour pressure, mm Hg Fig. 9.34 Example 5 Vapour Pressure-temperature plot. VP. of VP. of Temperature. | Ethanol, | Methanol, mm Hg (B) | mm Hg (A) 64.7 430 760 1.0 10 610 470 830 0.806 0.880 70.0 540 950 0.537 0.671 73.0 620 1080 0.304 0.432 76.0 700 1200 0.120 0.189 78.4 760 1300 0.0 0.0 6. It is desired to separate a feed mixture containing 40% heptane and 60% ethyl benzene, such that 60% of the feed is distilled out. Estimate the composition of the residue and distillate when the distillation process is (i) equilibrium distillation, and (ii) differential distillation. Equilibrium Data: x{0} 0.08 | 0.185 | 0.251 | 0.335 | 0.489 | 0.651 | 0.79 | 0.914 | 1.0 y| 0} 0.233 | 0.428 | 0.514 | 0.608 | 0.729 | 0.814 | 0.910 | 0.963 | 1.0 +, y: Mole fraction of heptane in liquid and vapour phase respectively. 290 — Mass Transfer—Theory and Practice Solution. (i Plot the equilibrium data and draw the diagonal. Draw a line with a slope of -W/D diagonal corresponding to xf = 0.4 and its intersection on the equilibrium curve and read them as x, and yp as shown in Fig. 9.35. - 0.4/0. Sy = 0.24 and yp = 0.5 0 02 Fig. 9.35 Example 6 Solution for flash distillation. (ii) Compute 04 06 — 08 10 and plot it against x as shown in Fig. 9.36 0.667 from a point on the yor x 0 Joos Jo1ss [o2si [0335 [oss9 [oss [07 osi4 | 10 y 0 [0233 [0428 [0514 [0608 [0729 |osi4 [os 0963 | 10 y-x_ [0 [0153 [0243 [0263 [0273 0163 [012 [009 | 0 sax |@ [654 [412 [3.80 | 366 613 |833- |20a1 law We know that a dey, RG=s 0.916 By trial and error, find the x-co-ordinate which will give the area under the curve as 0.916 from zp = 0.4. x, = 0.2. By making component balance, Yp = 0.533. 1. Distillation 291 Xw Xe ot 02 O4 06 08 x Fig. 9.36 Example 6 Solution for differential distillation. A feed mixture containing 50 mole % Hexane and 50 mole % Octane is fed into a pipe still through a pressure reducing valve and flashed into a chamber. The fraction of feed converted to vapour is 0.6. Find the composition of the distillate and residue x 0] 45 | 192 | 40 [69 100 y 0 | 17.8 | 53.8 | 78 | 93.2 100 x, y mole percent of Hexane in liquid and vapour phase respectively Solution. Draw the equilibrium curve and diagonal. From the feed point draw a line with a slope of w a4, [-$ = 9g = 70.667 From graph shown in Fig. 9.37, we get Ay = 0.275, yp = 0.65 292 Mass Transfer—Theory and Practice 10 08 Yo" 085; 7 02 9275 04 05 06 08 10 x— Fig. 9.37 Example 7 Flash distillation. 8. A equimolar feed mixture containing A and B is differentially distilled such that 70% of the feed is distilled out. Estimate the composition of the distillate and residue. Equilibrium data x |0 |1 |8 |14)21| 29) 37| 46 | 56 | 66 | 97 | 100 y |O |3 | 16} 28] 39| 50] 59 | 65 | 76 | 83 | 99| 100 x, y: mole fraction of benzene in liquid and vapour phase respectively. Solution. x 0 | 0.01 | 0.08 | 0.14 | 0.21 | 0.29 | 0.37 | 0.46 | 0.56 | 0.66 | 0.97) 1.0 y 0 | 0.03 | 0.16 | 0.28 | 0.39 | 0.50 | 0.59 | 0.65 | 0.76 | 0.83 | 0.99 | 1.0 yx | 0 | 0.02 | 0.08 | 0.14 | 0.18 | 0.21 | 0.22 | 0.19 | 0.20 | 0.17} 0.02] 0 <= | a@| 50 | 125] 7.14 | 5.56 | 4.76 | 4.55 | 5.26| 5.0 | 5.88] so | a Distillation Plot We know that, against x as shown in Fig. 9.38 dey) F sy (YX) Ww Let the feed be 100 moles Therefore, D = 70 moles and W = 30 moles h F I 100 nl 7 | =!| "30 | = 1208 ay By trial and error, locate x,, such that J Ga» = 1204 yrx We get, %y = 0.23 Making material balance, we get F=W+D Fxg = W xy + Dyp Substituting for various quantities, we get 100 x 0.5 = 30 x 0.23 + 70 x yp Solving, we get, yo = 0.616 10 he 00 02 040506 08 10 ~— Fig. 9.38 Example 8 Solution for differential distillation, 293 294 Mass Transfer—Theory and Practice 9. A liquid mixture of components A and B containing 30 mole percent A is subjected to differential distillation. What percentage of the original mixture must be distilled off in order to increase the concentration of A in the residue to 65 mole percent? The relative volatility of B in respect of A is 2.15. Solution. ; F Solving, |] =7. solving, we get [F| 115 Therefore, if F = 100 kmol, W = 12.91 kmol. Hence, 87.09% of feed has to be distilled. 10. Nitrobenzene (NB) has to be steam distilled. If the vaporization efficiency is 85%, estimate the amount of nitrobenzene in the distillate if 100 kg of steam is present in distillate. The distillation takes place at a total pressure of 760 mm Hg. Vapour pressure data for nitrobenzene: TC 44.47 71.6 [84.9 [99.3 [115.4 [125.8 [139.9 185.8 [210.6 VPofNBmmHg | 1 | 5 |10 |20 | 40 | 60 [100 |400 |760 Vapour pressure of water: TC 20 | 40 | 6 | 80 100 VP of water, mmHg | 17.5 | 55.3 | 149.4 | 355.1 | 760 TCC) | 71 78 80 82 90 96 100 Ps 5 75 9 10 14 io 4\Pi Pa 2425 |340 |355 [4125 |515 | 605 760 Solution. From total vapour pressure curve: Boiling point of mixture = 99.0°C At 99°C, vapour pressure of nitrobenzene = 20 mm Hg vapour pressure of water = 740 mm Hg Distillation 295 Vaporization 7) = [(Actual NB/Actual water)] [ Actual NB | ‘Actual water a [ Theoretical NB ] an in moles) Theoretical water 0.85 = ‘Actual NB Theoretical NB Rctual water = °'°5 * | Theoretical water = 0.85 x 20 x 123 740 x 18 = 0.85 0.1847 = 0.157 kg of NB/kg of steam Mass of NB per 100 kg of steam = 15.7 kg kg of NB/kg of steam 800 760 700 ‘Sum of vapour pressures 650 Smemene & Vapour pressure, rm Hg —> Bag 2 40 60 80 100 120 140 160 180 200 220 ro Fig. 9.39 Example 10 Determination of boiling point for steam distillation. 296 11. Mass Transfer—Theory and Practice A methanol-water solution containing 36 mole % methanol at 26.7°C is continuously distilled to yield a distillate containing 91.5 mole % methanol and a residue containing 99 mole % water. The feed enters at its bubble point. Distillate is totally condensed and refluxed at its bubble point. (i) Find the minimum reflux ratio. (ii) For a reflux ratio of 3, estimate the number of plates by Ponchon-Savarit method. Enthalpy data: xory mole Enthalpies of Enthalpies of ‘fraction of saturated liquid saturated vapour methanol kJ/mol kJ/kmol 0 8000 48000 1 7500 39000 Equilibrium data: x% | 4 10 | 20 | 30 | 50 | 70 | 90 | 95 y% | 23 42 58 66 78 87 96 | 98.15 x, y are mole fractions of methanol in liquid and vapour phase respectively. Solution. @ xp = 036, % = (1-099) = 001, xp = 0.915 Both feed and Reflux are at bubble point. Plot H-x-y diagram and xy diagram as shown in Fig. 9.40. By intrapolation, Hg, = 39765 ki/kmol Locate F corresponding to xp = 0.36 on the bubble point curve. Through F draw a tie line and extend it to intersect the vertical line drawn at xp = 0.915 Poin (from graph) = 62500 ki/kmol (Qnin = Ho,) _ (62500 - 39765) _ Rain = (Hg, —H,) ~ G9165— 7542.5) 7056 ‘Minimum reflux ratio = 0.7056 Gi) For R=3 pe a Ha) __(O'-39765) (Hg, —Hi,) G9765— 7542.5) Q = 136432.5 ki/kmol Enthalpy, klknoie —e 140000. 120000. 100000. ‘20000: 60000 40000 a 03 02 0. Distillation Xy=0.01 0.915 02 o4 06 08 x 10 x— Fig. 9.40 Example 11 Ponchon-Savarit method. 297 298 Mass Transfer—Theory and Practice 12. We know that Ap, Aw and F (Zp, Hp) lie on a straight line (Zp -2y) _ (Hp -Q") (p-%r) (Q'- Hr) Q” = -73004.5 kJ/kmol Locate Ap(’, xp) and A,(Q”, x4) on Hyy diagram. Randomly draw construction lines starting from Ap and A, and obtain the operating curves for both sections on xy-diagram. Stepwise construction between equilibrium curve and operating curve will give the number of stages. Number of stages (including reboiler) = 6 Number of plates in tower = 6 - 1 = 5 A continuous distillation column is used to separate a feed mixture at its boiling point, containing 24 mole % acetone and 76 mole % methanol into a distillate product containing 77 mole % acetone and a residue product containing 5 mole % acetone. A reflux ratio of twice the minimum is to be used. The overall plate efficiency is 60%. Determine the number of plates required for the separation. Equilibrium data: x | 0.0} 0.05| 01 | 02 | 03 | 04 | OS | 06 | 0.7 [08 109 [1.0 y | 0.0 [0.102 [0.186] 0.322 [0.428 [0.513 [0.586] 0.656]0.725 [0.82 [09 [1.0 Solution. x, y Mole fraction of acetone in liquid and vapour phase respectively. tp =0.24, xp =0.77, x, = 0.05 Rectuat = 2Rmin Nevers = 60% Plot xy diagram and draw the feed line with its corresponding slope of infinity to equilibrium curve and let it be F. Let the point D on the diagonal corresponds to xp. Join DF and extend it to y-axis. The point of intersection is Xp - Reg 1 * 0-19 (from Fig. 9.41) Rin = 3.053 Ractuat = 6.106 xp _ O77 | Racuar +1 ~ 7.106 eee Locate 0.108 on y-axis and let it be A. Join AD. The point of intersection of AD with feed line is Q. DQ is the operating line for enriching section. Locate W on diagonal corresponding to xy = 0.05. Join W and Q. WO is the operating line for stripping section. By stepwise construction the number of stages = 14 (including reboiler) Number of plates is 13 (Theoretical) Actual number of plates = a = 21,7, ie. 22 plates Distillation 299 02 o4 06 os 10 Fig. 9.41 Example 12 McCabe-Thiele method. 13. A fractionating column separates a liquid mixture entering at 5000 kmol/h containing 50 mole % A and 50 mole % B into an overhead product of 95 mole % A and a bottom product of 96 mole % B. A reflux ratio of twice the minimum will be used and the feed enters at its boiling point. Determine the number of theoretical stages required and the location of feed point. Equilibrium data: x | 0.03 | 0.06 | 0.11 | 0.14] 0.26 | 0.39 | 0.53 | 0.66 | 0.76 | 0.86] 1.0 y | 0.08 | 0.16 | 0.27 | 0.33 | 0.50 | 0.63 | 0.71 | 0.83 | 0.88 | 0.93] 1.0 , y mole fraction of A in liquid and vapour phase respectively. Solution, tp=05, 1p = 0.95, x, = 0.04 Feed-saturated liquid F = 5000 kmol/h Total condenser (i) Total material balance F=D+W Component balance Exp = Dxp + Wey 5000 = D + W ay 300 Mass Transfer—Theory and Practice (5000 x 0.5) = (D x 0.95) + (W x 0.04) @Q 5000 = D+ W Distillate D = 2527.5 kmol/h Residue W = 2472.5 kmol/h Gi) Rain = [p - YO" - **)) (0.95 - 0.720) San [ (0.720 ~ 0.3) | = 1.045 Also, by graphical xp/(Rnin + 1) = 0.46 and Rin = 1.065 (ii) Rycual = 2 * Ravin Racuat = 2% Rin = 2 X 1.045 = 2.09 (Taking Rnin value as 1.045) xp 095 (R+1) (2.0941 oe With the above intercept, draw both enriching and stripping operating curves. By McCabe-Thiele method, Number of plates (including reboiler) = 11 Number of plates in tower = 11 - 1 = 10 The location of feed tray is 6th tray. 10 os: 02 04 ~ 06 08 ~ 1.0 Fig. 9.42 Example 13 McCabe-Thiele method. 14. A mixture of benzene and toluene containing 38 mole % of benzene is to be separated to give a product of 90 mole % benzene at the top, and the bottom product with 4 mole % benzene. The feed enters the column at its Distillation 301 boiling point and vapour leaving the column is simply condensed and provide product and reflux. It is proposed to operate the unit with a reflux ratio of 3.0. Locate the feed plate and number of plates. The vapour pressures of pure benzene and toluene are 1460 and 584 mm Hg respectively. Total pressure is 750 mm Hg. Solution. vapour pressure of pure benzene _ 1460 or = Vapour pressure of pure benzene _ 1460 _ ‘vapour pressure of pure toluene 584 2.5 Soaeanox [1+(@=Dsl Compute equilibrium data. y x]0 | 01 [02] 03] 04] 05] 06 | 07 | 08 | 09 [10 y | o [o22 [038 [052] 063 [0.71 | 0.79 [oss [0.91 [o96[1.0 Draw the equilibrium curve, diagonal and locate feed, distillate and residue points as shown in Fig. 9.43. xp _ 0. [R+1] 341 we can get the number of stages. No. of stages = 8 (including reboiler) and feed plate is 4 Locate the intercept = 2.25 and by stepwise construction 0 "01 02 03 o4 0S 06 o7 O8 o9 10 pe Fig. 9.43. Example 14 McCabe-Thiele method. 802 — Mass Transfer—Theory and Practice 15. It is desired to separate a mixture of 50% vapour and 50% saturated liquid in a plate type distillation column. The feed contains 45 mole % A and the top product is to contain 96 mole % A. The bottom product is to contain 5 mole % A. Determine the minimum reflux ratio and the number of theoretical plates needed if a reflux ratio of twice the minimum is used. Eq, data: x 0 0.1 [0.16] 03 | 04 | 05 | 06 | 0.7 | 08 | 0911.0 y 0 {0.215 | 0.30 | 0.52 | 0.625 | 0.725 | 0.78 | 0.89 | 0.89 | 0.95 | 1.0 x,y : mole fraction of A in liquid and vapour phase respectively. Solution. Xp |e [a = ]033 Rain +1 = 953 Rein = 1-909 q = 05 (Fraction of liquid) Ge ee0 Se Slope of q-line [5] =Osl17 71 Racual = 2.0 X Ryin = 2.0 x 1.909 = 3.818 Yo factual +1 Number of stages = 10 10 os 02 oz oa os os 10 Fig. 9.44 Example 15 McCabe-Thiele method. Distillation 303 16. A fractionating column separates a liquid mixture containing 50 weight % chloroform and 50 weight % carbon disulphide into an overhead product of 94 weight % CS, and a bottom product of 95 weight % chloroform. A reflux ratio of twice the minimum will be used and the feed enters at its boiling point, Determine the number of theoretical stages required. Equilibrium data: x [0.03 [0.06 | 0.11 | 0.14 [0.26 | 0.39 | 0.53 | 0.6 | 0.76 | 086 | 1.0 y [0.08 | 0.16 | 0.27 [0.33 [0.50 [0.63 | 0.71 | 0.83 | 0.88 [0.93 | 1.0 x, y mole fraction of carbon disulphide in liquid and vapour phase respectively. Solution. Molecular weight of carbon disulphide = 76 Molecular weight of chloroform = 119.5 50 weight % of carbon disulphide, (ss) ue = 0.611 (in mole fraction) aps to) T7350, 50 76 * 119.5 Similarly, the distillate and residue compositions in terms of mole fraction of carbon disulphide are yp = 0.961 and x, = 0.076 respectively. From graph (Fig. 9.45), ey] =0.49 Rain = 0.96 Racy = 2X Ryn = 1.92 Therefore, (22a) = 0.329 = 0.33 actual Number of theoretical stages (from Fig. 9.45) including reboiler = 9 17. A laboratory rectification column is operated at atmospheric pressure and at total reflux, for benzene-chlorobenzene mixture. Samples of liquid from the condenser and reboiler analyze 95 mole percent benzene and 98 mole percent chlorobenzene respectively. Assuming a perfect reboiler, a total condenser, constant molal overflow and no heat loss from the tower, calculate the actual number of plates in the column, The average plate efficiency is 70%. The relative volatility of benzene to chlorobenzene is 4.13. 304 Mass Transfer—Theory and Practice 10 08 02 02 04 06 08 1.0 x Fig. 9.45 Example 16 McCabe~Thiele method. Solution. ax >" +@-Dal Compute equilibrium data. x | 0} o1 | 02 | 03 | 04 | os | 06 | 07 | 08 | 09 | 10 y | 0 | 031 | 0.51 | 0.64 | 0.73 | 0.81 | 0.86 | 0.91 | 0.94 | 0.97 | 1.0 Draw the equilibrium curve, diagonal and locate feed, distillate and residue points. By stepwise construction, the number of stages determined is 5. Hence, the theoretical plates required is 4. 4 Actual plates required will be 5.11 ~6. Distillation 305 ° 02 04 06 08 % 10 x Fig. 9.46 Example 17 McCabe-Thiele method. Alternatively, we can use the Fenske equation and determine the number of stages. Yo. Neos Sw =o" Ty) Gm) 0.95 _ og sqNpoy 0.02 T=0.95) ~ 19)" Go.07 19 =(4.13)""*! x 0,02041 Hence, Np + 1 = 4.82 stages~5 stages Therefore, the theoretical number of plates = 4 116 Actual plates required will be a (Same as obtained from the graphical procedure) 18. A continuous rectification column is used to separate a binary mixture of A and B. Distillate is produced at a rate of 100 kmol/hr and contains 98 mole % A. The mole fractions of A in the liquid (x) and in the vapour (9) respectively from the two adjacent ideal plates in the enriching section are as follows:

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