o the ine FS. ~ * ~~ and locate the point M on ie line ER through the poii praw the tie line rougn the point M. The term; eat () and raffinate concentrations, yp and xp. The amount often the te line Bive the extract (Eand R) and the percentage of the solute Separated from th teat and raffinate phases from Eqs. (8.3) and (8.4) or Eq, (8.7), le feed can now be calculated it required percentage Separation of the solute is ' pecaleasted. However, this will involve a tia and-enor te necessary solvent rate ple 8.2 using the right triangular coordinate, Procedure. This is illustrated in wu AMPLE 8.2 (Single-stage extraction) One-thousand fi (6.3,ining 50% acetone is: contacted With 800. kz of chloroteen en oe souation qnoved. Equilibri qeous phiase’ one pe 7 Gites -Acetenie Water cea ea a WY se HOM a, ee 08872, 7869 4 0942 DAE. v. ors 0 7 i ee BE MRE So aaa SE eae ~ Solution 2 Given: mass of the feed, F = 10007 kg; mass fraction acetor the mass fraction of chlorobénzene in the feed, xp - = 0, mass, S= 800 kg; Yes = 0.005; ne (C) in the feed, xep = 0.5; and — , (a) Solvent: Yas = 0.995 From Egs. (83) and ©) Prop +8 ep += 1800 AMC EET LE = 10000105) + (800), are plotted using the right triangular coord 1800 Fi The equilibsium aac the diagram; the point 4¢ jg Fand So ooh pis determined tl aking tie line R& Scanned with CamScannerDesign Caleulations for Stage- Wise Extraction 439 gives the equilibrium ; curve alongside on the same scale. Itis to be noted that a point on the xe~¥e Cure Em corresponds ‘Cousentrations ofthe solute (C) inthe two phases. The point ? on the x-Yo ap i \d the extract, . mee ae 880) or 8.800), the solute concentrations in the raffinate () an se are: oe xen = 0.236 and Yor = 0.302 From Eqs. (8.3) and (8.7), 28 ~ 0.236 0302= 0.28 = [362.4 kj Mass of acetone leaving with the raffinate = (R)Gcx) = (1200)(0.302) = [362.4 ke = E=[1200kg E+R=1800 and pales Figure®.8 Single-stage extraction calculation itustrated: (a) Right viangular coordinate, and(t) x-y diagram. Mass of acetone in the feed = (1000)(0.5) = 500 kg Acetone entering with the solvent = (800)(0.005) = 4 kg ‘Net amount of acetone transported to the extract stream = 362.4 - 4 = 358.4 kg Fraction of acetone removed by extraction = at ie. 111% (b) If 90% of the acetone is removed, acetone remaining in the aqueous phase = (500)(0.1) = 50 kg and ni ‘o be noted that at this low concentration of the solute, the mutual solubility of water betas is negligible, Therefore, the raffinate may be assumed to be virtually free from. zene. Then the concentration of acetone in the raffinate is 50/550 = 0.0909. At xx = 0.0909, we have libri , Yo = 0.105 (from the equilibrium curve). Also the mass of the raffinate, R = 550 kg “ Scanned with CamScanner440 Coaprer 8 Liguid-Liguid Extraction If Sis the mass of the solvent required, we can write the following material balance for the. solute, (1000)(0.5) + (S)(0.005) = (S + 450)(0.105) + (550)(0.0909) = $ = 4027 kg 8.4.2 Determination of the Tie Line Through a Point on-the Equilibrium Line ; from G; that meets the conjugate li ical li igate line at K;. A verti libri at H). Then GH, is the tie line through the hp Sines Beet he eit cae (or Scanned with CamScannerChapter 8 Liguid-Liguid Extraction AMPLE 8.3 (Cross-current extraction caleulation) One thousand kilograms of an aqueous # jon containing 35 mass% trimethyl amine (TMA) and 65% water is to be extracted using pe as the solvent. A three-stage ctosé-current extraction scheme is suggested, The amounts 4 si colvent (98% benzene, 2% TMA) to be used in successive stages are 815 kg, 950 kg and’ Ve el vt Ske. Determine the fraction of the s6lute removed if the: stages ate ideal. The compositions jhe raffinate and the extract (two phases) as.well as the tie-line data are given below (water: spenzene: B; TMA: C). $ ring i seosich phase: 3p 0004” 01008". oot 003” ‘does = oor aa? 3) ma xo 005 Of". ons 0% 050 0am flow . ae 095 090.” aay" 7" 063 phase: yp E A 06 050° os may yas ang ee de 005 0d” a5 ww 0% a4 © the plis dam eo 00K. 0083" Gag. Ye * G35" 0088." Jojgg: (8.9) lution extraction he problem is solved using the right triangular coordinate, ns a Ge fing Fee P= 1000 kg, Feed composition: 35% TMA (xcp = 0.35); 659% water Gar = 0.65). ine Procedure The equilibrium data are plotted and the tie lines are drawn (dotted lines) in Figure 8.11. 05 at. Putting 19 o4 Equilibrium curve int M, is ating the 03 Ie points 10% nothing 02 yoint Ry ated on 1 i ou a give Ry tacitly oo Ss nown. “0.0 02 04 - 06 os 10 stages 0 tute ie < Figure 6.11 Grenier = 0.98, yes = 0.02 (2% TMA, nt rate, S, = 815 kgs Ya, rest benzene). Jy. and Stage 1: The ven eee [(1000)(0.35) + 815)O.02)/1815 = 0.202 ee My = 1000 + cs = 0.02) te located on the diagram, The rein 20, xep = 0:35), 5 (in = 0.98 2 is dew Jt The points F in ine PS Gan 0.202). Te te ie Rui ean THIS point My is Toca em apositins of the raffinate and extrac ove the tie line give phe e i the extremities of -° phases leaving stage 1 in equilibrium. 5 Scanned with CamScannerDesign Calculations for Stage-Wise Extraction 443 From the figure, cri = 0.24; yog = 0.166 Total material balance: Eq. (8.3), M, = R, + Ey = 1815 @ Solute balance: MD Gca) = Rida) + EdOce > (1815)(0.202) = (R,)(0.24) + (E,)(0.166) Gi) Solving the material balance equations (i) and (ii), Ry = | 882 kg |; E, =| 933 kg Stage 2: The raffinate from stage 1 (R,) is the feed to stage 2. Solvent added, S, = 950 kg; Jose = 0.02. Mz = Ry + Sz = 882 + 950 = 1832 kg; solute balance: Maxcun = (Ricca) + (Ses) Putting the values of different quantities, xcyyp = 0.126. The composition of the solvent to the second stage being the same as that to the first, it is Tepresented by the same point S. The line R,S is joined and the point M (x4qo = 0.126) is located on this line as shown in Figure 8.11. The tie line Ry is drawn through the point Mp. The compositions of the raffinate and the extract phases from stage 2 are obtained from the figure as: xem =0.15 and —yeg) = 0.105 Material balance equations similar to Eqs. (i) and (ji) are written. Solving these equations, we get R,=[8543kg] & = [977.7 kg Stage 3: Similarly, the third stage receives Ry = 854.3 kg ‘feed’ and Sy = 2625 kg of the solvent. Proceeding in the same way we can locate the point Ms (x43 = 0.052) on the line RpS and draw the tie Tine through M; to meet the equilibrium curve at the points Ry (xcgs = 0.0596) and Es O'ces = 0.0506). The amounts of the phases can be obtained from material balance as before: Ry = [5408 kg and E3 = [29385 kg] Total amount of TMA leaving the stages = Ev0ce) + E)0ce) + (Eee) = (933)(0.166) + (977.7)(0.105) + (2938.5)(0.0506) = 406.2 kg Total amount of TMA entering the three stages with the solvent = (Si + Sp + S3)Qcs) = (815 + 950+ 2625)(0.02) = 87.8 kg Net amount of TMA removed = 406.2 ~ 87.8 = 318.4 kg ‘Total amount of solute in the feed = (1000)(0.35) = 350 kg Fraction of TMA removed = (318.4/350)(100) = [91% 8.4.4 Countercurrent Extraction—Determination of the Number of Ideal Stages A countercurrent extraction cascade, along with the flow rates and concentrations of the i and output streams.at.the stages, is shown in Fig ae jure 8.12. The concentrations and flow rates Scanned with CamScannerTNR yy cores ttn posting the values of he mater 1 = 396.6 kgs mass of the underflow = 1 , 5 oe Nas ‘ ms O75 S ass of the overflow = VL 4 L = 1695 - 396.6 line £44 the the gra balance Bays. (9 Hance Eqs, (9.6) and (9.7), we get 396.601 4 203 y= 12017 = 12984 kp * . 2v) = (1298.4\(1 4.0) = 129 Neving 0493 praction of the oil extracted = WV OydF = (1298, fei ae ae “eee MOMSI9S = 0.796, ve, (760% | encom Ths erence between the fractional extraction figures j « Ted < gecmoe eating he wea on figures in parts (a) and (b) arises from ( 9.6.2 Cross-current Contact The schematic of a three-sta “stage Cross-current contact unit is shown in Figure 9 is ts similar PER E_ 1 Figure 4.16). The flow rates and the consentak hown in Figure 9.14 (this is simil 2385) from different se centrations of the input and output streams to and sand ‘ages are also shown. The underflow from the first ‘Stage is pumped to the second age and so on, Extraction calculations can be done graphically as illustrated in Exarnple 9:3 Yin2y, Solution 2 We shall solve the problem by graphical construction using the X-Y-Z diagram. Consider stage 1 (see Figure 9.14). The input streams are: F = 1000 kg, (xc) = 0.195; S = 500 kg, (ve)s = 0. The quantities expressed on solid-free basis are: F’ = 195 kg, Zp = 805/195 = 4.13; S’ = 500, Zy = 0 (no solid in the feed solvent). The mass and solid content of the mixed stream in stage 1, M{,=F’ or: % $59" = 195 + 500 = 695; Zy; = (805 + ones 7 XoYe The points F’ and S’ are located on the ‘Ponchon— nataiy | Savarit’ diagram (Figure 9.15). The point Mj is Fa epoca yan located on the line S“F’ such that Zy; = 1.16. The tie rchon-Sa Scanned with CamScannernL ——_ Solid-Liquid Extraction Calculations 495 i 7), we { eet line £{V4 through Af; (L4V% is a vertical line for the given ‘equilibrium data’) is dawn.!From { 7 kg the graph, 24; = 1.96, Zy, « 0. { Writing a “solid balance’, we get olid-free), Lida + Feu, = £501.96) 4 ViQ0) = (695K1.16) = £5 = 411; Vi = 284, oe] Now consider sta 8¢ 2. The inputs to stage 2 are the streams L/ Amount and the coy ind 5" If M3 and Zys are the ' mount a meentration ofthe mixed stream, the point Mf can be located onthe [gd joining i ises from Hand S’, ; M3 = Li +S’ = 411 + 500 = 911; 2us = (ALN(L.96) + (S00(0)V911 = 0.884 ' The tie line ZV} passing through ‘Mj is drawn, From the graph, Zu = 2.02, Zy,= 0. : Again, by a ‘solid balance’, eae 1iliy + Vidvs= MiZig= 805 => 14 = 2985, V4 = 911 - 398.5 = 5125 po i By the same procedure we can construct the tic line for stage 3. 5 93, _ MS = 14 +S” = 398.5 + 500 = 808, Also from a material balance, (Zy) + WY Zy) = (M5)(Zy4s) = (L5)(2.04) + (V5)(0) = (898.5)(0.896) i = Ly = 394.6; V5 = 898.5 — 394.6 = 504 Mass of oil leaving with the underflow from stage 3 = (Aleay Fractional oil recovery = (195 - 21.7)/195 = 0.89, ic. 39% Tt has been found in Example 9.2 that the recovery of ol is about 75% if all the solvent is, used in a single-stage. = (394.6(0.055) = 21.7 kg. 9.6.3 Countercurrent Contact An N-stage countercurrent extraction cascade is schematically shown in Figure 9.16. The flow rates are expressed on ‘solid-free basis’, and the solution concentrations in the | overflow and in the undecflow are given in mass fraction of the solute on ‘solid-fre bass” [Xe : or Yc, kg Chkg (B + Q). i (Envelope I) } Ly ii ty thy ly { \; 1 Wa, Veer Woes ( y 08 a : Woz \\_ Won Yoneit_\\ ow Cos i % % Veet! Wy t t Scanned with CamScannerzie ye Styg tution retained in the solid is constant, T= Vs p> qhuces 10 V’) as well, the above equation VA Tht = Xp 4 rYo- KX, pe Voll’ (9.15) gwe further assume that the co, and oe ie. X, = ¥,), the above difference ing the pense te canal aes wien ‘ing the procedure described in = £) and a constant overniow ( neentrations of the overt equation can t general solution low be solved followi X= Kr + (Xr, K utting n=O, the value ofthe constant K’can be found out Again puting n= N, the foll tion for the number of stages W can be obtained (Chen, 1964), = constant (9.16) lowing (9.17) Solution Mass of inerts = 750 kg/h; mass —s= (750)(0.45) = 337.5 kg/h of solute entering = 220 kg/h; solution leaving with the inerts i Mass of solute leaving with the sludge (for 99% recovery) = (2200.01) = 2.2 kg/h; solute concentration in the liquor entrained in the sludge leaving the battery = 2.2/337.5 = 0.00652 mass ; -uaction (solid-free basis) = X,. “L, The strong solution leaving the battery has 16% solute in it (Yy = 0.16). We make a solute ota material balance. : the 2.2 + [my ~ (337.5 - 2.2)1(0.16/0.84) = 220 = my = 1478.75 kgf ate (Solute leaving (Solute leaving with the | bi with the sludge) strong solution) Note: Water entering with the feed = 30 3a feed); 3b= kg; m, = water entering (including that present in the water leaving with the sludge = 337.5 — 2.2 = 335.3; water leaving with the strong liquor m, ~ 335.3; water entering as solvent = Vo = 1478.75 - 30 = 1448.75] = 1=VGL' = 1448,75/337.5 = 4.293; Xy © ¥y) = 0.16; Yo=0=Xq X, = 0.00652 Patitg the values in Eq. (9.17), the required number of stages, N=3|, Scanned with CamScannerSupercritical Fluid Extraction 499 The preceding techniques of determination of the number of stages can be used for the clesign of a continuous extractor (for example, a moving belt or even a moving basket extractor) i the ‘equivalent length’ of the extractor corresponding to a stage is defined and estimated. Thus, the length of a moving belt extractor for a particular separation is the product of the number of stages and the equivalent length. Since an extractor plant uses volatile solvents, due consideration should be given at the time of design to safety and health hazard. Disposal of the solid waste should also be taken care of. 9.7 SUPERCRITICAL FLUID EXTRACTION Lixtraction of a solute from a solid (less frequently from a solution) using a supercritical fluid is a recent addition to separation technology. A fluid is called supercritical if both the temperature and pressure are above the critical values. At supercritical state, a fluid remains as 2 highly condensed phase and may have a density even more than its density in the liquid state. The state and density of CO», the most widely used supercritical solvent, is shown on the pressure temperature plane in Figure 9.19. The constant density lines as well as the supercritical region are indicated. The density may be as high as 1200 kg/m”. 350 1100 ke/m? 300 are indicated). Figure 9.19 Pressure-temperalure diagram for CO2 (constant density lines t capacity norattl ana of a liquid. The solvent ty Scanned with CamScanner