Fundamentals of Industrial Separations, SOLUTIONS TO PROBLEMS

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Chapter 1: INTRODUCTION
Exercise 1.1 Compare and discuss the advantages and disadvantages of making separations using an energyseparating agent (ESA) versus using a mass-separating agent (MSA). Exercise 1.2 The system benzene-toluene adheres closely to Raoult’s law. The vapor pressures of benzene and toluene at 121°C are 300 and 133 kPa. Calculate the relative volatility. Exercise 1.3 As a part of the life system support for spacecrafts it is necessary to provide a means of continuously removing carbon dioxide from air. If it is not possible to rely upon gravity in any way to devise a CO2-air separation process. Suggest at least two separation schemes, which could be suitable for continuous CO2 removal from air under zero gravity conditions. Exercise 1.4 Gold is present in seawater to a concentration level between 10-12 and 10-8 weight fraction, depending upon the location. Briefly evaluate the potential for recovering gold economically from seawater. Exercise 1.5 Assuming that the membrane characteristics are not changed as the upstream pressure increases, will the product-water purity in a reverse-osmosis seawater desalination process increase, remain constant or decrease? Exercise 1.6 Propylene and propane are among the light hydrocarbons produced by thermal and catalytic cracking of heavy petroleum fractions. Although propylene and propane have close boiling points, they are traditionally separated by distillation. Because distillation requires a large numbers of stages and considerable reflux and boilup flow rates compared to the feed flow, considerable attention has been given to the possible replacement of distillation with a more economical and less energy-intensive option. Based on the properties of both species, propose some alternative properties that can be exploited to enhance the selectivity of propylene and propane separation. What separation processes are based on these alternative properties?
Property Molecular weight (kg/mol) VdWaals volume (m3/mol) 2 VdWaals area (m /mol) Acentric factor Dipole moment (Debije) Radius of gyration (m·1010) Melting point (K) Boiling point (K) Critical temperature (K) Critical pressure (MPa) Propylene 0,04208 0,0341 5,06 0,142 0,4 2,25 87,9 225,4 364,8 4,61 Propane 0,04410 0,0376 5,59 0,152 0,0 2,43 85,5 231,1 369,8 4,25

1-2

INTRODUCTION

SOLUTIONS
Exercise 1.1 Compare and discuss the advantages and disadvantages of making separations using an energyseparating agent (ESA) versus using a mass-separating agent (MSA). Answer ESA Advantages Known technology Phase separation Relatively simple High selectivities possible Disadvantages Energy consumption may be expensive Heat integration required Recovery of agent requires additional separation

MSA

Exercise 1.2 Calculate the relative volatility of benzene-toluene. Answer For an ideal system such as benzene-toluene, by definition (Eqs. 1.3 and 1.5)

SF ≡ α ≡

y B / xB P o 300 = B = = 2.26 o (1 − y B ) /(1 − xB ) PT 133

Exercise 1.3 Suggest at least two separation schemes that could be suitable for continuous CO2 removal from air under zero gravity conditions. Answer a. Adsorption of CO2 on activated carbon. Regeneration by exposing to vacuum outside the spacecraft. b. Absorption of CO2 in a suitable solvent at the low temperature outside the vessel. Regeneration of the loaded solvent at room temperature, releasing the overpressure via a valve to the outer space. Exercise 1.4 Briefly evaluate the potential for recovering gold economically from seawater. Answer The lower the concentration of the desired substance, the more expensive the required technology. At the given extremely low concentrations, huge amounts of seawater have to be treated, either by evaporation or by (membrane)filtration. Either method is not feasible due to the highenergy costs or pumping costs. The thermodynamical basis is given by the change in chemical potential upon mixing, which is proportional to ln(activity) a negative value, indicating a spontaneous process. Separation of the mixture, on the other hand, requires at least that amount of work, which is extremely large at very low values of the activity (or concentration).

Fundamentals of Industrial Separations, SOLUTIONS TO PROBLEMS

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Exercise 1.5 Assuming that the membrane characteristics are not changed, as the upstream pressure increases, will the product-water purity in a reverse-osmosis seawater desalination process increase, remain constant or decrease? Answer The water flux is proportional to ΔPext – ΔΠosm and will increase with increasing ΔPext. The salt flux is proportional to cfeed – cpermeate and will not be effected by a change in ΔPext. Hence, the product purity will increase with increasing ΔPext. Exercise 1.6 Based on the properties of propylene and propane, propose some alternative properties that can be exploited to enhance the selectivity of propylene and propane separation. What processes are based on these alternative properties?
Property Molecular weight (kg/mol) VdWaals volume (m3/mol) 2 VdWaals area (m /mol) Acentric factor Dipole moment (Debije) Radius of gyration (m·1010) Melting point (K) Boiling point (K) Critical temperature (K) Critical pressure (Mpa) Propylene 0,04208 0,0341 5,06 0,142 0,4 2,25 87,9 225,4 364,8 4,61 Propane 0,04410 0,0376 5,59 0,152 0,0 2,43 85,5 231,1 369,8 4,25

Answer Difference in molecular weight Difference in VdWaals volume

Difference in dipole moment

Ultracentrifuge Kinetic separation by preferential adsorption of the component with the smallest volume in a molecular sieve adsorbent Absorption, adsorption, extraction or extractive distillation

1-4 INTRODUCTION .

SOLUTIONS TO PROBLEMS 2-1 Chapter 2: EVAPORATION & DISTILLATION Exercise 2. C’ = 362. B’ = 2154.2. B = 2755. lnPi0 = A − B with pressure units in atm and temperature in °C. K.8 1 benzene liquid and vapor mole fractions .3 Vapor-liquid equilibrium data for benzene-toluene are given at 1.4 0.5 atm.0 atm 80 70 0 0.9). °F. Check the phase compositions at 100°C and total pressures of 1.1 In Vapor-Liquid Equilibrium Data Collection the following form of Antoine-equation is used log Pi0 = A′ − 0 B′ T + C′ with Pi saturation pressure in mmHg and temperature T in °C (760 mmHg = 1 atm).3716. Exercise 2.01325 bar and T(°F)=T(°C)·9/5 + 32. the following Antoine constants apply for benzene A’ = 5.2 With temperature in degrees Fahrenheit and pressure in pounds per sq. C = -53.Fundamentals of Industrial Separations. 2. T +C Exercise 2. ‘B = 1196.97 (atm.9. 2.2082. C = -54. inch. B = 3090.0 atm and at 1. B and C in the Antoine-equation as defined in Eq. Noting that 1 atm = 14.696 psi = 1.1°C.64. the Antoine constants for benzene and toluene are.5 atm 100 90 Ptot = 1.5 atm in the T-x diagram below. calculate the saturation pressure of benzene in bar at 80.0 and 1.78.161. 130 120 temperature / C 110 Ptot = 1.2 0.87987. respectively A = 9.1606.00 and A = 9. For benzene in benzene-toluene mixtures the following values are reported: A’ = 6.49 (psi.760 and C’ = 219.6 0. Expressing the saturated vapor pressure in atm as a function of temperature in K. Calculate the constants A. 10log P expression). Eq.

The tray temperature is equal to the feed temperature. The average density of liquid pentane and hexane amounts to 8170 and 7280 mol/m3.40 should produce a liquid with x = 0.5. The distance between the trays amounts to 0. Equilibrium data for the benzene-toluene system can be approximated with a constant relative volatility of 2. c.4 A liquid benzene-toluene mixture with z = 0. Calculate the feed temperature Calculate the vapor stream from the reboiler Calculate the required energy in the reboiler Construct the y-x diagram Construct the operating lines and locate the feed line Determine the number of equilibrium stages Determine the height of the column . what is the corresponding liquid composition and what are the liquid and vapor flow rates? Find the compositions and flow rates of all unknown streams for a two stage flash cascade where 40% of the feed is flashed in the first stage and the liquid product is sent to a second flash chamber where 30% is flashed. The feed.35 in a flash drum at 1. b.50 m. find the liquid and vapor compositions If we desire a vapor composition of 60 mole%. b. a.98.6 Distillation is used to separate pentane from hexane. where benzene is the more volatile component. b. Feed rate to the still is 700 moles/h. a. f. Operation of the still is at 1 atm.05 and xD = 0.5 We wish to flash distill isothermally a mixture containing 45 mole% of benzene and 55 mole% of toluene. g. The heat of vaporization amounts to 30 kJ/mol. resp.25. If 60% of the feed is evaporated. e.2-2 EVAPORATION & DISTILLATION Exercise 2. d. c. Plot the y-x diagram for benzene-toluene.0 atm. enters the column exactly on the feed tray. Exercise 2. The pentane vapor pressure is given by: P5o =e 11*(1− 310 ) T (K) (bar) The vapor pressure of hexane is 1/3 of the pentane vapor pressure over the whole temperature range. The reflux ratio is 2. at the bubbling point. The column pressure is 1 bar. The feed amounts 100 mol/s and has a mole ratio pentane/hexane = 0. a. Calculate the required feed temperature Calculate the equilibrium vapor-liquid ratio in the flash drum. d. The bottom and top products have the compositions xB = 0. Exercise 2.5.

3 kg/h the saturated steam required in kilograms per hour for heat to the reboiler using enthalpy data below Steam: ΔHVAP = 2000 kJ/kg Benzene: ΔHVAP = 380 kJ/kg Toluene: ΔHVAP = 400 kJ/kg Vapor-liquid equilibrium data (1 atm. For an operating pressure of 1 atm.703 0.21 0.79 0. b. It is introduced to the column at its bubble point to the optimal plate. The feed contains 14.40 0.91 0.918 0.8 A feed to a distillation unit consists of 50 mol% benzene in toluene.0321 0.50 0.86 0.12.075 y 0.0 atm.60 0.0523 0.918 0. using a reflux ratio (L’/D) of 50% more than the minimum.30 0. e.96 . Determine the minimum number of stages and minimum reflux Determine the feed stage location and number of theoretical stages required for a reflux ratio of 1.10 0. mole fraction benzene) x 0.516 0. calculate: a.72 0.963 Exercise 2. The distillate is 99 mol% pure.46 kg/h methanol and 10.225 0.813 0. the minimum reflux ratio the minimum number of equilibrium stages to carry out the desired separation the number of actual stages needed.352 0.70 y 0.Fundamentals of Industrial Separations. d. mole fraction methanol) x 0.64 0.80 0.349 0. The feed is subcooled such that q = 1.90 0. The column is to produce a distillate containing 95 mol% benzene and a bottoms of 95 mol% toluene.7 Methanol (M) is to be separated from water (W) by atmospheric distillation.593 0.2940 0.51 0. a.1900 0. SOLUTIONS TO PROBLEMS 2-3 Exercise 2. b. Vapor-liquid equilibrium data (1. the bottom product contains 5 mol% of methanol.154 0. the product and residue stream in kilograms per hour if the feed is 907.20 0. c.37 0.44 kg/hr water.

= A− T + C′ T +C convert the pressure in (I) into form (II) and compare the three resulting constants with A. (760 mmHg = 1 atm) For benzene A’ = 6.1606 [-]. units in psi and °F) A’ = 5. respectively A ′− B′ T ′+C (mmHg) Solution 0 lnPB (atm) = ln 10 B′ ln(10) = A′ ln(10) − ln(760) − T + C′ 760(mmHg/atm) Hence A = A′ ln(10) − ln(760) = ln(10)[A′ − log(760)] B = B′ ln(10) A = 9.16 [°C] C = C’ Given Antoine constants benzene (10logP expression. calculate saturation pressure at this temperature in psi and convert result to bar. Two different approaches: a. 2. B’ = 2154.2-4 EVAPORATION & DISTILLATION SOLUTIONS Exercise 2.1°C = 176. or b.696 psi = 14.696 psi 14. B and C.2082 [-] B = 2755.18+C ′ = 14. convert temperature to °F. B’ = 1196.9. B and C in the Antoine-equation as defined in Eq. Antoine-equation in the form: log Pi0 = A′ − Find Thoughts The constants A.1. Solution Method a: Temperature conversion: Saturation pressure Pressure conversion Method b: o Pbenzene [bar] = 1.2 [-].161 [°C].87987 [-].696 10 B [psi] = exp(A − ) T (°C) + C 14.49 [°F] Find Thoughts Saturation pressure of benzene in bar at 80.1°C.1 Given B′ with Pi0 saturation pressure in T + C′ mmHg and T temperature in °C.01325[bar/atm] ⋅ 80.18) = 10 Pbenzene A ′− 9 + 32 ) 5 B′ 176.6 [-] C = 219. C’ = 362.18°F ( °C ⋅ o (176.696[psi / atm] A′ − B′ T (°F ) +C ′ with T (°F ) = T (°C) ⋅ 5 − 32 9 .760 [-] and C’ = 219.01325 bar 14. Compare both forms of the Antoine-equation side by side: 0 log Pbenzene = A′ − B′ B 0 (I) and ln Pbenzene (II). recalculate Antoine constants in the required units as shown in Exercise 2.696 atm = 1.

1°C = exp( A − Exercise 2. Antoine constants toluene (T) 9.3 .9) Find Thoughts The phase compositions at 100°C and total pressure of 1.5 atm The mole fraction in a binary mixture at a given temperature and total pressure can be calculated from the distribution coefficients of both components. 2.2 0.64 [-] C = 219. Eq.16 [°C] B 1 ) = 1.8 benzene liquid and vapor mole fractions 1 1 Check boiling point of benzene in T-x diagram in exercise 2. Eq. SOLUTIONS TO PROBLEMS 2-5 hence A = A′ ⋅ ln(10) + ln B= C= 5 ⋅ B′ ⋅ ln(10) 9 5 ⋅ (C′ + 32) 9 1. 110 Ptot = 1.97 (atm.01325 14..78. 2.1+ C Saturation pressure of benzene at 80.0 atm 80 70 0 0.01325 bar 80.18. 2755.696 A = 9. for a given value of Ptot and calculated saturation pressures. -54.4 0.9.3716.Fundamentals of Industrial Separations.2083 [-] B = 2755. 2. K. solve both Eqs. The distribution coefficient of a component follows from its saturation pressure and the total pressure. The saturation pressure at a certain temperature is given through the Antoine equation. 2.5 atm 100 90 Ptot = 1.0 3090. -53. see Eq.3 Given Antoine constants benzene (B) 9. temperature / C 120 .5.6 0.6 for x and y: o o ⋅ x and Ptot ⋅ (1− y ) = PT ⋅ (1− x ) Ptot ⋅ y = PB Solution 130 .2082.64.0 and 1. 1. Eq. Alternatively.

4 y = 0. calculating the saturation pressures as shown in the previous exercise.0 atm b. 2.776 = 1.776 = 1.5 KT (T ) = 0. mole fraction in liquid product xliq = 0.6) gives the total pressure: 0 0 (T ) + (1− x ) ⋅ Ptol (T ) Ptot = x ⋅ Pben Thoughts Solve this equation for T. 2.732 = 0.456 0 ⋅ (1− x ) Ptot ⋅ (1− y ) = Ptol x = 0.0 α= KB (T ) = 2. boiling point of benzene – toluene feed mixture at 1. Use the Antoine constants given in Exercise 2.35 a.732 atm Ptot = 1.0 KT (T ) = 0.732 1.456 1+ (α − 1) x Ptot = 1.18 with q = L/F = 1/(1+V/L).871 1+ (α − 1) x Second approach Ptot = 1.16) = 0.5 atm KB (T ) = x= 1. all other parameters.257 KB (T ) − KT (T ) y= αx = 0. such as temperature and yvap.2-6 First approach 0 (T ) = exp( AB − PB 0 (T ) = exp( AT − PT EVAPORATION & DISTILLATION BB ) T + CB BT ) T + CT 0 PB (100 + 273.257 Ptot = 1.425 KT (T ) 1− KT (T ) = 0.0 atm KB (T ) = x= 1. V xliq z L yvap .732 = 0. Summation of the partial pressures of benzene and toluene (Eq.488 1.0 atm 0 ⋅x Ptot ⋅ y = Pben and and and and 0 ⋅ (1− x ) Ptot ⋅ (1− y ) = Ptol x = 0.0 atm At a given Ptot and xliq.5 1− KT (T ) = 0.16) = 1. or via Eq.871 Given Find mole fraction benzene in feed z = 0.3. are fixed.40. yvap and z. The vapor – liquid ratio follows either from applying the lever rule (see diagram) to the values of xliq.776 1. vapor – liquid ratio in the flash drum at 1.776 atm 0 PT (100 + 273.736 Exercise 2.736 KB (T ) − KT (T ) y= αx = 0.5 atm 0 ⋅x Ptot ⋅ y = Pben y = 0.184 1.

while the equilibrium line still holds.toluene liquid and vapor composition at 60% evaporation liquid and vapor flow rates at a vapor composition of 60% compositions and flow rates for a two-stage flash cascade where 40% is flashed in the first stage and 30% of the remaining liquid in the second stage Thoughts a. 2.7b for α = 2. The operating line (Eq. Solution a.6. Note that mol A in gas total mol A − mol A in liquid x F F − qxF x F − qx = = = y≡ mol gas (1 − q )F 1− q mol gas the same idea as before. hence q = 0. d. d. y and x. see diagram on next page. Eq. V/F = 0. b.4 (Eq. isothermal flash a. 2. This defines a set of two equations with two unknowns.5.Fundamentals of Industrial Separations. Apply Eq. xF = 0.13). SOLUTIONS TO PROBLEMS 2-7 MathCad work sheet a.45( 2 ). here with y = 0.6 draw a process scheme and apply mass balances and equilibrium equations c. 2.7 relates equilibrium vapor composition y and liquid composition x for any α b. the y-x diagram for benzene . Exercise 2. 2.14) relates y and x between two subsequent stages for any q. c. (2) Note that either z or xF is used to represent the mole fraction of the more volatile component in the feed .5 Given Find F = 700 mol/s.

8 1 b.360 and y1 = 0. two equations determine the system: the operating line and the equilibrium line.3 + 0.2 0 0 0.4) · 0. x = 0.2 0.4) · (1 . Following the same procedure.375.538 c.7 mol/h.5 y 0.511 40% F 30% L 1=0.0.4.511. αx x −q ⋅x = see diagram) or solve the equation: ( y =) F for x with q 1− q 1+ (α − 1) ⋅ x = 0. L = q·F = 466.8 α = 2. including the over-all mass balances: Repeat the procedure in (b) (given the feed composition and fraction flashed) for the first stage.585 · 0.667.4) 0. x and y x − (1− q ) ⋅ y = .0.295 d.4/(1-0.585 V 2=0.g.42 F x2 = 0. With q1 = 0.4 = 0.6F x1 = 0.18F y2 = 0.295 and y2 = 0. via either equation.6 and z = 0. e.3) + 0.6 x 0.4 slope = -0.511 · (1 . or eliminate..6 follows q = 0.45 . Again.700).4F y1 = 0. solve the remaining equation for q: ( x =) F q α − y ⋅ (α − 1) With y = 0. The following scheme applies. In either case follows x = 0.4 0. The second stage has also a given feed composition x1 = 0.2-8 1 EVAPORATION & DISTILLATION 0.295 · (1 . it follows that x2 = 0.45 it follows x1 = 0.6 0. x and q. V = F – L = 233.585. Solve for the two unknowns.318 and y = 0.360 and a known fraction flashed (q2 = 0. This point can be found either graphically (draw in the x-y diagram the operating line with slope –q / (1-q) and read the required values. Check: xF = 0. The compositions are found at the intersection of the operating and equilibrium line.0.360 L 2=0.3 mol/h and. V 1=0.

6 Given F = FP/FH = ρP = ρH = ΔHvap = 100 mol/s 0.98 0. hence V” V " = F + L′ − B = F + R ⋅ D − B L” B D and B are calculated from the mass balance over the entire column (Eq.5) relates the partial pressures of both components in the vapor phase to the concentrations in the liquid phase. Combination of Raoult’s law (Eq. The feed temperature can now be calculated by the given equation for the pentane vapor pressure. 2. The pentane vapor pressure is given by: o PP =e ⎛ 310 ⎞ 11⋅ ⎜1− ⎟ ⎝ T (K) ⎠ (bar) The vapor pressure of hexane is 1/3 of the pentane vapor pressure.4 mole/s.05 1 bar 2. 2. Mass balances define the vapor stream from the reboiler.5 8170 mol/m3 7280 mol/m3 30 kJ/mol xD xB Ptot R H B = = = = = 0. f. 2.20): F = D + B and x F F = x D D + x B B . SOLUTIONS TO PROBLEMS 2-9 Exercise 2. L´ = R·D . c. the feed temperature the vapor stream from the reboiler the required energy in the reboiler the y-x diagram the operating lines and locate the feed line number of equilibrium stages height of column Thoughts Raoult’s law (Eq.19) and the component material for pentane (Eq. The last four problems can be solved graphically. by definition. The mass balances over the reboiler and the feed stage give V " = L" −B = q ⋅ F + L′ − B with q = 1 F=FL L’ while. . 2.2 mole/s and B = 68. b. Find a.5 K b. hence V” = 101. Note that q = 1.4) yields o o + (1− xF ) PH Ptot = xF PP with PHo = F FP 0.5 1 1 o PP and xF = P = = = F F + F + 1 0.25 0. respectively Solving these two equations for the unknowns D and B yields D = 31.5 3 3 P H hence o o Ptot = x F PP + (1− x F )PP / 3 ⇒ Ptot = o = PP 1 o 1 Po 5 o PP + (1− ) P ⇒ Ptot = PP or 3 3 3 9 ⎛ 310 ⎞ ⎟ T ⎠ 9 Ptot 5 11⋅ ⎜1− 9 Now the temperature is calculated from Ptot = e ⎝ 5 ⇒ T = 327. d.50 m The feed enters exactly on the feed tray at its boiling point. e.8 mole/s. 2.Fundamentals of Industrial Separations. g. Solution a.5) and Dalton’s law (Eq.

5): PPo PPo = =3 1 o PHo PP 3 The calculated values are plotted in the x-y diagram below: α PH = 1 0.6 0. the operating line for the stripping section is (Eq.8 1 e.26): y= L" B L" L " −V " L" ⋅ x P − ⋅ xB = ⋅ x P − ⋅ xB or y − xB = ( x − x B ) V" V" V" V" V" B B representing a straight line through y = xB and x = xB with slope V”/L”. 2.2 mole/s and V”/L” = 1.678. with constant relative volatility α. The total energy to vaporize a total mole flow V” required is: Qreb = ΔHvap ⋅V " = 3042 kJ / s d. Herein the slope L’/V’ can be calculated from Eq.1.8 0. the equilibrium curve is given by Eq. L” = V” + B = 170.22): y= L′ D L′ V′ − L ′ L ′ ⋅ x + ⋅ xD = ⋅ x + ⋅ x D or yP − xD = ( x − xD ) V′ V′ V′ V′ V′ which represents a straight line through y = xD and x = xD with slope L’/V’.2 0.4 xp 0. The operating line for the rectification section is written as (Eq. . 2. 2.2-10 EVAPORATION & DISTILLATION c.23: R 2. For an ideal binary mixture.25 L′ = = = 0.25 + 1 Similarly.4 0.7b: yp = αPH x P 1+ (αPH − 1) x P The relative volatility for this (assumed) ideal mixture equals to (Eq. 2.6 yp 0.2 0 0 0.692 V ′ R + 1 2.

see Chapter 4). Start from (xD. The feed line is fixed by two points: the intersection of the two operating lines and the intersection of the vertical through xp = 1/3 and the diagonal. 1 0. Continue carefully this staircase construction.5 equilibrium stages. The composition of the vapor from the 2nd tray is found on the operating line by drawing a vertical line between the first equilibrium point and the operating line.8 yP 0. gives 4.2 0 0 xB 0. on the equilibrium line by drawing a horizontal line. . Find the composition of the liquid leaving the upper tray. so q = 1.3 m . The feed enters the column exactly at bubbling point (no vapor). The number of equilibrium stages (minus the condenser) estimates the minimum column height = Hspacing ⋅ Nts − 1 = 5.Fundamentals of Industrial Separations.2 xF 0.8 equilibrium stages.6 xD xP 0.8 1 Operating and feed lines in y-x diagram for pentane/hexane. SOLUTIONS TO PROBLEMS 2-11 Both operating lines are plotted in the figure below.4 0. Read in the diagram above that 6.yD). ( ) The real height requires estimation of the number of real stages Ns = Nts / Eo (Eo = over-all efficiency. starting from the bottom composition. The resulting feed line is vertical and given by x = 1/3. including the reboiler and the feed tray. A similar construction in the stripping section. g. In total 11.7 equilibrium trays are required in the rectifying section. see page 2-17. which is in equilibrium with V’ leaving the column.6 0. the point on the operating line at the upper exit of the column.4 0. f.

i.23.7 EVAPORATION & DISTILLATION Given FM = 14. The stair case is constructed between the diagonal of the y-x diagram and the equilibrium curve. From the next diagram one reads (L’/V’)min = 0.0321 y 0.2 0. Any operating line goes through (xD.918 0.435. The reflux R is related to the slope of the slope of the operating line (L’/V’) through Eq. the line with the R= 1− L′ / V′ smallest slope goes also through the intersection of the feed line with the equilibrium line.8 xmethanol xD 1 Minimum number of stages at maximum reflux.349 0.e.8 0. the feed stage location and number of theoretical stages for a reflux ratio R = 1. The minimum number of stages is obtained at maximum reflux.77.4 0.82 (however. Rmin = 0. The minimum number of stages is obtained at maximum reflux. 2.4 Note that in this case the reboiler does not contribute to the separation because the liquid entering the reboiler is entirely vaporized: its composition equals that of the vapor leaving the reboiler (total reboiler). xD). 0 . the minimum number of stages and minimum reflux.4 0.075 0.46 kg/h FW = 10.0523 0.918 0. D = 0 and B = 0.0.6b and draw the operating line for the stripping section.12 P = 1 bar 0.2 xB 0 0.23: L′ / V′ .98 xB = 0. The Underwood expression (Eq. 1 ymethanol 0. the minimum number of stages amounts to 5.6 0.47 ) would give Nmin = 5. the Fenske expression (Eq.6 0. b. Hence. As shown in the first diagram below.813 0. slopes of operating lines amount to unity.8. Hence the slope of both operating lines equals unity.2-12 Exercise 2. Thoughts Solution a. q should equal unity for Eq.58 (Eq.e. Calculate V” and L” as explained in Exercise 2. With αav = 3.703 0. Draw the operating line for the rectifying section for R = 1. 2.0 according to Eq. 2.225 0.05 B q = 1. 2.2490 0.1900 0. The minimum reflux is obtained at infinite number of stages.38.953 0. 2.54 to be applicable).516 Find a.154 0.48).352 xD = 0. 2. i.54) would give Rmin = 0.593 0. 2. according to Eq. both operating lines intersect the feed line on the equilibrium line.44 kg/h x 0.

xD 0. the staircase lies between the equilibrium and the lower operating line.8 q-line 0. 0. B B .23: R = 0.8 xmethanol 1 Minimum reflux at minimum slope of operating line. The equilibrium stage closest to the intersection of the feed line and the equilibrium line constitutes the optimal feed stage.6 0.8 0 . From that point.4 0. Draw the operating line through both points.6 x 0.724).5 L′ / V′ = R+ 1 The operating line in the stripping section goes through (xB.2 0. including reboiler 1 with reflux ratio R=1.xD) between the equilibrium line and the upper operating line downwards.6 operating line with minimum slope 0.8 methanol xD Number of stages. xB) and the intersection of the upper operating line and the feed line. 0. 2. (0.469.2 xF 0 1 ymethanol 0.6 feed tray 0.6 stages 0.4 0. see diagram.435 0.4 N=15.4 xF 0. SOLUTIONS TO PROBLEMS 2-13 1 ymethanol 0.2 0.2 0 0 xB 0. Start the staircase construction at (xD. The slope of the operating line in the rectifying sections follows from Eq.Fundamentals of Industrial Separations. b.

2-14 EVAPORATION & DISTILLATION Alternatively.e. 2. Hence the slope of both operating lines equals unity. the compositions of all equilibrium stages in the rectifying section can be calculated from that operating line and the equilibrium line (Eq. 2. Applying the Underwood expression.96 0. e. the number of equilibrium stages required at a reflux ratio 1.72 0. both operating lines intersect the feed line on the equilibrium line. which depends on the composition of that stream. 2. i.50 0.7 is given). The compositions are given in mole fractions. 2. After that point. Exercise 2.54) or find graphically. y3. d. Apply the Underwood expression (Eq. Note that in case of total reflux.e. Thoughts Solution a.8 Given F = 907. C6H5CH3 = 400 kJ/kg 0. Determine the composition of the liquid leaving tray 2. 2. the operating line in the stripping section. the top and bottom product in kg/h. or solve in the x-y-diagram. In either procedure.60 0.22) L ′ yn+1 = xD + ⋅ [xn ( y n ) − xD ] V′ Starting at the top with y1 = xD. c.20 0.90 0. C6H6 = 380 kJ/kg ΔHvap. Repeat this procedure until the equilibrium composition passes the intersection of the feed and the equilibrium line.98 Find a. see note in part a.5 times the minimum.37 0.79 0.51 xD = 0.05 z = xF = 0.50 B ΔHvap.21 0. The minimum number of stages is obtained at maximum reflux.3 kg/h P = 1 bar q = 1. repeat the same procedure using Eq.70 0. 2. D = 0 and B = 0. Apply the Fenske equation. 2.86 0. so to calculate the product streams in kg/time the appropriate mole balances have to be converted to mass balances. the minimum number of stages does not include the reboiler because all liquid is evaporated entirely (total reboiler).40 0. the minimum number of equilibrium stages.0 x y 0.54 (q = 1) . from Eq. the number of equilibrium stages found includes the reboiler.48. calculate x1 = x1(y1).22. Eq. the minimum reflux ratio.10 0.64 0. This numerical procedure gives accurate results then a drawing.30 0. i. in equilibrium with y2 and calculate the composition of the vapor coming from tray 3. the energy demand in the reboiler in kg steam/h The minimum reflux is obtained at infinite number of stages.29. b. the composition of the liquid from tray 1 in equilibrium with the vapor leaving that tray (or read x1 from the equilibrium line in the x-y-diagram if no equilibrium function such as that in Eq.95 xB = 0. H2O = 2000 kJ/kg ΔHvap. Eq. The conversion factor of a particular stream is its molecular weight.80 0.

7 may be applied.6 xbenzene 0. .8. an alternative method would be to calculate each subsequent equilibrium y-value yn+1 from the operating line. x D − xF 1− x B x ln[ D ⋅ ] 1− xD x B = 6. 2.079 .7b. xD) and the intersection of the vertical feed line (q = 1) and the equilibrium line: αa v ⋅ xF y= = 0. in excellent agreement with the Underwood approach.48: Nmin = lnαav Like in Exercise 2.519 .38 Rmin = 0.2 0. see diagram below.8 xD xD 1 0 Hence.21.6 q-line 0. Eq. in αa v − (α av − 1) ⋅ y n good agreement with the result from the Fenske expression. SOLUTIONS TO PROBLEMS 2-15 xD 1− xD − αav x 1− x F Rmin = F α av − 1 with an average value of the relative volatility according to Eq.080. 1− 0. Applying the Fenske expression. calculated from the reciprocal yn of the equilibrium expression: xn = from which Nmin ≈ 6.8 operating line with minimum slope 0. with L’/V’ = 1: yn+1 = xn with xn.4 0. 1+ (αa v − 1 ) ⋅ xF 1 ybenzene 0.519 xD − 0.4 0.48: αav = α B ⋅α D ≈ y 1 1− x 1 y 9 1− x 9 ⋅ ⋅ ⋅ = 2. for this rather ideal system. 2. the equilibrium on the previous stage n.2 xF 0 0. 1− y 1 x 1 1− y 9 x 9 Alternatively.519 = 1.716 = 0. Eq.53 gives Rmin = 1. 2. 2.Fundamentals of Industrial Separations. 2. draw the equilibrium line in a x-y-diagram. αa v ⋅ x yeq (x ) = 1+ (αa v − 1) ⋅ x The operating line in the rectifying section goes through (xD. x = xF.4 b. Eq. the minimum slope of the operating line equals Follows with Eq.716 .

4 0.672.4 0.2 0.382 xF − xB V" d. The following overall mole balances apply (Eqs.19 and 2. xB) and (xF. B B B B Similarly to the outline given in exercise 2.6 0. x = xF.20) F=B+D XF·F = xB·B + xD·D B .618 L′ / V′ = 1. Draw the operating line through (xB. xB) and the intersection of the upper operating line and the feed line.5 ⋅ Rmin + 1 The operating line in the stripping section goes through (xB. 2. xD) between the equilibrium line and the upper operating line downwards. apply the stripping operating line.23: 1.2-16 1 ybenzene 0.2 0 0 xB 0.8 xbenzene xD 1 c.7: L ′ yn ⋅[ − xD ] V′ α av − (α av − 1) ⋅ y n The slope of the operating line in the stripping section is calculated as yn+1 = xD + L" 0. see x-y-diagram. 2.672 − xB = = 1. Substitution of x = xF into the upper operating line gives y = 0. Start the staircase construction at (xD. Beyond the feed stage. the y-compositions of all equilibrium stages in the rectifying section can be calculated by elimination of yn xn from the operating line using = x n .672).8 feed stage EVAPORATION & DISTILLATION 0.7b. 0.5 ⋅ Rmin = 0. the reciprocal form of αav − (αav − 1) ⋅ yn Eq. The slope of the operating line in the rectifying sections follows from Eq.6 0. 2.

2.0 kg/h Φ B = Φ F − Φ D = 487. The conversion is reads Φ F = M F ⋅ F = [x F ⋅ M ben + (1− x F ) ⋅ M tol ] ⋅ F = 907. B and D in mol/h.H 2O . the feed ΦF is given in kg/h.20 gives B = D = 5337 mol/h and Φ D = M dis ⋅ D = [x D ⋅ M be n + (1− x D ) ⋅ M tol ] ⋅ D = 420.0 kg/h e.7 kg/h ΔHvap. However.19 and 2.3 kg/h With xF = 0.3 kg/h Φ D = Φ F −Φ B = 420.6b).ben + (1− x B ) ⋅V " ⋅M tol ⋅ ΔHvap. The amount to be evaporated equals V” = 13981 mol/h (following the procedure explained in exercise 2.5 it follows that F = 10675 mol/h. Solving Eqs. The steam consumption required at the given reflux: x ⋅V " ⋅M ben ⋅ ΔHvap.Fundamentals of Industrial Separations.tol Φ steam = B = 254. The heat required to evaporate liquid bottom product is delivered through condensation of steam. SOLUTIONS TO PROBLEMS 2-17 With all x mole fractions and F.3 kg/h or Φ B = M bo t ⋅ B = [x B ⋅ M ben + (1− xB ) ⋅ M tol ] ⋅ B = 487.

2-18 EVAPORATION & DISTILLATION .

4 A vent gas stream in your chemical plant contains 15 wt% of a pollutant. The absorption equilibrium at 25°C is given by the relation yNH3 = 1.1 mole% ammonia in water. 1. The local authorities want to reduce the pollutant concentration to less than 1 wt%. Operation is at 10 bar.1 bar 100% water.5 times the minimum liquid flow rate. Exercise 3. the rest is air. The Henry coefficient of CO2 in water at 5°C is 875 bar.01325 bar. 2% ethyl alcohol. 98% CO2. 25°C) of air are fed to the tower per m3 of waste water. Because of cooling coils the operation can be assumed to be isothermal. Assume that air is not soluble in water and that water is nonvolatile. ρwater = 1000 kg m-3. At 30°C your laboratory has found that at low concentrations the equilibrium data can be approximated by y = 0. If the liquid flow rate is 1.1 Chapter 3: ABSORPTION & STRIPPING Exercise 3. 1.414 xNH3.5·x (where y and x are weight fractions of the pollutant in vapor and liquid).314 J mol-1K-1. Calculate the concentration of ammonia in the exit water if the inlet liquid concentration is 0. You have decided to build an absorption tower using water as the absorbent. Exercise 3. how many equilibrium stages are required to absorb 92% of the CO2. 1 atm = 1.1 bar 95% The vapor pressure of ethanol amounts 0. isobaric conditions in the tower and neglecting mass transfer of all components except ethanol.2 When molasses is fermented to produce a liquor containing ethanol.3 A gas stream consists of 90 mole% N2 and 10 mole% CO2. The inlet water is pure and at 30°C. and its liquid phase activity coefficient at infinite dilution in water can be taken as 7. Exercise 3. the inlet air is free of ammonia and 2000 standard cubic meter (1 atm. We wish to absorb the CO2 into water. Mwater = 0. a CO2-rich vapor containing a small amount of ethanol is evolved. R = 8. a) b) Find the minimum ratio of water to air (L’/G’)min on a solute-free basis With an L’/G’ = 1. For the following conditions.22 (L’/G’)min find the total number of equilibrium stages and the outlet liquid concentration . Entering gas: Entering absorbing liquid: Required ethanol recovery: 180 kmol/h. determine the number of equilibrium stages required for countercurrent flow of liquid and gas. The inlet water is pure and is at 5°C. 30°C.5. The alcohol can be recovered by absorption with water in a sieve tray tower.1 A plate tower providing six equilibrium stages is employed for stripping ammonia from a wastewater stream by means of countercurrent air at atmospheric pressure and 25°C. 30°C. assuming isothermal.10 bar at 30°C. Choose a basis of 1 mole/hr of entering gas.Fundamentals of Industrial Separations. The operation is essentially isothermal.018 kg mol-1. SOLUTIONS TO PROBLEMS 3.

e. What happens for L/G = 0. Construct the equilibrium and operating lines for desorption with yN+1 = 0 and L/G = (L/G)max/1.5 A gas treatment plant often has both absorption and stripping columns as shown in the figure. Calculate the vapor-liquid equilibrium coefficient and draw the equilibrium line.01.0002 and L/G = 0.3. . d. xN and x0 are to be taken from the absorber operating at L/G = 0.001 x out Wet DEG Schematic of natural gas absorptive drying operation a. f. Determine the number of theoretical stages required to reduce the water mole fraction from yN+1 = 0. A very common type of gas treatment plant is used for the drying of natural gas by physical absorption of water in a hygroscopic solvent such as diethylene glycol (DEG). Calculate analytically the number of theoretical stages in both sections.01.02. Desorption takes place at 120°C and 1 bar. At a temperature of 70°C and a pressure of 40 bar the saturated vapor pressure of water is equal to 0. c. The heat exchanger heats the saturated solvent. How many stages are required for L/G = 0.004. Determine the minimal L/G-ratio to obtain the desired separation. Determine the number of theoretical stages in the stripping section graphically. In this case dry nitrogen is used as the stripping gas.02 Dry DEG 70 C 40 bar Wet CH4 A B S O R P T I O N S T R I P P I N G 120 C 1 bar Dry N2 y in=0.005.2 bar. y1=0. changing the equilibrium characteristics of the system so that the solvent can be stripped.0002 Wet N2 x in=0. In this operation the solvent is continually recycled.001 to y1 = 0. Construct the operating line for x0=0. Comment on the chosen value of the liquid mole fraction at the outlet of the absorber. The saturated vapor pressure of water is equal to 2 bars.2 ABSORPTION/STRIPPING Exercise 3. It is known that water and DEG form a nearly ideal solution. Dry CH4 y out=0. b.5.0002.

2 and 3. K. 4.018 kg mol-1. for xout.414 The stripping factor: S = = = 2. The flow rates have to be converted to molar units. R = 8.3 are Solution Calculation of the distribution coefficient: KA = γ A ⋅ pA = 7.1 bar Absorbent: pure water (xin = 0) T Pvap.02 − 0. 1 atm = 1. solve the Kremser Eq. (L/G)min .1 = 0.16 K Ptot = 1 atm Nts = 6 theoretical stages G/L = 2000 standard cubic meter air per cubic meter waste water Mwater = 0.314 ⋅ 298.max − x in 0. Eqs.EtOH in water Find The required number of stages to recover 95% of the ethanol.680 G 81750 KG 1.02 / 0. mole fractions can be used.01325 bar.414 xammonia. xin and yin = 0.33) is applicable.02 ⋅ (1− 0. SOLUTIONS TO PROBLEMS 3.44·10-6 Nts +1 From Eqn. 3. Thoughts Mole fractions can be used because the concentrations are sufficiently small. 3. used to calculate the distribution coefficient KA.5 ·(L/G)min. This will be discussed in the next chapter.2 Given gas flow rate = 180 kmol/hr.01325 ⋅ 105 ⋅ 2000 = 81750mol / unit time 8. Exercise 3. with known Nts.1 Given Waste water with ammonia. This equation links the number of theoretical stages and the aqueous concentrations at inlet and exit (yin = 0). with Eq. clean air as strip gas K = 1. Note that the actual number of stages is larger than the number of theoretical stages because an actual plate does not operate at 100% efficiency.EtOH = 30°C = 0. The equilibrium line is a straight Solution 1 m3 water / unit time equals ρwater/Mwater = 55556 mol / unit time 2000 m3 NTP / unit time equals P ⋅V / R ⋅T = The L/G-ratio in mole units: 1. S.1 bar = 7. The required number of stages is then found from a McCabe Thiele diagram or from the Kremser equation. (yout = 10 ) G min x out.9.5 γ ∞.680 L = 0. Eq. is equally applicable and more convenient in this case.648 .feed = 0. so a reasonable value has to be assumed: take L/G = 1. 3.682 − 0 .16 L 55556 = = 0.7: -3 L y in − y out 0.682 ptot 1. see Eq. Thoughts Because the concentrations are low. The liquid-to-gas-ratio is not given in this exercise.34.5 ⋅ 0.34: xin − xout = S Nts +1 −S Alternatively.Fundamentals of Industrial Separations. 3.33.99356 y in S − 1 xin − K yin = 0 Æ xout = xin · (1 – 0. 3.95) = = = 0. The volume change due to absorption is neglected.081 0.314 J mol-1K-1.3 SOLUTIONS Exercise 3.1 0 Calculation of the minimum slope of the operating line. giving the fraction stripped. However.99356) = 6. 98% CO2. Find The ammonia concentration in the exit water line and the Kremser equation (Eqn. 3. 2% C2H5OH P = 1. ρwater = 1000 kg m-3.001 T = 298.

005 xout xout.682.972 and the equilibrium line with slope K = 0.025 0.in = 90 mol% CO2.28 gives: G ⋅ K 0.03 Exercise 3.3 and 3.015 0. Start the step case construction at (0. number of equilibrium stages for a CO2 recovery of 92% is calculated from the Henry coefficient according to Eqs. 3. 3. conversion to mole ratios extends the applicability: Y = KA·X still holds at higher concentrations.4 ABSORPTION/STRIPPING hence L = 1.02 x 0.3.425 Eq. The number of stages can be determined graphically from a McCabe Thiele diagram or by applying a Kremser equation (Eq.001). While the linear expression y = KA·x (Eq.025 operating line 0.max = yin /K yout 0 0 0.28).01 equilibrium line 0.36 theoretical stages ln A For a graphical McGabe-Thiele solution. Thoughts Mole ratios have to be used because of the rather large concentrations.3 Given N2.01 0. KA. The number of equilibrium stages. Both expressions have the same initial slope.4.015 Å0.972 .3 0. draw the operating line through (xin. 3.3) applies to low concentrations only.max = Yin/KA = Yin/KCO2. The distribution coefficient KA . 3. see YX diagram on next page. counted on the equilibrium line. The minimum absorbent flow rate can be found either graphically or from a mass balance assuming equilibrium between the exiting absorbent and the entering gas.5°C = 875 bar L/G = 1.e. With A = L 0. is appr. Xout. 0.in = 10 mol% Isothermal operation Absorbent = pure water Ptot = 10 bar T = 5°C HCO2. 0.972 = = 1.5 ⋅ L G G min = 0.005 0.3. i.5 (L/G)min Find Nts.yout) with slope 0. 5.02 yin y 0.682 ln( Nts = 1 y 1 + (1− ) ⋅ in ) A y out A = 5.

1 Yin = 0. After conversion to mole ratios it follows: ⎛L⎞ Yin − Yout 0.111 = 8. 3.4. Yout) = (0.5 = 120.4 gives the distribution coefficient KCO2 = H CO2 / Ptot = 875/10 = 87.5 = 1. 3.4 0.5 0.5 The actual absorbent flow rate: L/G = 1. Y CO2 = 87.5.2.9·10-3 xin = Xin = 0 Dividing Eq.7.28 can be applied with A = 120.6 x 0.Fundamentals of Industrial Separations.001 0.1 Å0.4 x.max − X in −0 87.8 y. resulting in Nts ≈ 4. Check in the graph below that Nts ≈ 4. hence.8 1− x Solution yN+1 =yin = 0. 0.5 · 80. see also Fig.8 / 87.6.8 In the McCabe-Thiele diagram below one can count the number of equilibrium stages on the equilibrium line.5·XCO2. All operating lines intersect at (Xin. Minimum absorbent flow rate from mass balance Eq. X= KA 0. 3.9·10-3).2 0.111 ⎝ G ⎠min X out. 3.38.6 0.111− 8.15 Y Xout Xoutmax Yin 0.4 0.5 ⎜ ⎟ 0.92)·0. 8. Eq.0015 X . 3. Y= y 1− y 0.9 ⋅ 10−3 = = = 80.05 Yout 0 0 5 10 4 0.111 Yout = (1-0. Alternatively.3 by Eq. SOLUTIONS TO PROBLEMS 3.2 0 0 0.

22 · (L’/G’)min basis. Eq.6. 3.4 Given ypollutant = 15 wt% in gas stream T = 30°C. 3.15: Nts = 8.01 = 0.471 = 0.5.26: X out = 0.575/0. see Fig.3.28) gives with A = 0.4 The Kremser equation (Eq. The slope of the corresponding operating line is calculated from: ⎛ L′ ⎞ Yin − Yout 0. 3.5·x (30°C.176 ⎝ G′ ⎠min X out. low concentration) The minimum water-to-air-ratio (L’/G’)min and the number of stages and outlet liquid concentration at L’/G’ = 1.1 0.22 · 0. weight fractions. Yout = yout = 0.575 Y − K ⋅ X out Note: Some textbooks use AN = in which is essentially Eq.25 for xin = 0. see previous exercise.6 ABSORPTION/STRIPPING Exercise 3.15 0.2 Yin 0.01 The highest value of xout is obtained at the lowest possible liquid flow rate.2. Find Thoughts Weight ratios have to be used because of the high concentrations to allow working on a solute-free Solution Yin = y in = 0.1 0.5·X All operating lines through the point: Xin = xin = 0.05 Xout Xoutmax Yout 0 0 0.max − X in −0 0.176 . The minimum L’/G’ ratio can be found from the mass balance assuming equilibrium between the entering gas and the exiting liquid because that gives the highest possible value for xout.2 0. This conversion extends the linear equilibrium line with K = 0. Yout ≈ yout 1− y in Equilibrium line: Y = 0. 0.471 ⎜ ⎟ 0.575 and the expression for the operating line becomes Y = 0. Yout .5 The L’/G’ ratio to be applied is L’/G’ = 1.01 = = = 0.224. Xout follows from the overall balance.176 − 0.289 or xout = 0.3 0.5 = 1. 3.575·X + Yout The McCabe Thiele diagram looks as follows 0. isothermal operation Desired exit concentration: ypollutant = 1 wt% Absorbent: pure water Equilibrium: y = 0.176 − 0.

abs = (b) Operating line through (xin.001 Desorption: T = 120 °C Psat. the minimum L/G both from the McCabeThiele diagram and from a mass balance (d) the number of theoretical stages for desorption at L/G =(L/G)max/1.001 to 0. The line is shown in the figure below.01 (c) idem for L/G = 0.Fundamentals of Industrial Separations.5 Find P = 40 bar x0 = xin = 0.0002: Nts = 2.1 and 3. 0 Pw 0. All operating lines intersect at (xin. an infinite number of stages is required. (f) the concentration in liquid phase at inlet of stripper Kw can be calculated from Eqs. 0.01·x. The K-value for stripping can be calculated from Eq. the more difficult the separation will be.yout) = (0. The operating line will now be located below the equilibrium.001 xin xout yin Å0.3: Kw = Kw.25.5 (e) the number of theoretical stages in both absorption and desorption using the Kremser-equations.2 . 40 P Thoughts (a) (b) (c) (d) (e) (f) Solution (a) From Eqs.28 (absorption) and in Eq. 0.1 and 3.1 0.7 Exercise 3. The Kremser equation is given in Eq.33 (desorption/stripping). 3.25 5·10 4 operating line equilibrium line yout 0 0 0.3. Investigate the limiting values at absorber inlet and stripper outlet.02 y1 = yout = 0.15 x 0.005 and L/G = 0. Idem. 3.0002) and have as slope (L/G). It can be expected that the results of the Kremser equations with mole fractions agree quite well with the graphical results.2 bar yN+1 = yin = 0. because the direction of mass transfer is reversed. 3.02.004. the lower (L/G). At the minimum value of (L/G).0002) with slope L/G = 0. 0.1. Conversion of mole fractions to mole ratios is not necessary. Reduction of the water mole fraction in the gas from 0.0002 P = 1 bar yN+1 = yin = 0 (a) the distribution coefficient and the equilibrium curve (b) the operating line and number of theoretical stages for L/G = 0.5 Given Absorption: T = 70 °C 0 Pw = 0. H2O = 2 bar L/G =(L/G)max/1.0015 y 0.3. 3.01 In this case the intercept y1 – x0·L/G = 0 Æ y = 0.02.yout) = (0. The concentrations are sufficiently small to assume the equilibrium curve to be a straight line.05 0. SOLUTIONS TO PROBLEMS 3.2 = = 5 ⋅ 10−3 .

15 0.1 0.1 x 0.2 0 0.max = Kw·xin yout Å0. meaning equilibrium between entering gas and exiting ‘wet’ DEG: L y in − y out y N+1 − y1 0.1 xout xin 0.1.3. the operating line and the equilibrium line are parallel and N = 8. After desorption.5 = w in = = 2.1− 0 L 2.2 0.8 .0015 ABSORPTION/STRIPPING y 0.001 yin 5·10 4 5·10 4 yout xin 0 0. 0.3 x 0.667 ⎜ ⎟ x in − x out 0. 0.4 (c) For L/G = 0.2 − 0.str = 0 Pw 2 = =2 1 P The water concentration in the exiting DEG stream can be found from the operating line: xN =0.001.004. the water concentration has to be reduced to x = 0. The minimum L/G-ratio can be found by drawing an operating line which intersects the equilibrium line at the specified concentrations (0.44 ⋅ 10−3 G min x out.8 0.0015 0.5 ⇒ = = 1.05 0.02 G 1.005.2 stripper yout.05 0.02.02 (d) Kw = Kw.001 y in y xin xout operating line 0.1 0.1− 0.max − x in y N+1 / Kw − x 0 0. the separation cannot be achieved: the operating line and equilibrium line intersect at a y-value lower than 0.001− 0. dry nitrogen is used: y = 0.02.0002 = = = = 4.25 y 0.15 . The maximum L/G ratio follows from the mass balance: ⎛L⎞ K x − y in 2 ⋅ 0.5 ⎝ G ⎠max 0. For L/G = 0.001). As strip gas.15 xout equilibrium line yout 0 0 x 0.05 operating line 0 0 0.

Any value in between would work and would fix L/G in both columns. Kremser equation for stripping. Follows Nts = 2. ysin = 0. Eq. 3.32.02. 3. with A = 0. and xsout = 0. xin = 0. (f) At a given L/G ratio xout at the absorber outlet follows from the overall mass balance (Eq.Fundamentals of Industrial Separations.667 = 1.80.6 and L/G = 0.2. The highest possible liquid concentration at the outlet of the absorber amounts to yin / Kw. 3. .abs = 0.10 L The upper and lower limits of L/G are determined by the maximum concentration leaving the absorber and the minimum concentration at the inlet. Eq.01 / 5·10-3 = 2.9 (e) Kremser equation for absorption. The lowest possible liquid concentration at the inlet of the absorber equals the lowest outlet concentration of the stripped liquid and amounts to zero.33. with S = 2 / 1.20. Follows Nts = 2.01) G x out = ( y in − y out ) + x in = 0.02.1.001. SOLUTIONS TO PROBLEMS 3. and yout = 2·10-4. xsin = 0.28. yin = 0.

10 ABSORPTION/STRIPPING .3.

25.106 kg mol-1. Mwater = 0.31 J mol-1 K-1. the plate efficiency c.015 m3s-1.Fundamentals of Industrial Separations. a. Lab scale experiments showed that the overall mass transfer coefficient kOV = 3·10-3 m s-1 at this gas load.6.029 kg mol-1. is proportional to 1/R – 1/r. Show by calculation that this column can produce the required reduction at the given flow rates.4 An aqueous waste stream of 0. To this purpose an existing tray column with 5 trays is available. Preliminary calculations (see exercise 3. where r is the distance to the centre of the droplet. Calculate: a.3. d. Calculate the mole fraction of benzene in the effluent.81 m s-2.018 kg mol-1.9%? Calculate the plate efficiency EMV. The column should have the capacity to treat QV = 3 m3 gas per unit time at this condition (40 bar. 70°C). saturated with benzene. Laboratory experiments at 1 bar and 294K show that the overall mass transfer coefficient based on the gas phase. f.5 m. e. . 1 How many theoretical stages are required to reduce the benzene content by 99.9%. SOLUTIONS TO PROBLEMS 4. starting from the stationary state balance given in Eq.0·10-3 at this temperature. At this temperature the distribution coefficient Kbenzene = 152 and the saturation pressure of benzene is 0. Comment on the chosen value of the airflow.8 ms-2. This is possible by stripping with (pure) air. should be purified by reducing the benzene content by at least 99.10 to 0.104 bar.010 and Nts = 2.77 m2.01325 bar. At this airflow the interfacial surface area is 50 m2 per m2 tray area. Hspacing = 0. ρwater = 1000 kg m-3.2 Derive the rate expression in Eq. The gas phase is assumed to obey the ideal gas law. c.932 m3STPs-1. g = 9. 4.1 Chapter 4: GENERAL DESIGN OF G/L CONTACTORS Exercise 4. Exercise 4. g = 9.1 An aqueous droplet with radius R is surrounded by a stagnant. Exercise 4. b.0080 m s-1.0 mol% H2O. the height of the column Exercise 4. The effective surface area of a single tray amounts to 1. the difference in ammonia concentration in the vapor phase and at the LVShow that y − y r r =R interface. The equilibrium constant K = 5.016 kg mol-1) from 0. R = 8. Assume that the resistance against mass transfer from the vapor to the liquid is mainly situated in the vapor phase. 4.3 A tray column is to be designed to reduce the water content in natural gas (Mmethane = 0. the minimum column diameter b. Mair = 0. inert vapor phase containing a low concentration of ammonia. ρDEG = 1100 kg m-3) containing 2.078 kg mol-1. kOV = 0. Mbenzene = 0. 1 atm = 1. The stripping process is carried isothermically out at the same conditions with an airflow 1 of 0. How should the exiting gas flow be treated to avoid dumping of benzene? 1 m3STP means 1 m3 at standard temperature (0°C) and standard pressure (1atm) .5) resulted in a slope of the operating line L/V = 0.02 mole% by absorption of water at 70°C and 40 bar in diethylene glycol (MDEG = 0.

90 and a surface area per unit bed volume a = 200 m2 m-3. pressure and liquid flow rate remain unchanged . The height of the packing is 2. the internal diameter of the column 0. Calculate the flooding velocity for two different packing materials: a. Lmin? How many transfer units NOV characterize this absorption process at the given process conditions? Calculate the overall mass transfer coefficient based on the gas phase. ρwater = 1000 kg m-3. Air containing 2. b.2 GENERAL DESIGN OF G/L CONTACTORS Exercise 4.5 kg water s-1. containing 5 mol% NH3 at a total flow rate of 5 mol s-1. Mair = 0.029 kg mol-1.81 m s-2. Mlucht = 0. Exercise 4. 25 mm metal Hiflow rings with a packing factor of 125 m-1. clean water is fed to the top of the column. At a liquid flow rate L = 65 mol s-1 the SO2-content in the effluent is reduced to 0.018 kg mol-1.017 kg mol-1.6 To study the rate of absorption of SO2 in water. Mammonia = 0. Mwater = 0. the density of water may be taken as 1000 kg m3. d.0 m. The diameter of the rings is 15 mm. Temperature.018 kg mol-1. e. is scrubbed in a packed column by a countercurrent flow of 0. How much larger is the chosen value of L compared to the theoretical minimum value. a laboratory scale column packed with plastic Hiflow rings is used. a. The absorption of SO2 in water is studied in counter-current operation at 1 bar and 285 K. 25 mm ceramic Raschig rings with a packing factor of 540 m-1.31 J mol-1 K-1. Mwater = 0.4. At what (superficial) velocity of the gas feed flooding will start? Calculate the concentration of SO2 in the gaseous effluent in case the air feed is increased to 75% of the flooding velocity. kOV.50 mol%.029 kg mol-1. g = 9. The bed has a porosity εbed = 0.0 mol% SO2 is fed to the column at a rate of V = 2.25 mol s-1.5 An air-ammonia mixture. At 20°C and 1 bar 90% of the ammonia is absorbed. c. R = 8. and b. At this temperature the distribution coefficient KSO2 = 32.33m.

* Thoughts Try to eliminate the composition at the interface. yNH3·ΦNH3.3. 4.bulk − y R ].1 Given Find A water droplet with radius R absorbing ammonia from a stagnant gas phase. Note that ΦNH3 < 0 meaning transport in the direction of decreasing r (towards the L/V-interface).6 from Eq. 4. in mol/s. Eq. this equation transforms into Φ NH3 = − DNH3 ⋅air ⋅ 4πr 2 ⋅ ρV ⋅ d y NH3 dr = constant. Note that y Ai = y Ai Solution Extract the differences in compositions from the two balance equations. replacing x by the equilibrium relation y*/K. * = y A − y Ai * * y Ai − yA = kV ALV ρV KΦ A kL ALV ρL ΦA + Φ A ⎡ 1 1 KρV ⎤ * yA − yA = ⎢ + ⎥ ALV ρL ⎣ kV kL ρL ⎦ and.3. Hence the rate of absorption is given by r yR Φ NH3 = −4πR ⋅ DNH3 ⋅air ⋅ ρV [y NH3 .Fundamentals of Industrial Separations. is small compared to the first term and. as long as yNH3 is sufficiently small. Thoughts The concentration of ammonia is small. This rate is given by Eq.3 SOLUTIONS Exercise 4. replacing z by r and with Ar = 4πr2.2 Derive Eq. ALV ρL * * (yA − yA ) = kOV ALV ρL ( y A − y A ) ⎡ 1 ⎤ 1 KρV + ⋅ ⎢ ⎥ ⎣ kV kL ρL ⎦ ΦA = with 1 1 1 KρV = + ⋅ kOV kV kL ρL . SOLUTIONS TO PROBLEMS 4.1a. d r −1 4 π ⋅ ρV ⋅ DNH3 ⋅air Integration from yNH3 = yR (= yAi) at the L/V interface (r = R) to yr at distance r from the centre of the droplet results in yr ⎡ 1 1⎤ Φ NH3 ⋅⎢ − ⎥ yr − y R = − 4π ⋅ ρV ⋅ DNH3 ⋅air ⎣ R r ⎦ R ybulk Separation of the variables gives d y NH3 = Φ NH3 As r → ∞. 4. with Φair = 0 and yNH3 being very small. after rearrangement. yNH3 → ybulk. quite a while. 4. thus the droplet may absorb ammonia at a constant rate for Solution The second term in the RHS of Eq. The concentration of ammonia as a function of the distance r from the droplet centre. Exercise 4. 4.1a.

5. xwater.016 kg mol-1 = 3·10-3 m s-1 = 9.186 = 12. Hspacing ⋅ ρDEG ρ y ⋅ M CH4 =0. Hence. .5 m2. 4.9 (Nts = 2. the minimum column diameter b. the plate efficiency and the overall efficiency c.010 Keq = 5.81 m s-2 Find Thoughts Because the concentrations are very small.25/0.25 Hspacing = 0. the interface area ALV in Eq. c) The overall efficiency EO is given by Eq.0002 T = 343 K Ptot = 40·105 Pa MDEG = 0.03 N m-1 and φ = 0.4. L = 42. EO = 0. 4.27) π ⋅ 0.1 = 6.713 m s-1.9) Hcolumn = Hspacing·Ns = 0. taking γ = 0.148 (Eq. a. The flooding velocity is the key parameter. 0.06·10-3 m3 s-1. 4.0·10-3 Nts = 2.25) and the column height with Eq.5 m a.3 Given Drying of natural gas by absorption of water in DEG xwater. 4. c.1) uflood = 0.6e for a discussion) 2) Nth = 2. On the other hand. ρ y ⋅ M CH4 In Fig.0 m (Eq.8.0095. 4.12 and 4. Eqs.8).4e and 4.046. 4. 4.106 kg mol-1 ρDEG=ρL = 1100 kg m-3 L/V = 0.in = 0.95 m2 and Dmin = 0. Note that L and V (parameters in slope of operating line) are in mole s-1 and QV and QL (parameters in flow parameter) in m3 s-1.25.25.5·12.13 are applicable for trays. Flow parameter = QL QV ρL = 0. However. 4. (This value can be calculated with Eq.7 m (Eq.85 b) The interfacial area ALV = 30·4. see exercise 3.046 ⋅ g . which can be read from Fig.138 (Eq.95 = 148. Calculate the number of real trays with Eq.10 once the flow parameter is known. 4.exp (-NOV) = 0. Solution a) L = (L/V)·V and V = QV·ρy with ρy = P/RT = 1403 mol m-3. Amin = QV = 4. Ptot or QV influence the column dimensions? (see Exercises 4.12) and the tray efficiency QV EMV = 1. Assume the lowest value to be on the safe side.186 and Ns = Nth 2 )/ EO = 2.DEG QV MCH4 kOV g = 0. its value is known to range from 30 to 100 m2 per unit surface tray area. 4.19: ln[ 1+ EMV (S − 1)] E0 = ln(S) In this case of absorption.12 is not known. the number of transfer units k ⋅A NOV = OV LV = 0. How would a change in the value of L/V.10 the corresponding value on the vertical axis is the limiting value. b.1 mol s-1 and QL = L·MDEG/ρDEG = 4. V = 4209 mol s-1. the flow rate is constant throughout the column. S = Aabs = L/KV = 2.out = 0. 4.4 GENERAL DESIGN OF G/L CONTACTORS Exercise 4.02 = 3 m3 s-1 = 0.1 (Eq. 4.85 ⋅ uflood 4Amin = 2. the height of the column Conversion of mole fractions to mole ratios is not necessary in this case.13). 4.001 xwater.

999 N = 5 trays kOV = 0.77 m2 T = 294K Mair = 0. b. 4.932·294/273 = 1. Solution a. Thoughts a.029 kg mol-1 R = 8. Hence the overall efficiency Eo = Nts/Ns has to be calculated from Eq.4 Given QL = 0. With Eq.078 kg mol-1 1 atm = 1.8 ms-2 MB = 0. xout follows from xin (saturated solution) and the actual stripping factor.388·10-6 (0.932·105·1.01325 bar B Find a. L = QL·ρwater/ Mwater = 833.932 m3STPs-1 Atray = 1.999 . The actual number of theoretical stages Nts = Eo·N = 0. Nts +1 f= S Nts +1 −S e.62 and the actual value of B B B c. SOLUTIONS TO PROBLEMS 4.6 mol/s. The mole fraction benzene yB in the gas phase = PB In equilibrium (saturated solution). Ns < 5. 4.104 bar Mwater = 0. the capacity can be somewhat higher.706 transfer units.5 Exercise 4. 2.5/1.34) is applicable Use the number of transfer units NOV from Eq. Substitution of the values of S and EMV gives Eo = 0.13 the resulting plate efficiency EMV = 1 – exp(-0.506.5 m2. = 0.9: Ns = Nts/Eo.59.999.0080·88. hence the stripping factor can be even (slightly) higher than the required value of 0. xin = yB / KB = 6.018 kg mol-1 g = 9. The real number of stages should be not larger than N = 5. V = QV·ρy = QV·Ptot/RT = 0. 4. 4. f. The volumetric flow rate at 1 bar and 294 Q = 0. the number of theoretical stages. 4. 3. From Eq. Nts the plate efficiency.999 or. 4. 3. with f = 0. 1. c.31·273) = 41. d. the stripping factor S = K·V/L has to be calculated. b.31 J mol-1 K-1 ρwater = 1000 kg m-3 Ptot A KB B = 1 bar = 50 m2 per m2 tray area = 152 fraction f stripped = 0.00 = 0.12 follows NOV = 0. e. where V and L are in mol/s.0080 m s-1 0 PB = 0. The Kremser equation in the form of the amount stripped (Eq. because f ≈ 1.3 mol/s and follows S = K·V/L = 7.00 m3s-1. is given by Eq. hence Nts = 3. The minimum airflow is determined by the maximum slope of the operating line which.724 and Ns = 4. d.84·10-4 (Eq.3).Fundamentals of Industrial Separations. 0 / Ptot= 0. Take Hspacing = 0. 4. c.34. d.706) = 0.99943 .19. b. Check the minimum and maximum allowable gas flow.724·5 = 3.01325/(8.015 m3s-1 QV = 0.13. The total LV-bubble interphase area ALV = A·Atray = 88.5 m.9% under the given conditions xout out how a change in airflow will effect the operation a way to dispose of the benzene in the effluent safely. EMV out whether the fraction benzene stripped is at least 99. In order to apply Eq. coincidences with the equilibrium line: 3) = Nth in Eq.61.34 theoretical stages 3 . f= S Nts +1 −S −1 S Nts +1 = 0. −1 S xout = (1 – f)·xin = 0.12 to calculate EMV in Eq.104 (Eq.5). The real number of stages.4 ppm). Ns. e.19 .

which is 25% higher than the actual flow. Q Qmin ≈ 0.max L/V K yin xout xin L /V max − y in −0 y y y = out.132 m3 s-1.013 1 ρ ⋅ V Hspacing ⋅ g ρwater = 0.48 mol s-1.max = K x in − (1− f ) x in x in − x out x in For clarity.max = out.16.10 uflood = 0. ρV 1. Not taken into account is the influence of flow rate on the interphase area. QL Q ρwater 0.431. The flooding velocity determines the maximum airflow. which is appr.203 From Fig.25 Q Q It should be noted that in the comparison above.max ≈ out.85·0.4. however.830 = 0.00 1.25 m3 s-1. higher flow rates may decrease bubble diameter and increase ALV. 4. max = 1. 6 times smaller than the actual flow.830 ms−1. and Qmin = 0. .705 m s-1. the value of xout in the figure above corresponds to f = 0. Working at a higher capacity by increasing both L and V does not change the stripping factor either.203 kg m-3 and ρV Q = QV·294/273 = 1.473 mol m-3. Vmin = L/K = 5. a reasonable assumption because generally kOV and QV are proportional in a wide range of flow rates.9996 this point would almost coincidence with the origin). the efficiency is assumed to be constant.00 m3 s-1.80 (with f = 0. f.6 GENERAL DESIGN OF G/L CONTACTORS yout. ρV = Ptot/RT = 41. Qmax = umax·Atray = 1. The flow parameter = QL Q ρwater with ρV = ρy·Mair = 1. at low concentrations it is standard practice to burn the traces.015 1000 = = 0. Benzene may be recovered by cooling. umax = 0. Qmin = Vmin/ρy.

18 is to be used. 4. Thoughts Fig.02 K L/V y out = 0. e.max − x in y in − x in −0 32 KSO2 the actual liquid flow rate is 20% higher. = 2. the volume flow Solution QL = 0. isothermal operation fraction ammonia absorbed 90% Mair = 0.029 + 0. QV = 5·8.001 .018 kg mol-1 xin =0 KSO2 = 32 T = 285 K.36 applicable. MV = 0. b. d. 4. ρV Read the ordinate in Fig.32 relates Hcolumn.31 J mol-1K-1 = 2. calculate absorption factor A Eq.02 − 0. kOV minimum flooding velocity ySO2 in effluent at 75% of maximum airflow rate translate figure in solution to exercise 4.005) = = = 54.017 = 0.0 mol s-1.6) to absorption (position operating line!) low concentration.90 Find Lmin b. SOLUTIONS TO PROBLEMS 4. isothermal operation εbed = 0.46 m s-1.5 / 1000 = 5·10-4 m3 s-1. .18: uflood uflood(Fp = 540) = 1. ρV = 105 ⋅ MV Q = 1.166 kg m-3.029 kg mol-1 xNH3 = 0. uflood(Fp = 125) = 2.18 m s-1.max 0. The largest vapor stream is found at the bottom of the column and the flooding velocity should be calculated at these conditions.Fundamentals of Industrial Separations. d. 4. To calculate uflood at a given value of the packing factor. 0.81 m s-2 Mwater = 0. Exercise 4. 0.95·0.18.005 ρL = 1000 kg m-3 Ptot = 1 bar D = 0.Solution a.0 m = 200 m2 m-3 Mair = 0.7 Exercise 4.4 (page 4.02 = 65 mol water s-1 = 8. e.5 kg water s-1 F25raschig = 540 m-1 Mair = 0.25 mol s-1 = 0.029 kg mol-1 Ptot = 1 bar Find the flooding velocity for both types of packings rate and the density of both phases have to be calculated.05 ρL = 1000 kg m-3 F25hiflow = 125 m-1 T = 20°C.02 x out. Equation 4.025 y in = 0.33 m g = 9.120 . constant flow. hence the flow parameter = L R ⋅T QV Fp ρV ⋅ = 0. Lmin = V ⋅ ( y in − y out ) V ⋅ ( y in − y out ) 2.122 m3 s-1.31·293/105 = 0.5 Given V = 5 mol s-1 MNH3 = 0. Fp.028 kg mol-1.005 0x = 0 in x out.017 kg mol-1 ΦL = 0. Just changing the air volume flow rate changes NOV as well as the absorption factor. Thoughts a. kOV (via Htu) and NOV calculate the flow parameter and uflood from the corresponding value at the ordinate in Fig.30 g ρL ρL = 0. 4.05·0. c.6 Given V yin L R H a a.25 ⋅ (0. NOV c.029 kg mol-1 yout = 0.

605 m. Q ρL Flow parameter = L ⋅ = 0.0850 = 17.36 is applicable: ⎡ 1 0.552 m.25 ⋅ = = 0. Htu ⋅ Ah 0.68 ⋅ 10−3 m s . 4. Qy = (π·D2/4)·uflood·0.903 0. (umax = 0.903 0. QV ρ y ⋅ M air uflood = 0.0/3.466 mol s-1 Sabs = A = L/KV = 0.779 m s-1.172. corresponding to 0. 4.25 = 2. 4.0533 m3 s-1 and 5 42. 4.605 = 3.36 for yout: yout = 5.903 − 1 ⎣ 0.005 − 0 0.552 ⋅ 17.3 m-1. Increasing the gas flow decreases NOV = Hcolumn/Htu = Hcolumn·kOV·Ah/Qy and decreases the absorption factor Sabs = A = L/KV. By definition (Eq. QL = L·Mwater/ρL = 1. which is almost 20% higher than the value at the lower gas flow. NOV = 2/0. 4.62 = 0.32 Htu = Hcolumn/NOV = 2.0584 m3 s-1 Htu = 0. Absorption factor Sabs = A = L/KV = 0. .0 m /m QV 0.33): kOV = QV = V mol/s 3 c.25) Fp = a/ε3 = 274.020 − 0 1 ⎤ NOV = ⋅ ln⎢ + ⋅ (1− )⎥ = 3.18 = 0.0584·42. QV with Htu ⋅ Ah ρ y mol/m π 4 =V ⋅ RT 8.4.17·10-3 m3 s-1.75 = 0. kOV does not change.842 Now solve Eq. Linear operating and equilibrium lines.2 Ptot 10 2 Ah = a ⋅ kOV = D 2 = 200 ⋅ 0.8 GENERAL DESIGN OF G/L CONTACTORS b. hence Eq.916 m s-1. Estimation of the packing factor (page 4.2 = 2.31 V = Qy·ρy = 0.903 ⎦ From Eq.85·uflood = 0. assuming Ah is constant.903.0662 m3 s-1) e.31⋅ 285 2.0533 -1 = = 5.617 -> ordinate in Fig.172 Fp ρV ⋅ g ρL = 0.93·10-3.24 – 4.0 d.62 0.

1 A water solution containing 0.0008 Toluene yN+1 S=1000 N=9 xÕ N Figure 5.0001 mole fraction benzoic acid. b. Determine R’ and xN’ for the regeneration column c.01 R=100 y1 Water xÕ 0 =0. Water and benzene can be assumed almost insoluble. dioxane benzene/wtfr.2.1.005 mole fraction of benzoic acid is to be extracted by pure toluene as the solvent. dioxane water). A single batch extraction Two crosscurrent stages using equal amounts of benzene Two countercurrent stages An infinite number of crosscurrent stages An infinite number of countercurrent stages . Extraction of acetic acid Exercise 5. Exercise 5. RÕ 40 C 25 C N=11 xN=0. Calculate the solvent requirements for: a.033 at 25°C and 0. If the feed rate is 100 moles/h and the solvent rate is 100 moles/h. a. c.2 The system shown in Fig.1 is extracting acetic acid from water using toluene as the solvent. Is this a practical way to concentrate the acid? Feed x0=0. find the number of equilibrium stages required to reduce the water concentration to 0. A temperature shift is used to regenerate the solvent and return the acid to the water phase. Determine y1 and yN+1 for the extraction column b. d.102 at 40°C. 5.2. The indicated number of stages refers to equilibrium stages.3 1000 kg of an aqueous solution of 30 wt% dioxane is to be treated with benzene at 25°C to remove 95% of the dioxane. Compare the McCabe-Thiele method with the analytical Kremser method. SOLUTIONS TO PROBLEMS 5-1 Chapter 5: LIQUID-LIQUID EXTRACTION Exercise 5. The distribution coefficient of dioxane at low concentrations is constant and has a value of KD = 1. The benzene is dioxane free. Operation is isothermal and countercurrent. The distribution coefficient of acetic acid between the toluene and water phase (KD = yA/xA) amounts 0.446 * mole fraction benzoic acid in toluene.Fundamentals of Industrial Separations.2 (wtfr. The equilibrium represented by: mole fraction benzoic acid in water = 0. e.

Inlet butanol is pure.613 (wtfr. Find the number of equilibrium stages required and the ratio of water to 1-butanol by using the McCabe-Thiele diagram design method. d.5 1000 kg per hour of a 45 wt% acetone in water solution is to be extracted at 25 °C in a continuous countercurrent system with pure ethyl acetate to obtain a raffinate containing 10 wt% acetone. determine with the aid of a ternary diagram: a.5. b. in butanol/wtfr.5 wt% in the water and 9. We desire outlet concentrations of 0.5 wt% mixture of acetic acid in water is to be extracted with 1-butanol at atmospheric pressure and 25°C in countercurrent operation.6 wt% in the butanol.2 EXTRACTION Exercise 5.5 89 10 7 3 2 1 0. Required steps: a. number of stages required for a solvent rate equal to 1.5 Extract Raffinate Tie-line data . flow rate and composition of each stream leaving each stage Acetone wt% 60 50 40 30 20 10 55 50 40 30 20 10 Raffinate wt% acetone 44 29 12 Water wt% 13 4 3 2 1. The minimum flow rate of solvent b. c. Using the following equilibrium data. in water).5 times the minimum c. Convert the streams and equilibrium data to mass ratio units Plot the equilibrium curve Plot the operating curve to determine the water to 1-butanol ratio Step off the equilibrium stages Exercise 5. The acetic acid equilibrium distribution is given by K = 1.5 1 35 43 57 68 79 89.4 An 11.5 Extract w% acetone 56 40 18 Ethyl acetate wt% 27 46 57 68 78.

The flow diagram of this extraction section is shown in Fig. b.Fundamentals of Industrial Separations. In the first column caprolactam is extracted from the aqueous phase. SOLUTIONS TO PROBLEMS 5-3 Exercise 5. determine the final concentration of caprolactam in the water after both extractions. The initial concentration amounts 65 wt% caprolactam.7. Equilibrium data are as follows: TMA wt% 5 10 15 20 25 30 35 40 5 10 15 20 25 30 35 40 Extract wt% TMA 40 22 13 8 4 Water wt% 95 89 84 78 72 66 58 47 0 0 1 2 4 7 15 34 Raffinate w% TMA 31 15 9 7 3 Benzene Wt% 0 1 1 2 3 4 7 13 95 90 84 78 71 63 50 26 Extract Raffinate Tie-line data Exercise 5. find the original feed composition and the water-to-feed ratio with the graphical ternary diagram method. Determine the caprolactam concentration (wt%) in and the amount (ton/hr) of the extract stream when 1.6 Benzene and trimethylamine (TMA) are to be separated in a three-stage liquid-liquid extraction column using pure water as the solvent. 70 and 3 wt% TMA. The objective of this extraction is to obtain an aqueous raffinate stream with only minimal amounts of residual caprolactam. . a. If the solvent-free extract and raffinate products are to contain respectively. Determine the minimal required solvent flow for the first column.1 on next page.7 Caprolactam is industrially recovered and purified by extraction with benzene. 5.5 time the minimal required benzene stream is used. When 15 ton/hr water is used for the extraction in the 2nd column. c.

3 81.6 51.4 95.6 Benzene wt% 100.0 0.6 74.2 23.7 1.9 90.0 7.2 37.0 45.5 Caprolactam wt% 0 1.0 98.0 71.0 Caprolactam wt% 0 9.5 18.2 10.7 1.8 Suggest the extraction equipment that should be considered for: a.4 EXTRACTION Benzene + Caprolactam(+W) Caprolacta R2 E1 65 wt% Caprolactam in Water 20 ton/ ton/h Pure Water F1 S2 S1 Pure Benzene F2 Water R1 Water + Caprolactam Caprolactam(+B) E2 Figure 5.4 82.4 0.1 0. Extraction of large volumes of copper ore leachate with only 2 to 3 stages required b.2 2.3 3. Extraction of caprolactam Equilibrium data at 20°C are as follows: Extract Water wt% 0.5 4. Recovery of penicillin from an fermentation broth .1 0.3 88. Recovery of caprolactam from aqueous carrier stream in chemical plant c.5.1 Exercise 5.2 0.9 16.0 39.0 8.4 Benzene Wt% 0.4 0.7.9 53.1.1 61.6 28.8 91.2 0.4 Raffinate Water wt% 99.

Fundamentals of Industrial Separations. Determine the size and composition of the extract leaving the second stage. 5. Determine the value of flow E1. SOLUTIONS TO PROBLEMS 5-5 Exercise 5.2. d. The concentration of pyridine in the raffinate RN should be reduced to 5 wt% (or less). E1 1 F=R0 E2 2 R1 R2 N S=EN+1 RN Figure 5. a. This stream should be purified in a counter current extraction process (see Fig.9. Determine the number of equilibrium separation stages. . c. Calculate the minimum solvent stream. compositions in wt%. 5. Pure benzene is to be used as solvent S.11 kg s-1 comprises of pyridine and water in equal weights. The ternary equilibrium diagram of water-pyridine-benzene is given in Fig.1). N. E2. The solvent stream S is chosen to be 0. Equilibrium diagram water-benzene-pyridine. Smin.9 An aqueous stream F of 0.2. b.1.9.11 kg s-1.9. N-stages countercurrent extraction pyridine feed water benzene benzeen Figure 5.9.

13 ⎡⎛ x − y / K ⎞⎛ 1 ⎞ 1 ⎤ ⎡ 0.002 0.u. Exercise 5.1 op.005 − 0 ⎛ 1 ⎤ 1 ⎞ in ⋅ ⎜1− ln⎢⎜ in ⎥ ⎟⎜1− ⎟ + ⎥ ln⎢ ⎟+ ⎣⎝ x out − y in / K ⎠⎝ E ⎠ E ⎦ ⎣ 0.242 ⎦ N= = = 4. xout 0.1 Given x0 = 0. the remainder can be estimated as 0.) xN = 0.0001 x = 0.u. x’N and R’ for the regeneration column c.242.) Regeneration: x’0 = 0 KD = yA/xA = 0. 5. yN+1) and has slope =1.242 0.004 eq.005 xN = 0.13 ln E ln2.006 In the McCabe-Thiele diagram above. The two solutions agree well. 4 equilibrium stages are plotted on the equilibrium line (the upper one).6 EXTRACTION SOLUTIONS Exercise 5. by the McCabe-Thiele method and the Kremser equation Thoughts The equilibrium relationship is given.006 y yout 0. E = K·F/S = 2.002 xin 0 0 0. ≈ 0.33 is applicable with mole fractions. is this a practical way to concentrate the acid? .242) yN+1 = 0 F/S = 100/100 =1 isothermal operation Find N. y1 and yN+1 for the extraction column b.446·y (K = 2.1 equilibrium stage. Kremser Eq.102 N = 11 S = 1000 (a.242 ⎠ 2.5.0001− 0 ⎝ 2. number of equilibrium stages.004 x 0. the operating line intersects (xN.01 KD = yA/xA = 0. Solution Number of stages from the Kremser equation: N = 4.033 N =9 T = 25°C Find a.2 Given Extraction: x0 = 0. Both lines are straight.0008 T = 40°C R = 100 (a.

5. the value of K = 1.33) can be used because the solute concentrations are sufficiently low. 5. a large amount of recycle toluene and a temperature shift.98)·300 = 15 kg per unit time.) x’N is calculated from the overall mass balance of the regeneration section: S ⋅ yN ′ +1 + R′ ⋅ x o ′ = S ⋅ y1 ′ + R′ ⋅ x ′ ′ = 0.12 and 3. The resulting aqueous stream is still quite large and the concentration is hardly twice the feed concentration (0. 2.u. 0. 3.1.05 and K = 1.9. b. Dioxane in = 300 kg per unit time. When using weight Solution In all cases. Alternatively. All ‘y’ (toluene) concentrations are known from the previous part.018).2 The solvent-to-feed ratio follows from the extraction factor: E = S E K ⋅S ↔ = F F K .16 and 5. the phases x and y should be renamed and the equilibrium constant recalculated. Solution a. a. 70 wt% water Solvent: 100 wt% benzene K = 1. dioxane out = (1 – 0. Exercise 5.Fundamentals of Industrial Separations.33 for stripping): A = R’/K·S. As the direction of mass transfer is changed. single batch in Eq. Xout/Xfeed = (15/700)/(300/700) = 0.565 → R’ = K⋅S⋅A = 51. Xout/Xfeed = 0. 5.17 and countercurrent operation in Eq.01 resp. 5. The only unknown in the Kremser equation is yin = yN+1. benzene/water) T = 25°C Isothermal operation Water and benzene immiscible Find The solvent/feed ratio for 95% dioxane removal for a number of process configurations ratio’s. Calculation of yin and yout in a MathCad work sheet: b. 3.28 for absorption and Eq. 5. crosscurrent operation in Eqs. No. Apply overall mass balance to extraction column with yout = y1 and E = K·S/R. so the Kremser equation can be used once more. 3. SOLUTIONS TO PROBLEMS 5-7 Thoughts The Kremser equation (Eq. Thoughts Weight ratios have to be used because the concentrations are rather large.13). the Kremser equation should be adapted (compare Eq. Adapted Kremser equation for the regeneration column with xin = 0: ⎡⎛ 1 ⎞ y 1⎤ ln⎢⎜1− ⎟ in + ⎥ R′ ⎣⎝ A ⎠ y out A ⎦ with A = and N =9= KS ln A y = K ⋅x Solving for A gives A = 1. Note that yout(extraction) = yin(regeneration) and vice versa. This operation requires two columns.0178 N → xN c.8.6 (a.2 (wt fractions.2 can still be used(see Eqs.23a.3 Given Feed: 30 wt% dioxane.05. The extraction factor is defined in Eq.

Check that the Kremser equation is also applicable. Thoughts The steps that have to be taken are described in the assignment.3).9 X out 1 S 19 = = 0. equal amounts of benzene (Eq. 1 S 6.23a): 1 1 X∞ = = 0.5 wt%.78 2 F 1.5.2 Exercise 5. Assume that conversion to weight Solution is given on page 5. Infinite number of crosscurrent stages (Eq.2 X feed 1+ E b.05 ⇒ E = 19 and = = 15.8 EXTRACTION a.613 (weight fractions) y1 = 0 wt% yN+1 = 9.00 and = = 2. Infinite number of countercurrent stages (Eq.8 F 1.89 and S 3. Two countercurrent stages (Eq. The straight line through the origin is the equilibrium line.94 X2 = = 0.9 as a MathCad worksheet. 5. Single batch extraction: Eq.94 and = = 5. half of the total amount of benzene is used.95 (Use lim N → ∞ for = 1− E for E < 1) ∞ N X feed n n ∑E ∑E n= 0 n= 0 S 0. almost 4 equilibrium stages are required for an acetic acid reduction from 11. 5.24 F 1.0 = = 0.16): In each stage. 5. Two crosscurrent stages.95 = = 0.17): X∞ 1 S 3.5 wt% = 0. 5. .2 d.5% to 0.50 X feed exp(E ) F 1. The solvent-to-feed ratio is the slope of the operating line. because both operating and equilibrium line are straight.23a): X2 = X feed 1 ∑ En n= 0 2 = 1 1+ E + E 2 = 0.89 = = 3.4 Given x0 xN T y/x = 11.2 X feed ⎛ ⎞ ⎜1+ E ⎟ ⎝ 2⎠ c.05 → E = 6.05 → E = 3.2 e.5 wt% = 298 K = 1.05 → E = 0.6 wt% p = 1 bar Find The number of stages and the water-to-butanol ratio ratio’s assures a constant K-value in the given concentration range (see also Exercise 5.05 → E = 3. 5.79 F 1.

with tie lines Feed F: (AC-H2O-EA) = (0. The new mixing point M can be calculated from the mass balances. The minimum solvent flow rate Smin is found if an infinite number of equilibrium stages is used.005) Solvent: pure EA = (AC-H2O-EA) = (0. number of stages N for S = 1. the operating line through the feed point F and the first extract E1* is parallel to the nearest tie line. E2 is found from extending the operating line through P and R1. the overall material balance and component balances for two of the components have to be evaluated.5 Given Ternary phase diagram for acetone (AC)-water(H2O)-ethyl acetate (EA). SOLUTIONS TO PROBLEMS 5-9 Exercise 5. minimum flow rate of solvent Smin b. . Now.55.Fundamentals of Industrial Separations.5 · Smin c. 0. b. etcetera. 0. In that case. 1) a. The first extract composition E1 is found by extending the line through RN and the new mixing point.10. 0. To calculate the compositions and flow rates. The corresponding mixing point Mmin is located at the intersection of F-S and RN-E1*.895. The indifference point P is found by extending the line between F and E1.45. R1 is connected to E1 by a tie line (equilibrium composition). a. the point Pmin can be found by extending the line through E1* and F. 0) Desired raffinate: RN = (AC-H2O-EA) = (0. The composition of E1* can be read from the chart. 0. flow rate and composition of each stream leaving each stage Find Thoughts All possible indifference points P are located on the line through S and RN.

02 0.74 0. b.N−1 ⋅ RN−1 + xE .01 EA 0.01 0.025 0.45·1000/M = 0.E ⋅ E + x H 2O.005 kg/hr 914 809 714 622 ≈500 acetone F M P Pmin Rn water * E1 S(EA) .3 kg/h and R = 536.04 0.5 c. The compositions can be read from the charts.45·1000 + 0 = 0. 0. E1 E2 E3 E4 E5 Ac 0.59 0.74 0. S = 1.E ⋅ E + x AC.84 0.M = 0.03 0.5.32 0. R1 R2 R3 R4 R5 Ac 0.M ⋅ M = x AC.E ⋅ E + x AC.02 0.S ⋅ S = x H 2O.55 ⋅ 1000 + 0 = 0.895 ⋅ R Results: E = 768.10 H2O 0.635 0.408 Solve E and R from both material balances: x AC.33) Material balances: * overall: + RN M = F + Smin = E1 per component: x AC.M ⋅ M = x H 2O.365 and xH2O. A small error is made when reading the compositions from the chart.89 kg/hr 769 673 590 472 ≈350 Raff.10 EXTRACTION c.38 0.43 0.M = 0.10 ⋅ E + 0.10 ⋅ R 550 = 0.2 kg/h and the total M = E + R = 1348.M = 0.S ⋅ S = x AC. Continuing the graphical solution defined above (see diagram) or solve the material balances for each subsequent stage (see c). it follows that N ≈ 4. so the mass balances do not close completely.F ⋅ F + x H 2O. 0.03 0.24 0.54 0.945 EA 0.F ⋅ F + x AC.5 ⋅ Smin = 348 kg/h and M = 1000 + 348 = 1348 kg/h xAC.E ⋅ E + x H 2O.M ⋅ M = x H 2O.M ⋅ M = x AC.04 ⋅ E + 0.8 kg/h.895 ⋅ R The flow rates of E and R can be solved from both component balances: E = 695.02 0.R ⋅ R → 450 = 0.333 and xH2O.R ⋅ R → x H 20.N ⋅ EN The approximate results are given in the table below.R ⋅ R → 0.05 H2O 0. see ternary diagram below. M = E + R = 1232. Use the material balance: xR.6 kg/h and R = 580.34 0.24 0.446 These values agree with the graphical result. Extr.R ⋅ R → x H 20.57. The composition of E1* can be read from the chart: (AC-H2O-EA) = (0.15 0.45 0.M = 0.51 0.N+1 ⋅ EN+1 = xR.8 kg/h.10·R 0.1 kg/h → Smin = 232.45·1000/M = 0.66 0.55·1000/M = 0.1 kg/h Location of point Mmin: xAC.10.57·E1 + 0.51⋅ E + 0. the flow rates are calculated from the material balances.55·1000/M = 0.N ⋅ RN + xE . Solution a.

By definition E2 and R2 are also connected by tie line and that the operating lines through E1 and R2 and through E2 and R3 both point P on the line S-R3.F ⋅ F = x benz. Find Thoughts A ternary phase diagram can be used to solve this problem.325. Finally.Fundamentals of Industrial Separations.97) Location of P. Furthermore.7/0. TMA.S = xTMA. From P and E1. the feed composition can be found by extending the line through P and E1: F = (H2O. 0.42.17) Raffinate TMA/benzene = 0.E 1 ⋅ E1 + x benz. benzene) = (0. The only unknown compositions are therefore E2 and R2. Because N = 3.323) TMA Extract F E1 E2 E3 P S(water) Raffinate R1 R2 R3 benzene . TMA. located on equilibrium line → extract = E1 = (H2O. As the raffinate and extract compositions Solution The compositions of extract and raffinate: Extract TMA/benzene = 0.556 (and E1/F = 1.F ⋅ F = xTMA. SOLUTIONS TO PROBLEMS 5-11 Exercise 5. x benz. 0.45) xbenz. Because the feed composition is unknown.03. R1 is connected to E1 by a tie line and E3 is connected to R3 by a tie line.03. R2 and R3 is found by trial and error. TMA. the water-to-feed ratio follows from the overall material balance and component balances. benzene) = (0.55.S = 0 and the three material balances read F + S = E1 + R3. the feed composition can be found. the raffinate is denoted R3.6 Given Ternary phase diagram for benzene (B) water (H2O) triethylamine (TMA). From P.3 = 2. benzene) = (0.E 1 ⋅ E1 + xTMA. 0.33. as shown in the graph.41. 0. E2 and R2 can now be found by trial and error.R 3 ⋅ R3 Solving for the three unknown flow ratio’s gives S/F = 0. the graphical method has to be used indirectly. R3/F = 0. 0. the compositions can be found easily.R 3 ⋅ R3 and xTMA. 0.97 = 0. with tie line data N = 3 equilibrium stages feed: mixture of benzene and TMA solvent: water solvent-free extract: 70 wt% TMA solvent-free raffinate: 3 wt% TMA The original feed composition and water-to-feed ratio (S/F) both have to be located on the equilibrium line.03/0. The correct location of P. The point P has to be located on the line through solvent S and R3. located on equilibrium line → raffinate = R3 = (H2O.

594.50.8 ton B/h.B = 40.5·Smin = 40.8/68. benzene . Draw a line through F parallel to the closest node line. F1 = 20 ton (C)aprolactam / h with xF. S = 1. c.7 ton E1/h.8 ton/h.0 = 16. xM2.M = 1. b. R2 = S1. E. Solution a. W = 0.1 ton/h.8 (B) + 0.5.02·40.60.C = 11. F2 = E1. Plot point M.7 = 0.M b.76. C = 0. xW = 0. Intersection of this line with the equilibrium line at the extract (benzene-rich) side gives the extract phase.1/68.0 ton/h.W = 8 / 60.8 ton/h. extend the line from W through M to the extract side of the equilibrium curve and read the composition of E1: xB = 0.22*40.172.6·F = 12.76 (C) = 53.67.22.7 = 0.7.76 (W) + 0. a.1 together with relevant equilibrium data. hence Smin = 27. C = 11.8/0.0 ton/h.46 B Caprolactam Solute 1 1 a.C = 0.W = 16.8/0. The mixing point M in the 2nd column now has the following overall composition: xM2. The figure on the next page shows how the mixing point M is constructed. W = 1. minimal solvent flow for first column concentration C(aprolactam) in E1 for S = 1. B = 40. giving a total of 68. Extend the line BM and read the composition of E2: xB = 0. defining the two liquid phases region.4·20 = 8.20.5·Smin final concentration of C in E2.13 and xM. xW = 0.04. representing particular raffinate – extract equilibria.7 = 0.197 and xM2.8 ton/h. The mixing point M in the first column now has the following overall composition: xM. with the highest possible concentration of C.36 .W = 0.8 = 0.B = 40.7 ton/h. xF.1+15.8 / 60.C = 0. B c.3 ton/h. This corresponds to 40. xM. This corresponds to the smallest amount of solvent B(enzene). 5. xC = 0. Find Thoughts The solution can be obtained from a ternary diagram with equilibrium line.12 FUNDAMENTALS OF INDUSTRIAL SEPARATIONS Exercise 5. giving a total of 60.8 = 0. The solvent-to-feed ratio follows from the ratio of the segments FM and MB: (S/F )min = feed . Construct this diagram and mark the composition of the feed on the CW-axes with F. and the node lines.8/68.7 Given A caprolactam extraction process is given in Fig.02 and xC = 0. S2 = 15 ton W(ater) / h. Feed (60 wt%) 40 ºC wi wi E(max) Raffinate (0 wt%) 0 Carrier Water M 0 P(min) 0 wi (gew%) 1 Benzene Solvent .4·F = 0.

a column extractor is most useful. c. therefore the short residence time in a centrifugal extractor is very advantageous. probably more difficult separation (N > 5). recovery of caprolactam from aqueous carrier stream.18 on page 5-24 of Fund. recovery of penicillin from a fermentation broth A suitable piece of extraction equipment for each case Find Solution Thoughts Apply the scheme in Fig.7c. depending on the available space in the facility. More data are required for the selection of the most appropriate column. no extreme risk of emulsification. The material to be extracted is relatively unstable and vulnerable. a. small floor area (common in chemical plants). extraction of large volumes of copper ore leachate with only 2 to 3 stages required. b. 5. Sepns. Large volume. Caprolactam Solute 1 1 40 º C Extract wi wi Feed M 0 Carrier Water 0 Raffinate (0 wt%) 0 wi (gew%) 1 Solvent Benzene Exercise 5.Fundamentals of Industrial Separations. either a series of mixer-settlers (quite common for the large volumes in metallurgy) or a column separator.8 Given Three extraction cases: a. SOLUTIONS TO PROBLEMS 5-13 5. Extraction of large volumes of copper ore leachate with only 2 to 3 stages required Large volume. potential emulsion formation (Æ centrifugal extractors or certain columns). . c. Recovery of penicillin from a fermentation broth Volume will be relatively low Æ separators or centrifugal extractors. A centrifugal extractor is probably too expensive for a relatively simple. large-volume separation. Ind. b. Recovery of caprolactam from aqueous carrier stream. small number of stages.

until Rn ≤ 0. Smin = 0.12 kg s-1 (R1 = 0. Three unknowns. Firstly. b. Then.g. b.9 Given Find Countercurrent extraction of pyridine (50 wt%) from an aqueous feed F (0. c. d.17 kg s-1.06 kg s-1).05 . Size and composition of E2.2B). xRpyr = 0. b. Alternatively. calculate Smin from the overall mass balance: F + Smin = RN + Emin Apply the overall mass balance: F + S = RN + E1 and an appropriate component balance A graphical solution: Mark the intersection of the extensions of F-E1 and RN-S. . Emin and RN.10 (read from the diagram) it follows that E2 = 0.173 kg s-1.11 kg s-1) with benzene.9. Smin. d.644. e. R2.S) all point to this operating point.66 (from diagram) or xEben = S/E1 = 0. R1 follows from E1 via the appropriate node line (equilibrium). xEpyr = 0. Following this procedure. hence the new mixing point M is exactly halfway F and Smin (see Fig. E1 = 0.131 and RN = 0. Emin.05 (required).052 kg s-1) Alternatively. S = F. R3 etcetera. Repeat the procedure outlined above to find. a. hence E2 is found as the intersection of R1-P and the phase equilibrium line.31 (read from diagram). RN.5. Draw F-Smin and RN-Emin. c. N. Repeat b for the stage number 1. find Emin leaving the 1st stage by drawing a straight line through F parallel to the nearest node line. R1 .071 kg s-1. xE ben ≈ 0. This is the operating point P. hence three equations are required: overall pyridine benzene F + Smin = RN + Emin xFpyr·F = xEpyr·Emin + xRpyr·RN Smin = xEben·Emin xFpyr = 0. 5.9. R1 . Lever rule: Smin/F = FM/MSmin = 0.EN+1 = RN .E2. solving for the two unknowns gives E1 = 0. The difference in flows between any two subsequent stages (F . Nts ≈ 3. Thoughts a. the unknowns Smin and RN can be calculated from the overall balance and the pyridine balance: overall pyridine F + S = RN + E1 xFpyr·F = xEpyr·E1 + xRpyr·RN xE pyr ≈ 0. Draw a straight line from RN to M and extend until its intersection with the phase line. Lever rule: E1/(E1 + RN) = MRN/E1RN = E1/(F + S).40 and xEben = 0. E3. Minimum solvent flow Smin for the process to work.: overall pyridine F + E2 = E1 + R1 xFpyr·F + xE2pyr· E2 = xE1pyr·E1 + xRpyr·R1 With xRpyr ≈ 0.073 kg s-1 (Emin = 0. respectively.50 (given).24 and xE 2 pyr ≈ 0.64 c. Smin = 0. The intersection is the mixing point M (see Fig.2A). points to P. 5.14 FUNDAMENTALS OF INDUSTRIAL SEPARATIONS Exercise 5.56 (read from the ternary diagram). Solution a.E1.E2. This gives point E1. RN . d. a graphical solution leads to approximately the same result. The unknowns R1 and E2 can be calculated from two equations. Extract flow E1 leaving the first stage for S = F The number of equilibrium extraction stages. Solve for Smin.

9.2B .9. 5. 5.Fundamentals of Industrial Separations. SOLUTIONS TO PROBLEMS 5-15 pyridine feed Emin Mmin RN Smin water wt% benzeen Fig.2A pyridine feed E1 R1 R2 R3 M E2 E3 S wt% P water benzeen Fig.

5.16 FUNDAMENTALS OF INDUSTRIAL SEPARATIONS .

kg/kg c = concentration of nitrobenzene. 1.770 95. the equilibrium adsorption isotherm appears to be linear: q = K·c with q = amount adsorbed.5 17.1 23. Fit both sets to a Langmuir-type isotherm and compare the resulting isotherms with the experimental data.2 9.9 and 1.9 12.5 1 2 5 10 12.092 1.096 100.1 125.260 55. kg/m3 1 K = Henry constant = 675 m3/kg V m3 waste water c in How many kg of activated carbon is required per m3 of treated water? 1 mC kg active carbon In Eqs.2 90.239 4.1 The following table gives the Langmuir isotherm constants for the adsorption of propane and propylene on various adsorbents.223 147.130 2.1 Chapter 6: ADSORPTION & ION EXCHANGE Exercise 6.1 4.0 Water (in toluene) on Activated Alumina c q (ppm) (g/100g) 25 50 75 100 150 200 250 300 350 400 1.01 0. Toluene (in water) on Activated Carbon c q (mg/l) (mg/g) 0. b.2 54. The solution is fed to an ideally stirred tank containing mC kg adsorbent.10 bA and b’A are Henry constants . c. see outline.000 58.915 Which component is most strongly adsorbed by each of the adsorbents Which adsorbent has the greatest adsorption capacity Which adsorbent has the greatest selectivity Based on equilibrium conditions.5 10. d.458 34. Adsorbent ZMS 4A ZMS 5A ZMS 13X Activated Carbon a. which adsorbent is the best for the separation Exercise 6.412 100.889 b (1/bar) 9.2 The following data were obtained for the adsorption of toluene from water on activated carbon and water from toluene on activated alumina.3 An aqueous amount of V m3 contains 0.5 165.226 2.919 2. SOLUTIONS TO PROBLEMS 6.5 30.436 2.Fundamentals of Industrial Separations.3 Exercise 6.2 0.05 0.01 kg/m3 of nitrobenzene.1 13.1 6.5 70.1 0.3 39.02 0. We want to reduce this to 10-6 kg/m3 by adsorption on activated carbon.680 4.2 5.9 3. Adsorbate C3 C3= C3 C3= C3 C3= C3 C3= qm (mmol/g) 0. At these low concentrations.5 8.

015 m3 s-1. the bed porosity εbed = 0. How long does it take to regenerate the column? In the second process. m s -3 Cf kg m W kg adsorbent in packed bed V m waste water -3 Cf kg m W kg adsorbent in ideally mixed tank 3 .0 m. Calculate from a component balance the amount of carbon per unit volume of waste water (Wcol/V in kg/m3) a2. an ideally stirred tank. it is regenerated with a water flow of the same size in which the concentration of nitrobenzene amounts to 2·10-5 kg m-3.6 and the particle density ρpart = 800 kg m-3.02 kg/m3 to a value of not more than 2·10-5 kg/m3.6. The length of the column L = 2. The rate of convective transport through the bed is such that local adsorption equilibrium is established throughout the column. Calculate the excess amount of carbon to be used in the batch process compared to that required in the continuous process. Nitrobenzene can be removed from water by adsorption on active carbon. a1. and .2 ADSORPTION & ION EXCHANGE Exercise 6. b2.4 Nitrobenzene in an aqueous effluent should be reduced from its initial concentration of 0. its diameter D = 0. b1. How much waste water (V in m3) is purified when the column is about to break through? After saturation of the column. calculate Wbatch / Wcol. a3. in other words.a batch process in an ideally stirred tank (see process scheme b below) The packed column contains Wcol kg carbon and is fed with wastewater at a rate of Q = 0. Comment on the answer of part b1. as long as the column is not saturated. The concentration profile is flat (plug flow). the outlet concentration is zero. This batch is treated with Wbatch kg active carbon. a Φf V m 3 b W kg Φf 3 -1 Q waste water. V m3 waste water (as calculated in part a1) is treated.a packed column (see process scheme a below).6 m. After equilibration the resulting concentration of nitrobenzene should be 2·10-5 kg/m3. The amount q of nitrobenzene adsorbed in equilibrium with its concentration c in water is given by the following Langmuir isotherm: q (c ) = 510 ⋅ c 1 + 4550 ⋅ c with c in kg/m3 and q in kg/kg Two different process schemes (see outlines below) are considered to carry out the required reduction: .

Exercise 6. desorption with He) the total gas flow ΦV was maintained at 4·10-6 m3/s at 20°C and 1 bar. In all experiments (flushing with He. In this equipment and at these conditions.cCO2 where monolayer capacity qm = 1. adsorption and desorption are isothermal processes.39 mol/kg. The temperature was kept constant at 20°C. Explain the form of the breakthrough curve qualitatively. They had to compare the results with a theoretical model based on local adsorption equilibrium. Calculate the desorption time. A column (L = 1 m.31 J/mol K. the adsorption constant b = 0.τ1.6 A couple of students got an assignment to determine experimentally the residence time of CO2 during adsorption and desorption in a packed bed column. internal diameter D = 5 mm) was filled with activated carbon and its exit provided with a CO2-detector. the feed was switched to pure He. The adsorption of CO2 at 20°C is given by a Langmuir-type adsorption isotherm: b. τ∞ . At time τ0 a CO2-He mixture. R = 8. adsorption with He/CO2. 6. b.g. 6. The concentration CO2 in the effluent was measured continuously and is given schematically (not to scale) in the plot below: cexit start adsorption start desorption time τ0 τbreakthrough τ1 τd τ∞ Additional data The particle density of the carbon ρpart = 790 kg/m3 and the bed porosity εbed = 0. Explain. . The following problems are to be addressed: a. containing 4 vol% CO2. at time τ1. this gives the same result as in part b. 6.5 Derive the expression for the time tsat required to saturate a freshly regenerated column (Eq.3 Exercise 6.Fundamentals of Industrial Separations. using Eq. c.22. was fed to the column. e. d. Some students calculated the breakthrough time from the ratio of the maximum amount to be adsorbed and the flow rate of carbon dioxide: τ breakthrough − τ 0 = Ws × q (cf ) Q * cf When calculated properly.40.23.τ0.cCO2 q = qm 1+ b. The column was pretreated by flushing with pure Helium. Some time after saturation.068 m3/mol and the concentration c is in mol m-3. Calculate the breakthrough time. τbreakthrough .22) from the mass balance over the entire column as given in Eq. SOLUTIONS TO PROBLEMS 6.

2 times the minimal ion exchanger stream. d.6. e. a. The concentration M+ has to be reduced from 15 to 1 mol/m3.0811 kg/mol) has been attached to each benzene ring. The concentration M+ on the incoming regenerated ion exchange resin equals 200 mol/m3. Determine the equilibrium diagrams for extraction and regeneration when the total ion concentrations in the resin. Determine the minimal required ion exchanger stream Determine the number of equilibrium stages and concentration M+ in the outgoing ion exchange resin for 1. The regeneration liquid contains 3000 mol/m3 Na+ and no M+.104 kg/mol) and 12 wt% divinyl benzene (MW = 0.8 A continuous stream of a soil/water mixture (0. c.3 m3/s) containing 15 mol/m3 of a heavy metal M+ is treated with an ion exchange resin to remove the heavy metal by exchange against the sodium Na+ ions present on the resin.7 A commercial ion-exchange resin is made of 88 wt% styrene (MW = 0.4 ADSORPTION & ION EXCHANGE Exercise 6. b. Estimate the maximum ion-exchange capacity in equivalents/kg resin when an sulfonic acid group (MW = 0.1302 kg/mol).2 times the minimal regeneration stream . Exercise 6. soil/water mixture and regeneration solution are given by: Resin: Soil/water: Regeneration liquid: [C+] = [Na+] + [M+] = 2400 mol/m3 [C+] = [Na+] + [M+] = 30 mol/m3 [C+] = [Na+] + [M+] = 3000 mol/m3 and the equilibrium follow ideal behavior with an equilibrium constant K = 5. Determine the minimal value of the regeneration liquid stream to obtain a regenerated resin with 200 mol/m3 residual M+ How many equilibrium stages are required with 1.

10.d. It can accommodate the largest number of molecules on its internal surface area. but what is the definition of the ‘best’ adsorbent? It is helpful.9 and 1. to plot the 8 adsorption isotherms in a single graph: Thoughts The strongest interaction can be found by comparing the values of adsorption constants (see Eq. which is defined in Chapter 1. Eq. The intrinsic selectivity is given by the separation factor. and is the best adsorbent for the propene – propane separation. much larger than for other zeolites.8). .Fundamentals of Industrial Separations. 1. ZSM 4A shows a ratio of about 10. The system propene – ZSM 5A has the highest b-value. 6. the separation factor equals the ratio of the initial slopes in the Langmuir plots above. 5 q / mol kg-1 4 Activated Carbon / C3 Activated Carbon / C3 = 3 = ZSM 13X / C3 ZSM 5A / C3 = 2 ZSM 5A / C3 ZSM 13X / C3 1 = ZSM 4A / C3 ZSM 4A / C3 0 0 0. qm. It should be noted that the parameter b in Eqs.8). Activated carbon has the highest value of the monolayer capacity. With this notation. hence the highest heat of adsorption (see Eq. = The best adsorbent for the C3 − C3 separation 6. b.5 SOLUTIONS Exercise 6. the Langmuir isotherm transforms into a linear isotherm with slope qm·b.05 0. At sufficiently low pressures. 1. c.1 0.15 0.1 Given Find Monolayer capacities and adsorption constants of a number of adsorbent – adsorbate combinations.2 p / bar Solution a. SOLUTIONS TO PROBLEMS 6.10 represents the slope of a Henry or linear isotherm.

plotting 1/q as a function of 1/c q c qmb q m would result in a straight line with intercept 1/qm and slope 1/b·qm. With these two parameters. whereas the adsorption data of water in the lower concentration range show a linear Langmuir plot. The Langmuir equation is not a linear 1 1 1 1 = ⋅ + .05 0. Solution For both systems a least square method is applied to all data points of both systems.1 1/q 1/q 0. Toluene on activated carbon 200 adsorbed / g kg-1 Water on activated alumina 150 adsorbed / g kg-1 100 100 50 0 0 5 10 0 0 200 concentration / ppm 400 concentration / g m-3 0. 6. Thus. Note that in both cases the amount adsorbed is expressed as g / kg.6.04 . as shown in the upper two graphs.2 Given Adsorption data for adsorption of traces toluene in water on activated carbon and for traces water in toluene on activated alumina Find Do these two different systems obey Langmuir type of adsorption? one but it can be linearized easily. The reciprocal of Eq.06 0. solid lines are the calculated (regression) lines. the Langmuir isotherms are calculated. Adsorption of toluene on activated carbon does not obey the Langmuir model. in case of Langmuir adsorption.02 0 0 50 1/c m3 g-1 100 0 0 0. see the lower two graphs. Symbols represent experimental data.02 1/c 1/ppm 0.04 0. then the value of b from the slope.7 gives linear relation between 1/q and 1/c: Thoughts Checking experimental data against a linear model is easy. qm is calculated from the reciprocal intercept.6 ADSORPTION & ION EXCHANGE Exercise 6.

6. q = K·c with K = 675 m3 kg-1 Find The amount of carbon per unit volume solution to ensure the required equilibrium concentration.20) with = c qm b (1+bc ) 2 (derived from the Langmuir equation.02) = 0.25πD2L(1 – εbed)ρpart = 181 kg and (applying part a1) V = W/0.02 kg/m3. During desorption. each with a velocity given by Eq. 6.6 h) and V = 0.180 kg /m3 a2. a. Dcolumn = 0.25πD2 = 0. c∞ = 2·10-5 kg/m3. The nitrobenzene mass balance reads: V ⋅ cin + mc ⋅ q in = V ⋅ c∞ + mc ⋅ q ∞ Thoughts The total amount of nitrobenzene initially present equals the amount present after equilibrium Solution with q in = 0 and q ∞ = 675 ⋅ c∞ The required ratio is calculated from kg mc cin − c∞ cin − c∞ . q(cin) = 0. = = = 14. 6. Q = 0.20. L = 2.111 – 0)/(cin – 0) = 5.02)/(510·0.111 = 0. c∞ = 10-6 kg m-3.02·(1 + 4550·0.22.111 kg/kg and Δq/Δc (shock wave) = (0. Velocity of the very last trace v c =0 ≈ dq dc ucarrier (1−ε bed )ρ part dq dc c= 0 (Eq.0 m.7) and dq dc = qmb . all concentrations travel through the column. Find Solution a1. the residence time τ = L/v.54 τ = 66898 s (= 18. Eq. Batch adsorption in CISTR cin = 0.8 V q∞ 675 ⋅ c∞ m3 Exercise 6. cout = 0 kg/m3. The amount of carbon per unit volume solution. superficial carrier velocity u = Q / 0.02 kg/m3.6. Lower concentration travel slower than higher concentrations (favorable isotherm).6 m. The amount of waste water to be treated till saturation of the column is the volume flow rate of the waste water times the residence (breakthrough) time τ of nitrobenzene and depends on the velocity v of nitrobenzene through the column. SOLUTIONS TO PROBLEMS 6.Fundamentals of Industrial Separations. with τ from Eq.0531 m/s. the amount of waste water treated until breakthrough and the regeneration time of a saturated column b. 6.3 Given cin = 0.180 = 1003 m3 a3. W kg carbon adsorbent. Alternative calculation: W = 0.01 kg m-3. The total amount of nitrobenzene before equals that after equilibration.02 / 0.4 Given Langmuir adsorption isotherm with qm·b = 510 m3/kg and b = 4550 m3/kg Plug flow in packed column: cin = 0. How much more adsorbent is required in a batch process? Thoughts a.015 m3/s. The amount of waste water treated until saturation of the column follows from volume flow rate and breakthrough time: V = Q· τ. W kg carbon adsorbent. c =0 .015 · 66898 = 1003 m3.7 Exercise 6. All nitrobenzene fed to the column just until break through is adsorbed on the active carbon. The component balance reads V·cin + W·q(0) = V·cout + W·q(cin) or W/V = cin / q(cin) = 0. εbed = 0. ρpart = 800 kg/m3.

the mass balance in words being: in = accumulation + out During saturation no adsorbable material leaves the column. resulting from a very high value of the adsorption constant (steep initial part of adsorption isotherm).2) hence W q* L q* = (1− εbed ) ρ part tsat = s ⋅ ucarrier cf Q cf Exercise 6. which is in equilibrium with the feed concentration.180 = 11. assume plug flow. vc=0 = 3.6 Given L cin R Find =1m = 4 vol% CO2 = 8. For plug flow. The same answer is obtained from Δτ = Wcarbon·q(cin)/ Q ·cin d.31 J/mol K εbed = 0.35·10-3 = 2. This carbon adsorbent is not feasible for regeneration. Nitrobenzene initially present in waste water = nitrobenzene after equilibration: in solution + nitrobenzene adsorbed V·cin = V·c∞ + W·q(c∞) or W/V = (cin – c∞)·(1+b·c∞)/qm·b·c∞ = 1.14 / 0.8 times more then the amount required in a column set-up to treat the same amount of waste water. the time required to saturate a column with c = cf cf Initial condition: c = 0 and q = 0 for 0 ≤ z ≤ L Start from mass balance over entire column. cf = feed concentration. Q = volume flow rate. q* = amount adsorbed in equilibrium with cf. 6.98·10-3/9. The result calculated above is 2. 6.8 ADSORPTION & ION EXCHANGE For the part with c = 0 at the inlet.3) Ws = Vpart·ρpart = Vbed·(1 -εbed)·ρpart and Vbed / Q = L / ucarrier (see section 6.25·10-7 m/s. Hence the resulting amount adsorbed is lower and more adsorbent is necessary to remove the same amount of nitrobenzene as in the continuous process.39 mol m-3 = 4·10-6 m3/s T b ρpart = 20°C = 0. Calculate the desorption time . Ws = weight of adsorbent Thought Solution Saturating a column is a non-stationary process. all other concentrations travel faster.22 c.068 m3/mol = 790 kg/m3 a.40 D qm Q = 5 mm = 1.22). Calculate the breakthrough time with Eq. The total time τ to regenerate the column is L/vc=0 = 6. b1. 6.6. Unlike the adsorbent in the column set-up.14 kg/m3 b2.3. which is much lower. the mass balance reads tsat·Q·cf = Ws·q* + 0 By definition (see Fig. Exercise 6.15·106 s = 71 days: the desorption takes an extremely long period of time. the adsorbent in the batch process is in equilibrium with the final concentration. it takes τ = L/vc=0 to travel to the exit of the column. Explain the rectangular shape of the exit concentration with time b.5 Derive tsat = L ucarrier (1− εbed ) ρ part q* (Eq.

v c =0 v c =cin b.385 mol benzene / kg dry polymer. the shockwave is built up fast.18 ucarrier = superficial velocity = Q /A with A = πD2/4 c. the form of this front remains the same: all concentrations travel with the same velocity because Δq/Δc = (q(cin – 0) / (cin – 0) = constant.33 eq.22 into Wcarbon·q(cin)/ Q ·cin d. higher concentrations (smaller dq/dc) will catch up with lower concentrations (larger dq/dc) until a shock wave has formed. vc=0 = 4. corresponding to 9. τ breakthrough – τ0 = L / vshockwave.1302 kg/mol Msulfonicacid = 0. The total desorption time equals τ ∞ . See part a3 in exercise 6. with vshockwave from Eq. plug flow exists in the entire column. 6. from 0 until cin in say 1 s.21 can be written as Δc 1 πD2 L(1− ε ) ρ bed part Δq W q c =cin − 0 4 = ⋅ ⋅ = ⋅ v CO2 1 ucarrier Δc Q cin − 0 2 πD 4 d.385/1.081 = 0. 6.643 mol m-3.56 mm s-1 it follows that z = 2. Langmuir-type is a favorable adsorption isotherm b.0811 kg/mol The ion-exchange capacity of a resin with the highest possible sulfon-group content group.760 kg sulfon-groups.22.104 + 0.760 kg resin.51 mm s-1 and vc=cin = 5. would overtake the lowest concentration. 6. starting from sulfon-free polymer. plug flow occurs Bonus: the time required to transform an inlet profile into a shock wave usually is relatively short. see part a3 of exercise 6.4 Solution a. With cin = 1. From that moment on.7 Given Find Mstyrene = 0. 6. At a certain distance z from the inlet. The weight after sulfonation is 1.140/1. If the feed enters as plug flow.4 mm z z = 1+ .104 kg/mol Mdivinylbenzene = 0. Complete saturation with sulforic acid requires that amount of moles.4.8 s. If any other concentration profile enters the column.τ1 = L / vc=0 = 222 s.3 s. c.000 + 0. In Eq. Neglecting the accumulation of CO2 in the gas phase between the particles. . Exercise 6. Thus. This takes time τ: τ= and τ = 5.130 = 9.12/0.Fundamentals of Industrial Separations.760 = 5. These values are small compared to L = 1000 mm and residence time L/vc=0 = 222 s. per unit weight of dry resin. SOLUTIONS TO PROBLEMS 6. Eq. except for the small entrance effect.88/0. This amount contains 9. which entered 1 s after the lowest concentration.760 = 1.385 mol of groups available for ion-exchange or 9. Imagine a linear rise in inlet concentration. the feed concentration Cin.64 mol m-3 (ideal gas law) and Δq/Δc = (q(cin) – 0) / (cin – 0) = 0.64 τ breakthrough – τ0 = L / vshockwave = 1 / 5·10-3 = 199.385·0. Try to convert Eq. meaning εbed << (1− εbed ) ρ p L Δq . cin = 1.9 Thoughts a. Express the result on a weight-basis: kg dry ion-exchange resin (polymer plus sulfon groups) Thoughts Calculate the number of moles sulforic acid required to provide every aromatic ring with a sulfon Solution Benzene in 1 kg dry polymer before sulfonation: 0.

Three operating lines are drawn. defined by the top of the extraction column where the fresh.rl ) c c 2400 ⋅ K ⋅ cM. The equilibrium diagrams for extraction and regeneration b. a. b.s cM. for the regeneration: ⋅c ⋅ (3000 − cM.exit = 1 mol m-3.l ) c 2400 ⋅ K ⋅ cM. in the regenerated ion-exchange resin these concentrations are cNa. The minimum amount of ion-exchange resin per unit volume feed c-e.l = cM.8 Given Feed L = 0. The maximum slope is L/Vmin = (2000 – 200) / (15 – 1) = 128.3 it follows that Vmin = 0.6 = 2. with L = 0. all going through the point.s = cM.6.s ) 30 + (K − 1) ⋅ cM.s Na. Find Thoughts a. since each M+-ion exchanges with one Na+-ion.sf = 200 + 2200 = 2400 mol m-3 ⋅c ⋅ (30 − cM.f = 30 mol m-3 cM.rlf = 0. and cM. regenerated resin is fed and the purified solution is withdrawn. The stream of ion-exchange resin (V in m3 s-1) and regeneration liquid (L in m3 s-1) are chosen as 1.rl K = M. M+ in solid mol m-3 resin 2500 2000 1500 1000 500 0 0 5 10 15 20 + -3 M in liquid / mol m 0 500 M+ 1000 1500 2000 -3 in regeneration liquid / mol m M+ in solid mol m-3 resin 2500 2000 1500 1000 500 0 b. The maximum slope of the operating line is given by a second point.sf = 200 mol m-3.s Na.s ) 30 + (K − 1) ⋅ cM.6.3/128. The initial sodium concentration in the regeneration liquid cNa. cM.f = 15 mol m-3 and cNa. cM.2 times the minimum values.rl ⋅ cNa.lr ⋅ (2400 − cM.10 ADSORPTION & ION EXCHANGE Exercise 6. Note that the sum of the ion concentrations in the liquid (and in the solid as well) is constant. The ion-exchange equilibrium constant K = 5.s cM.f = 15 mol m-3.sf = 2200 mol m-3 and cM.s and that in the aqueous phase.s + cNa.l Similarly.s = 5.f + cNa. cM. the point on the equilibrium line at the concentration of the metal in the feed.l = M.s = K = M. L/V.rl = M. respectively.l + cNa. Equilibrium diagram for extraction cM.333·10-3 m3 s-1. the required exit concentration cM. cM. Various process conditions The definition equation of the ion-exchange equilibrium contains both the concentration of the metal M in the ion-exchange resin.l. Solution a. .rl Both equilibrium equations are plotted in the two graphs below.l ⋅ cNa.sf + cNa. at 15 mol m-3.rlf = 3000 mol m-3.s = cM.l c = 5. the amount of resin per unit time follows from the slope of the operating line. Given the feed flow L.s cM.3 m3 s-1 with cM.l ⋅ (2400 − cM.

SOLUTIONS TO PROBLEMS 6.Fundamentals of Industrial Separations.11 M+ in solid resin mol m -3 M+ in solid resin mol m -3 2500 2000 1500 1000 500 maximum slope loaded resin out 2500 2000 1500 1000 500 maximum slope loaded resin out regenerated resin in 0 0 M+ out M+ in regenerated resin in 0 0 M+ out M+ in 5 10 15 20 M+ in liquid / mol m-3 5 10 15 20 M+ in liquid / mol m-3 .

6.12 ADSORPTION & ION EXCHANGE .

010 kg H2O/kg dry air. Calculate the total amount of water evaporating per unit time.Fundamentals of Industrial Separations.2 kg s-1.1 Chapter 7: Exercise 7.5 m.4 Water is dispersed in droplets of 0.121 The process is conducted in a packed bed with a length of 4 m and diameter of 0. To what temperature should the air be heated at least to avoid that the pores remain filled with 1 water? Exercise 7. At the start of the drying process the water vapor pressure increases linearly until the maximum value of 75% relative humidity is reached.073 N m-1. A laboratory experiment shows that the critical moisture content wc = 0. Calculate the relative change in saturation vapor pressure Exercise 7. The heated air flows along a flat tray filled with completely wetted material. 1 Hint: the saturated vapor pressure obeys Clapeyron . The heat of evaporation ΔHv = 44045 J mol-1.8 nm.3 (ρv)0.2 kg kg-1 dry and the constant drying rate rc = 0. Exercise 7. The surface area available for heat exchange with air is 0. wet surface of the solid at a velocity v = 5 m s-1.5 Air at 20°C and 1 bar with a relative humidity of 80% is available for drying a porous solid containing cylindrical pores with a diameter of 0. T = 300K and γw = 0.350 and K(60°C) = 0.2 kg kg-1 dry under similar conditions.36 g s-1 m-2.45 106 J kg-1. The air flows parallel to the flat.8.1 DRYING OF SOLIDS Air of 20°C and 1 bar with a relative humidity of 80% is heated to 50°C.1 mm radius. Drying is achieved by adsorption of water on porous alumina. The adsorption isotherms are given in the form of Henry’s law: kg water adsorbed = K × Hrel kg dry alumina with K(30°C) = 0.25 m2 and the heat of evaporation ΔHv = 2. How long will that take? Exercise 7. where ρ is the density of the moist air in kg moist air per unit volume moist air.6 Wet air of 30°C and 2 bar with a relative humidity (Hrel = pwater/p0water) of 75% has to be dried at a rate of 0. the constant drying rate. Regeneration takes place at 60°C.3 A wet solid is dried with air at 60°C and a humidity Hf = 0. Under these conditions the heat transfer coefficient h is given by h = 14. The moisture content of 2 kg of the solid (dry basis) is reduced from 0. The heat transfer coefficient h = 35 W/m2K and the heat of evaporation ΔHv = 2. Exercise 7.2 A wet solid with a moisture content w = 0.1 m2 on a flat tray. Calculate rc. SOLUTIONS TO PROBLEMS 7.4 to 0.5 kg kg-1 dry occupies 0.45 106 J kg-1.

7- 2

DRYING OF SOLIDS

The bed porosity εbed = 0.32 for a complete filling with the alumina particles of 2 mm diameter. The particle porosity εpart = 0.58. Furthermore it is given that the saturated vapor pressure of water, p0water equals 0.0418 bar at 30°C and 0.199 bar at 60°C. Mwater = 0.018 kg/mol and Mair = 0.029 kg/mol. a. b. Calculate the maximum kilograms of dry alumina the adsorption vessel can contain. When the first trace of water is detected at the column exit, only 70% of the column is saturated with water. Draw the concentration profile in the adsorption vessel (relative humidity as function of the place). How long did it take the first trace of water to exit the column? Calculate the total amount of water at breakthrough. How long does it take to completely regenerate the column by heating the inlet air to 60°C and reducing the pressure to 1 bar.

c. d. e.

Fundamentals of Industrial Separations, SOLUTIONS TO PROBLEMS

7- 3

SOLUTIONS Exercise 7.1 Given Find Hr = 80% ΔHv = 2.45 106 J/kg rC, the constant drying rate Tfeed h = 50°C = 35 W/m2K

Thoughts Eq. 7.20b seems to be the appropriate equation to apply. This equation requires the calculation of
the wet-bulb temperature Twb. Increasing the temperature from 20 to 80°C does only change the saturation pressure of water, not the partial pressure of water vapor. Note: the heat of evaporation is given as J/kg.

Solution The humidity is constant, the relative humidity decreases. Use the psychrometric chart (Fig. 7.3), draw a horizontal line (starting from the intersection of the curve representing 80% relative humidity and the vertical line at 20°C, see psychrometric chart below) to the point where T = 50°C. Now draw a straight line, starting from that point and parallel to the adiabatic cooling lines, to the saturation line (100%). Read the wet-bulb temperature: Twb = 26°C. Apply Eq. 7.20b: kg 35 × (50 − 26) rC = = 3.43 10−4 6 s m2 2.45 10

Temperature /

C

Humidity, kg moisture/kg dry air

7- 4

DRYING OF SOLIDS

Exercise 7.2 Given rC XC A

= 3.6 10-4 kg / m2s = 0.2 kg / kg dry (critical moisture content) = 0.1 m2

W X0

= 2 kg dry solid = 0.5 kg / kg dry

Find

tC, drying time to reduce the moisture content from 0.4 to 0.2 kg / kg dry.
period A’B in Figs. 7.7 and 7.8, where surface temperature and rate of evaporation are adjusting to reach the stationary state, is (probably) excluded.

Thoughts Eq. 7.23 is applicable. Timing starts at X = 0.4 whereas X0 = 0.5 kg / kg dry, so the initial drying

Solution

tC =

2 0.1× 0.36 10−3

(0.4 − 0.2) = 11111s = 3.09 h

Exercise 7.3 Given Tfeed = 60°C Ptot = 1.01325 105 Pa Mw = 0.018 kg/mol Hf = 0.010 kg / kg dry ΔHv = 2.45 106 J/kg

h A Mair v

= 14.3 (ρv)0.8 W/m2K = 0.25 m2 = 0.029 kg/mol = 5.0 m/s

Find

the total amount of water evaporating per unit time
the air speed v and density of moist air ρ. The latter is found from the weight of moist air and the total volume occupied by that amount. It is convenient to start from 1 kg dry air, then calculate the weight of moisture in that amount of air, and finally calculate the volume of air and moisture, assuming the ideal gas law to hold.

Thoughts This is similar to exercise 7.1, except that the heat transfer coefficient h has to be calculated from

Solution

The volume of dry gas Vair =

R.Tf 8.31× 333 m3 = = 0.942 , M air .Ptot 0.029 × 101325 kg dry air

the volume of water vapor therein Vw = Hf

R.Tf m3 . = 0.015 M w.Ptot kgdry air

ρmoistair =

1+ Hf 1.010 kg = = 1.055 Vair + Vw 0.9569 m3

. m2K The wet bulb temperature, determined similarly as in exercise 7.1 amounts to 29°C. kg h.(Tf − Twb ) 54.1× 31 The resulting drying rate is calculated to A. = 0.25 × = 1.7110−4 6 ΔH v s 2.45 10
Exercise 7.4 Given r droplet = 0.1 μm R = 8.31 J/mol.K ρw = 1000 kg/m3

h = 14.3 × (1.055 × 5.0)0.8 = 54.1

W

γw
T Mw

= 0.073 N/m = 300K = 18 10-3 kg/mol

Find

relative change in saturation pressure of water droplets at 300K
Note the difference between Eq. 7.17a and Eq. 7.17b. The molar volume Vm of water is calculated from its density and molecular weight.

Thoughts Eq. 7.17a is applicable. Droplets are spherical so r1 = r2 = r droplet.

Solution

psat
∞ psat

= exp(

2 × 0.073 10
−7

×

0.018 1 × ) = 1.0107 1000 8.31× 300

5 m εpart = 0. LUB-part) use Eq.exp(− ΔHvap R.Fundamentals of Industrial Separations. pw.018 kg mol-1 Tf K30 D = 30°C = 0. c. because the slope of the adsorption isotherm is constant.073 N/m Find the lowest temperature to evaporate the liquid water from the pores Thoughts The vapor pressure of water.31 J/mol.26 with dq/dc = K60 2 N. 7.350 = 0. Unlike pw. pw = 0. the saturation pressure of water increases exponentially with temperature.0418 bar pw Mair = 0.19: pw 0 psat (T ) = 0. independent of T. e. 0 psat (293) Increasing the temperature increases the saturation pressure of water. the weight of adsorbent in column The concentration profile at the time of breakthrough the adsorption time till breakthrough the total amount of water adsorbed at breakthrough the time required to regenerate the column at 60°C Thoughts a. at a temperature just slightly higher than 60°C the 2 pores will empty .5 Exercise 7.3 shows the key how to calculate the amount of adsorbent to be contained in the vessel.K =4m = 0.8 × exp(−ΔHvap / R. will remain . Further. A very thin water film at the pore surface. Exercise 7.K = 44045 J/mol = 18 10-3 kg/mol Hr T ρw γw = 80% = 293K = 1000 kg/m3 = 0. b. d.exp(− psat ΔHvap RT 0 ) but also psat (293) = C.029 kg mol-1 Pf K60 = 2 bar = 0. Eq. of the moist air is given through the relative humidity.B. The humidity should be sufficiently low (the temperature sufficiently high) that Eq.293 ).8 * psat (293) Solution The highest temperature at which the liquid water is in equilibrium with the vapor pressure in the feed gas follows from Eq.5: pw Hr = ⋅ 100 . Fig.32 = 75% = 0.58 0 (30) = 0. 6. e.293) exp(−ΔHvap / R.2K. c All concentrations travel with the same speed through the column. b. SOLUTIONS TO PROBLEMS 7.20 kg s-1 = 8.5 Given r R ΔHvap Mw = 0. Thus. 0 where C is some constant. According to the Clapeyron-equation: 0 (T ) = C. which does not change with temperature. 7. in equilibrium with pw at that temperature. thus decreasing the relative humidity.T ) = exp(− 2γ Vm × ).4 nm = 8. 6.T Solving for T gives T = 333.6 Given Φair R L εbed Hrel Mw = 0. r R. d.199 bar pw Find a.19 is obeyed.31 J/mol. 7.121 ρs = 3500 kg m-3 dp = 2 mm 0 (60) = 0. apply adsorption isotherm to the two sections (saturated.

714) ⋅ 3500 ⋅ 11. 1− εtot = (1− εbed ) ⋅ (1− ε part ) → εtot = 1− (1− 0.30·Walumina·K30·Hrel)/2 = 175 kg water . 70% with equilibrium load 30% with half load on average Total water load = 0.7.254 = 2.205 ⋅ 10−5 m / s (1− 0.224 m3 4 Walu mina = 3500 ⋅ 0.4 h tbreakthrough = d.6 Walu mina = ρs ⋅Valu mina with Valu mina = Vvessel ⋅ (1− εtot ) DRYING OF SOLIDS Solution a.205 ⋅ 10−5 = 181422 s = 50.224 = 785.714) = 0.32) ⋅ (1− 0. concentration in gas fase length c.1 kg π b.5 m3 / kg Mw p0 dcw w v water = 0.0106 Pf dq w K RT = K ' with K ' = ⋅ = 11.254 m / s (superficial velocity) M air Pf π 2 D 4 p0 y w = w ⋅ Hrel = 0.58) = 0.5 4 2. v water = velocity water v air (1− εtot ) ⋅ ρs ⋅ dq w dcw v air = (1− y w )Φ air RTf 1 ⋅ ⋅ = 0.714 Valu mina = ⋅ 0.52 ⋅ 4 ⋅ (1− 0.70·Walumina·K30·Hrel + (0. tbreakthrough = length .

SOLUTIONS TO PROBLEMS 7.279 m/s (superficial velocity) (1− εtot ) ⋅ ρs ⋅ K60 ′ M air Pf π 2 D 4 RT K 0.935 w tbreakthrough = 4 2.935 m3 /kg and v water = = 2.7h .279 reg K60 ′ = ⋅ = 0. v water = RTreg (1− y w )Φ air v air with v air = ⋅ = 0.Fundamentals of Industrial Separations.99 ⋅ 10−4 = 13403s ≈ 3.714) ⋅ 3500 ⋅ 0.7 e.99 ⋅ 10−3 m/s Mw p0 (1− 0.

7.8 DRYING OF SOLIDS .

62 (kg anhydrous salt/kg water) Exercise 8. isothermal evaporation of 25% of the free water isothermal evaporation of 25% of the original water cooling to 10°C and assuming 2% of the original water lost by evaporation.082 kg/mol). XC = 0.5 Calculate the maximum (theoretical) yield of pure crystals that could be obtained from a saturated solution of sodium sulfate (Manh = 0. NaC2H3O2 (MW = 0. How many kg/h of crystals can be collected theoretically? Temperature: Solubility: Exercise 8. from a saturated aqueous solution.142 kg/mol) with 0. Initially 100 kg of water is present. A saturated sugar solution at 80 °C has half of its water evaporated and the solution is then cooled to 20 °C. The solution is cooled to 10°C and 38 kg/h of water is evaporated in the process. a. Temperature: 20°C 80°C Solubility: 2.5H2O by combined evaporative/cooling crystallization.3 A cooling crystallizer is used to crystallize sodium acetate. b.25 kg anhydrous salt/kg free water by a. Calculate the maximum production rate of crystals Calculate the maximum yield in kg crystals per unit weight of solute fed Exercise 8.090kg anhydrous salt / kg solute-free solvent adding 0.04 3.4 Copper sulfate is crystallized as CuSO4. SOLUTIONS TO PROBLEMS 8-1 Chapter 8: CRYSTALLIZATION & PRECIPITATION Exercise 8. b.068kg Na2SO4·10aq / kg solute-free solvent 10°C 17. e.363 10 0. b.030kg anhydrous salt / kg solute-free solvent adding 0. XC = 0. If the anhydrous salt is dissolved in 100 kg of water/h. A saturated sugar solution is cooled from 80 °C to 20 °C. how many kg of crystals/h are collected? Temperature: Solubility: Exercise 8. c.545 40 0. 1000 kg/h of water is mixed with 280 kg/h of anhydrous copper sulfate (MW = 0.160 kg/mol) at 40°C.465 30 0. XC = 0.75 kg ethanol / kg free water. The feed rate is 5000 kg solution / h.2 A solution of 80 wt% of naphthalene in benzene is cooled to 30°C to precipitate naphthalene crystals.408 20 0.4 40°C 28.1 Determine the maximum yield of anhydrous sugar crystals deposited at equilibrium in the following situations.Fundamentals of Industrial Separations.39 (°C) (kg anhydrous salt/kg water) .5 (g anhydrous salt/100 g water) 0 0. d. The solubility of naphthalene at 30°C is 45 wt% in solution. The feed is initially saturated at 40°C while the crystallizer is cooled to 0°C until equilibrium conditions are established.655 60 1. The stable form of the crystals is a hydrate with 3 moles of water. a.75 kg ethanol / kg free water.

01 0. Calculate the population density distribution of the product crystals at mean size L over a size interval ΔL Determine the growth and nucleation rate graphically from the population density plot on a semilog scale.0 90 99 0. determine ΔE.174 kg/mol.9 18.16 is applicable with an apparent interfacial surface tension γ of 2·10-3 Pa. Exercise 8.6 Assuming that G∝Δc.7 1. Eq.6 . b. Weight on the sieve (g/kg of water) 2.7 3. supersaturation being achieved by cooling.s and a pre-exponential coefficient A = 1025. Assume that the crystal density is 1770 kg/m3 and the volume shape factor is 0. Note: c* depends on T and ammonium sulfate crystallizes as an anhydrate Given Temperature: 30 Solubility: 78 s: 0.3 20.7 Estimate the supersaturation s of an aqueous solution of K2SO4 at 30°C required to get a heterogeneous nucleation rate of 1 nucleus per second.8 Potash alum was crystallized from its aqueous solution in a laboratory scale continuous MSMPR crystallizer of 10 l capacity at steady state.0 10.05 G: 5.47.0 60 88 0.5 0. 8.9 28. The size analysis of the produced crystals resulting from a steady-state sample taken from the crystallizer operated at means residence time of 900 s.6 o C g anhydrous salt/100 g water 10-7 m/s Exercise 8.3 16.8-2 CRYSTALLIZATION & PRECIPITATION Exercise 8. its molecular weight 0. If it is valid.05 8. The density of the K2SO4 crystals is 2662 kg/m3. determine whether or not the Arrhenius equation is valid for (NH4)2SO4 crystallization. is given in the table below. Sieve Analysis Data: Standard sieve Size (μm) 850 710 500 355 250 180 125 90 63 45 The steps to be taken are: a.

Use a basis of 100 kg of entering water to which 0.10 Design a crystallizer to produce potassium sulfate crystals assuming an MSMPR unit operating continuously at steady state.100 kg/kg water = 2660 kg/m3 = 0. what linear growth rate G is required? Temperature: 10 Solubility: 40. What is the mean size of the product crystals Lp? If the residence time is 21 hours.9 A sodium acetate crystallizer receives a saturated solution at 60°C.Fundamentals of Industrial Separations. b.525 = 0. a.25 kg seeds is added.2 mm average size crystals and cooled to 10°C. SOLUTIONS TO PROBLEMS 8-3 Exercise 8.1167 kg/kg water = 1090 kg/m3 ρc kv Cout ρsoln .8 60 139 (°C) (g anhydrous salt/100 g water) Exercise 8. This solution is seeded with 0. The following specifications and data are available: relative nucleation kinetics: production rate: product dominant size: magma concentration: crystal density: shape factors: outlet concentration density of product solution B P LD MT = 1×1019 MT G2 (no/s kg water) = 1000 kg/h = 490 μm = 0. The sodium acetate crystallizes as the trihydrate.

maximum production rate b.62 and XC = 2. Solving for C gives C / F’ = XF – XC = 1. the yield of sugar crystals when a saturated solution is cooled from 80oC to 20oC. Solution a.60 kg anhydrous sugar crystals / kg water fed. sugar crystals produced C = = 0.795 1 Note that here S means solvent. naphthalene balance: naphthalene in = crystals produced + naphthalene in solution or XF·F = C + XC·S benzene balance: (1 – XF)·F = (1 – XC)·S both F and S refer to solution (solvent + solute): XF = 0. Solution a. not concentration. Thoughts The problem is easily solved by applying Eq. respectively Thoughts Derive the naphthalene and benzene balances.8-4 CRYSTALLIZATION & PRECIPITATION SOLUTIONS Exercise 8. when hydrates are involved). sugar balance: XF·F’ = C + XC·S’ water balance: water in feed = water evaporated + water in solution or F’ = 0. C = 0. XF = 3.6 and 8.45 kg/kg solution. not solid. sugar balance: sugar in = crystals produced + sugar in solution 1 or XF·F’ = C + XC·S’ water balance: F’ = S’ where F’ and S’ = solute-free solvent per unit time.58 kg anhydrous sugar / kg water fed.04 80oC 3.718 The maximum yield = XF ⋅F′ Exercise 8. A more versatile approach (which will also work in more complex situations. maximum yield (kg crystals / unit weight of solute fed) Note that now XF and XC are weight fractions of the total feed and total solution. and C means solid crystals.5·F’ + S’ Solving for C gives C / F’ = XF – 0. Base calculations on anhydrous sugar. The solubility data suggest to work on a solute-free basis.436 The maximum yield = sugar in feed XF ⋅F′ b.5·XC = 2.62 (kg anhydrous sugar/kg water) a. 8. b.2 Given Find F = 5000 kg/h. the yield of sugar crystals when a saturated solution is cooled from 80oC to 20oC and half of its water is evaporated.5.80 and XC = 0.1 Given Find Temperature: 20oC Solubility: 2.7). 8.8 with ϕE = 0 and ϕE = 0. e. XF = 80 wt% naphthalene and XC (30°C) = 45 wt% in solution a.04 kg anhydrous sugar / kg water. would be to derive both the water and the sugar balance (Eqs. Solving for C gives C = 3182 kg crystals / h b.g. respectively. The (maximum) yield = crystals produced (loss free) / naphtalene fed = C / XF·F = 0. .

(280 kg CuSO4.465 0. Solving for C gives C = 124.363 kg anhydrous acetate / kg water.655 and XC = 0.0aq/h + 1000 kg H2O/h → 28.6 kg / h. The product stream in kg crystals.4 kg crystals (waterfree basis) / h.5aq / h = C·(M5aq + Manh)/Manh = 195.090 kg mol-1 The stable form of copper sulfated crystals is a hydrate with 5 moles of water Temperature: Solubility: Find 10oC 17.6 & 8.018 = 0.408 0.1) Solution water balance: F’ = C·M3aq/MAc + S’ acetate balance (anhydrous): XF·F’ = C + XC·S’ where C = kg acetaat.082 kg mol-1 Tf = 40oC Tp = 0oC M3aq = 3 · 0.160 kg mol-1 M5aq = 5 · 0.545 0.0 kg / h.8 kg crystals (waterfree basis) / h.054 kg mol-1 The stable form of sodium acetate crystals is a hydrate with 3 moles of water.5 g anhydrous salt/100 g water The product flow of crystals collected.018 = 0. Thoughts Derive the water and acetate balances on a solute-free basis (see exercise 8.3aq / h = C·(M3aq + MAc)/MAc = 63.Fundamentals of Industrial Separations. Check that the feed concentration at 40°C is just below the saturation value. Solving for C gives C = 38.174 kg anhydrous sulfate / kg water. 8. XC = 0.3 Given F’ = 100 kg water/h MAc = 0.4 Given F’ = 1000 kg water/h CuSO4.0aq / h (note that the actual product carries 3 aq / mol salt) XF = 0. Exercise 8.7) Solution water balance: F’ = V +C·M5aq/Manh + S’ sulfate balance (anhydrous): 280 = C + XC·S’ where C = kg anhydrous sulfate / h. Temperature: 0 10 20 30 40 60 oC Solubility: 0.4 40oC 28.39 kg anhydrous salt/kg water Find The product flow of crystals that are collected after cooling to 0oC. Thoughts Derive the sulfate and water balances (see Eqs.363 0. SOLUTIONS TO PROBLEMS 8-5 Exercise 8. The product stream in kg crystals.655 1.0 g CuSO4/100 g H2O) .0aq = 280 kg/h Tf = 40oC V = 38 kg water evaporated/h Tp = 10oC Manh = 0.

Therefore. Hence.018 kg mol-1.268 and with the salt balance as in previous part XF·F” = C + XF·S” C = 0.068 kg hydrated salt/kg solute-free solvent after adding that much of ethanol crystallizer and the amount left in the saturated solution after precipitation. while XC is expressed per kg of solute-free solvent. XC = 0. The stable form of sodium sulfate crystals is a hydrate with 10 moles of water. Mw = 0.0aq or F” + XF·F”·1.75 kg ethanol / kg free water. cooling to 10 oC and assuming 2 % of original water lost by evaporation.268 = 0. Salt balance: XF·F” = C + XF·S” where C = kg crystals(anh) precipitated and S” = kg free water (both per unit time). in addition to F’ and S’ (solute-free solvent per unit time. b.25 The X F F ′′ .268) + C·1.268 kg water per unit time and the M anh total amount of water fed equals 1. at 10oC XC = 0.09 kg anhydrous salt/kg solute-free solvent d.142 kg crystals.25·F” + C·1. 8. it is convenient to introduce F” and S” in kg free water per unit time.268 + S” + XF·S”·1.317·F”. XC = 0. Note that bound water is the part of the solvent required to crystallize all of the solute.268 kg water / kg salt. Thoughts The weight of crystals precipitated is calculated from the difference between the amount fed to the Solution The feed to the crystallizer amounts to F” kg of free water per unit time.10aq / kg free water fed.25 kg anhydrous water/kg free water.268 = 0. Bounded water M aq ⋅ 10 = 1.0aq.4).75 kg ethanol / kg free water.8-6 CRYSTALLIZATION & PRECIPITATION Exercise 8. Find Calculate the maximal (theoretical) yield of crystals from a saturated aqueous solution of sodium sulfate by: a. Isothermal evaporation of 25% of the original water c.268 + S” + XF·S”·1.268 = 0. the remainder is free water.0aq Out per unit time = evaporated + water in precipitated crystals + free water in solution + water in solution bounded to XF·S” = XF·F” – C kg salt. The water balance now reads F” + XF·F”·1. adding 0. Water balance: In per unit time = free water + water bounded to XF·F” kg salt. see Eq. Manh = 0.6.030 kg anhydrous salt/kg solute-free solvent after adding that much of ethanol e.142 kg mol-1.25·( F” + XF·F”·1. this feed contains XF·F” amounts to M salt M w ⋅ naq anhydrous salt binding X F ⋅ F ′′ ⋅ = X F ⋅ F ′ ⋅ 1. 8. Then. Note also that in this exercise.5 Given XF = 0. a. isothermal evaporation of 25 % of the free water b.268 Solving these two equations for C gives the maximum theoretical yield = product stream of hydrated crystals amounts to C + C*1. adding 0. can solve this problem. similar to the overall balance in Eq. deriving the appropriate mass-balances. XF is expressed per unit weight of free water. naq = 10.

268 + S’ Solving for C gives Yield = C = 0.10aq / kg free water fed.Fundamentals of Industrial Separations. d.343 kg crystals.75 kg ethanol/kg free water decreases the solubility of the sulfate to XC = 0.268 + S’ Solving for C and conversion to hydrated crystals per unit weight of free water fed gives exactly the same result as in part d.268 + 0. Addition of 0.030 kg salt (anh) / kg solute-free solution (water + ethanol).187 kg crystals.268 = 0. Because XC is expressed per unit weight of solute-free solvent.75·F” = C·1. Expressing the solubility in kg hydrated crystals / kg solute-free solution changes the anhydrous salt balance.782 X F F ′′ and the product stream of hydrated crystals amounts to 2.75·F” = C·1. the anhydride balance now reads: XF·F” = C + XC·S’ where S’ = total water in solution (solute-free base) per unit time.02·( F” + XF·F”·1.268) + C·1. e. .268·C = 0.268 + S’ The salt balance is the same as in part c: XF·F” = C + XC·S’ Solving for C gives Yield = C = 0. The solvent balance (water + ethanol) now reads F” + XF·F”·1.329 X F F ′′ and the product stream of hydrated crystals amounts to C·2.268·C = 0.018 The solvent (water + ethanol) balance is the same as given in part d: kg solvent/unit time: F” + XF·F”·1.142 0.10aq / kg free water fed.604 X F F ′′ and the product stream of hydrated crystals amounts to 2. the amount of hydrated salt in solution has to be converted to an anhydrous basis: kg anhydrous salt/unit time: X F ⋅ F ′′ = C + X C ⋅ S′ ⋅ 0.443 kg crystals.10aq / kg free water fed.268 + 0. Water balance: F” + XF·F”·1.268 = 0. SOLUTIONS TO PROBLEMS 8-7 C (and S”) is solved giving Yield = C = 0.142 + 10 ⋅ 0. c.

8.23 kJ/mol . Note that the exponential factor n is unknown beforehand and should be determined by trial and error.01 0.8. Thoughts If the Arrhenius equation is valid (Eq. if so.29 and elimination of c*.8-8 CRYSTALLIZATION & PRECIPITATION Exercise 8.05 G: 5. 8. Assuming G ∝ Δc. 8. a plot of ln(kG) against 1/T will result in a straight line. Solution a.29 the following expression for kG is derived: ⎫ ⎪ n Eq.6 Given Temperature: 30 Solubility: 78 s (Eq.13. Taking n = 1 (+ in graph below) does not give a straight line when ln(kG) is plotted as a function of 1/T Taking n = 2 (o in graph below) a linear dependence is obtained → ΔE = 8.05 8.27). 8.27 kG = kG exp⎢ ⎝ s + 1⎠ ⎥⎪ ⎣ RT ⎦⎭ b. From Eqs.13): 0. determine whether or not the Arrhenius equation is valid b. 8. determine ΔE.0 90 99 0. an expression for kG can be found by rewriting Eq.0 60 88 0.27 and 8.8.29 G = kG (c − c *) ⎪ ⎡ − ΔE ⎤ ⎪ c −c * G o Eq.6 o C g anhydrous salt/100 g water 10-7 m/s ammonium sulfate crystallizes as anhydrate Find a.8.13 s = = kG exp⎢ ⎬ kG = ⎥ n c* ⎣ RT ⎦ ⎪ ⎛ c ⎞ ⎡ − ΔE ⎤⎪ ⎜c − ⎟ o Eq.

16E+07 4.5 54 ΔL [μm] 140 210 145 105 70 55 35 27 18 W [g/kg] 2. SOLUTIONS TO PROBLEMS 8-9 Exercise 8.47 ρc = 1770 kg/m3 The sieve analysis data is given in the shaded columns below .sieve size and W (the weight on the sieve). 8.00645 Note that at slightly higher values of s.3 20.54396 19.21E+08 2.37. the population density distribution over a size interval ΔL b.11E+10 6.02E+11 1.35109 25.26243 .16 is applicable. Thoughts The population density n.16054 24. On dissociation K2SO4 gives 2K+ and 1SO42.16).3 16. giving s = 0.9 18 10. The population density is given by (Eqs.91199 25.85895 21. 2 ⋅γ 3 16π ⋅ v m Solution Solve 1 = 1025 ⋅ exp(− 3 ⋅ 32 ⋅ (k ⋅ 303)3 ⋅ s 2 ) for s.7 3.20E+10 3.5 0. Find a.5 76.5 302.54E+11 ln(n) 17.hence ν = 3.5 215 152. Exercise 8.51973 23.31 and 8.72833 26./m kg 4. Solution a. is defined as the number of crystals (ΔN) in the size range of L to L+ΔL.20421 24.49E+11 2.9 28.s = 6.22E+09 1.7 1.02·1023 = R / Nav T ρsalt Msalt = 30oC = 2662 kg/m3 = 0.59E+10 1. 8.32): ΔN W n= = ΔL k v ρ c L3 ΔL Population densities n calculated as a function of average crystal sizes L: Sieve size [μm] 850 710 500 355 250 180 125 90 63 45 L [μm] 780 605 427.7 Given γ Nav k = 2·10-3 Pa.6 n no. molecular volume vm = Msalt/ρsalt·Nav Thoughts Eq.Fundamentals of Industrial Separations. Bo is increasing tremendously.8 Given MSMPR crystallizer V = 10 l τ = 900 s kv = 0. taking A ≈ 1025 nuclei / s cm3 (see text on top of page 8. the growth and nucleation rate graphically The nucleation and growth rate can then be found by a plot of ln(n) against L to give a straight line according to Eq. 8.174 kg/mol Find the value of supersaturation s to give a nucleation rate of 1 nucleus / s.5 107.

The total mass Seed ∝ n ⋅ kv ⋅ ρ ⋅ L3 seed where n = total number of seed crystals.693 2 R = 0.8 60 139 C g anhydrous salt/100 g water a.998 G = 1 / 0. 8.9 Given F’ = 100 kg Seed = 0. Thoughts a.0117x + 26.91⋅1011⋅0. the mean size of the product crystals. see graph below. the simple ΔL-law of Eq.37 and 8. or 3M water 3M water = L+P ⋅ F ′ + Seed ⋅ M anh.693. 8. Mass balance over water in the system: Water fed (F’) + crystal water in seed crystals = water in saturated solution (L) + crystal water in product crystals (P).26 applies: ΔG = ΔL / Δt Solution a. Combine Eqs.salt + 3M water .23a). Analogously for the total mass of product crystals: P ∝ n ⋅ kv ⋅ ρ ⋅ L3 product Hence find the ratio P / Seed from appropriate mass balances.095⋅10-6 = 3.salt + 3M water M anh. Exercise 8.082 kg/mol The stable form of sodium acetate crystals is a hydrate with 3 moles of water Temperature: Solubility: Find 10 40.25 kg (in the form of trihydrate) Lseed = 0.2 mm o = 60oC TF TP = 10oC MNaAc = 0.0117⋅900 = 0. When the linear growth rate is independent of crystal size and at constant supersaturation. b. The mass of a crystal is proportional to L3 crystal (Eq. b. 8.38 to give: n = ⎡ −L ⎤ B0 exp⎢ ⎥ ⇒ G ⎣ Gτ ⎦ ⎡ 0⎤ L B ln(n) = ln⎢ ⎥ − G τ G ⎢ ⎣ ⎥ ⎦ Plotting of ln(n) against L gives a straight line with slope of 1/Gτ = 0.0117 and intercept ln(Bo/G) = 26. as τ = 900 seconds: and 30 25 20 ln(n) 15 10 5 0 0 100 200 300 400 L 500 600 700 800 900 y = -0. the required linear growth rate G if the residence time is 21 hrs.8-10 CRYSTALLIZATION & PRECIPITATION b.095 μm/s B 0= 3.72*104 no/s kg. Thus.

02 m3. 8.19) = 1000 kg crystals/h = 490 μm = 0. 8. 8.78 kg water/s.Fundamentals of Industrial Separations. Eq.056 ton water. Production rate P and residence time τ determine the capacity of the crystallizer.082 mm/h G= Δτ Δτ 21 Exercise 8. 8.1167 kg/kg water = 1090 kg/m3 Design Thoughts Designing a crystallizer means to estimate the residence time τ of the magma (solid – saturated mixture).10 Given nucleation kinetics: production rate: product dominant size: magma concentration: crystal density: shape factors: outlet concentration density of product solution an MSMPR crystallizer B0 P LD MT ρc kv Cout ρsoln = 1×1019 MT G2 (no/s kg water) (see Eq.2 = = = 0.19 and the crystal growth rate G with Eq.40. 3 ⎛ P ⎞1/3 Seed ⎛ Lseed ⎞ ⎜ ⎟ L =⎜ ⎟ or product = Lseed ⋅ ⎜ Seed ⎟ = 1.93 mm P ⎝ ⎠ ⎝ Lproduct ⎠ b. 1 kg H2O corresponds to (1+Cout)kg solution. The initial population density n0 can be eliminated with Eq. SOLUTIONS TO PROBLEMS 8-11 Mass balance over anhydrous salt: Salt in feed + salt in seed crystals = salt in solution + salt in product crystals M salt M salt = L ⋅ xP + P ⋅ F ′ ⋅ x F + Seed ⋅ M salt + 3M water M salt + 3M water Solving for L and P with xF = 1. the nucleation rate B0 with Eq.39 and xP = 0.93 − 0. Follows for the linear growth rate ΔL Lproduct − Lseed 1. the crystallizer volume V and required feed flow rate Q.72m3 ρsoln kg solution/m3solution The crystals occupy 27056·MT / ρc = 1.525 = 0. 3600 ⋅ MT The capacity of the crystallizer = Q· τ = 27. Hence the total volume = 27.6 kg water and P = 223.41 relates residence time τ and magma concentration MT.41: MT = 6ρc kv ⋅ n0 ⋅ (Gτ ) 4 = 6ρc kv ⋅ B0 ⋅ (Gτ ) 4 = G LD LD 4 ⋅( ) 3τ 3 6ρc kv ⋅ 1019 MT G ⋅ (Gτ ) 4 = 6 ρc kv ⋅ 1019 MT for τ gives τ = 9740 s A production rate of P kg crystals/h requires a feed flow rate Q = P = 2. Solution Solving Eq. 8. 8.38.408 in kg anhydrous salt / kg water gives L = 11. the volume of the saturated solution equals (1+ Cout ) ⋅ 27056 kg solution = 27. the density of crystals and the density of the saturated solution determine the total volume required. .02 ≈ 29 m3.0 kg crystals (anhydrous).72 + 1.100 kg crystals/kg water = 2660 kg/m3 = 0.

8-12 CRYSTALLIZATION & PRECIPITATION .

Calculate value of L1 + L2 to ensure that no lead sulfide particles settle in the last chamber. ηwater = 0. The width of all three settling compartments is the same (say 5. Water mass flow rate Qwater =5000 kg/h.3 m3/s). . Calculate the required area of this settling tank operating under laminar flow conditions.s.s. b.005 10-3 Calculate the smallest particle diameter of lead sulfide in the first chamber. The gravitational acceleration g = 9.2 Design a gravity settling tank separator to handle 15 m3/h of an aqueous suspension containing 0. As shown in the drawing below the whole settler consists of three settling chambers. viscosity 1×10-3 Ns/m2). The density ρf of water at 20°C equals 998 kg m-3 and its viscosity ηf = 1. The oil is the dispersed phase.0 μm to 25. ηoil = 0.4 Calculate the diameter D of a settling tank to separate light oil from water.81 m s-2. Q = 0. dp = 1 mm) from an effluent stream (ρ = 1000 kg/m3.Fundamentals of Industrial Separations. The quartz and lead sulfide particles should be separated to the best extend. However. Exercise 9.05 m3 s-1) contains a mixture of spherical lead sulfide particles and spherical quartz (sand) particles.003 Pa. a. Laboratory tests have shown that the unhindered solids settling rate v∞ = 3. ρoil = 900 kg/m3. The values of L1. The droplet diameter dp = 150 μm.5 This exercise concerns the separation of minerals by density difference. It can be assumed that a uniform horizontal flow exists in which the particles can settle unhindered.3 A settling tank is used to separate ion exchange particles (ρS = 1200 kg/m3. each with its own length L. A water stream Qf (0. Both minerals are present in particle sizes ranging from 10. ρPbS = 7500 kg m-3 and ρquarz = 2650 kg m-3.54×10-4 m/s. η = 0.001 Pa.1 Chapter 9: SEDIMENTATION & SETTLING Exercise 9. L2 and L3 have been chosen in such a way that no quartz is collected in the first compartment and no lead sulfite in the last compartment.118 vol% of copper oxide. Qf PbS PbS + SiO2 SiO 2 L1 L2 L3 kg m-1 s-1. Exercise 9. SOLUTIONS TO PROBLEMS 9. this separation is complicated by the fact that smaller heavy particles can have the same settling velocity as larger but lighter particles.0 μm.001 Pa. ρwater = 1000 kg/m3.s. Oil mass flow rate Qoil = 1000 kg/h. Exercise 9.1 Calculate the terminal settling velocity v∞ of a 70 μm diameter sphere (density 2600 kg/m3) in water (density 1000 kg/m3. Exercise 9. The density of copper oxide is 5600 kg/m3.0 m).

Pilot runs on a laboratory tubular bowl centrifuge (L = 0.11 Estimate the diameter of hydrocyclones (H = 4D) required for the separation of polypropylene particles (dp = 10-4 m. what production flow rate could be expected when operating at 15000 rev/min? What is the effective cut size? b.2 SEDIMENTATION & SETTLING Exercise 9. What is the maximum volumetric flow of liquid through the centrifuge such that when the basket is rotated at 200 Hz all particles of diameter greater than 1 μm are retained on the centrifuge wall? Solid density ρS = 2600 kg/m3. r2 = 0. ρG = 600 kg/m3). internal radius R = 0.7 If a centrifuge is 0. respectively and the liquid viscosity η = 0. How many cyclones should be arranged in parallel to handle a stream of 600 kg slurry/s? . liquid density ρL = 1000 kg/m3.5 m long and 0.9 A centrifuge basket 600 mm long and 100 mm internal diameter has a discharge weir 25 mm diameter. Exercise 9. Densities and liquid viscosity as in the previous exercise.6 Compare the gravitational and centrifugal sedimentation rate at 5000 rev/min of yeast cells (dp = 8 μm.01 poise.9. Exercise 9.4 m3/min. The inlet velocity is limited to 3 m/s to limit the pressure drop. The solid and liquid densities are 2800 and 1000 kg/m3. ρS = 1050 kg/m3) in water (ρL = 1000 kg/m3. The centrifuge bowl has an inner radius of rc = 0.8 A continuous tube centrifuge with a bowl 1.0295 m. r1 = 0. at what speed should a laboratory centrifuge of 150 mm diameter be run if it is to duplicate plant conditions? Exercise 9. ηL = 10-3 Pa. ρp = 900 kg/m3) from butane (ηG = 10-4 Pa.10 A low-concentration suspension of clay in water is to be separated by centrifugal sedimentation. liquid viscosity ηL = 0.s. If the separation is to be carried out in the plant using a tubular centrifuge with L = 0.0220 m. All particles of diameter greater than 10 μm are being removed.734 m. Calculate the efficiency of this machine. Exercise 9.0521 m and R – r1 = 0.75 m diameter operating with a pool depth of 0.2 m.s).011 m) operating at 20000 rev/min indicate that satisfactory overflow clarity (50% collection efficiency) is obtained at a throughput of 8·10-6 m3/s. Exercise 9.2 m.9 m in diameter and rotates at 20 Hz.001 Pa.1 m at 1800 rpm is clarifying an aqueous suspension at a rate of 5.s. a.

9.9 and 9.14.9 with the appropriate expression for CD should be used (Eq. 9.15.Assume Re < 1 and solve Eqs.13). 9.12 or Eq.14 and 9. the values for concentration and density are not necessary to solve the problem. 9.8 = 4. Re is outside valid ⎝Re ⎠ ⎝0. Re is outside valid ⎝Re ⎠ ⎝0. the combination of Eqs. Eq.13: ⎛C ⎞ ⎛80 ⎞ .2 Given aqueous suspension.54⋅10-4 m/s Q = 15 m3/h The required tank area A ρS = 5600 kg/m3 cCu = 0. Thus. 9.13: ⎜ D ⎟ = ⎜ ⎟ . otherwise v∞ would follow from Eq. 9. gravity settling v∞ = 3. 9.3⎠ and v∞ follows from Eq. Solving for dp gives dp = 11. 9.11 is valid so v ∞ = 4.11 applies and v ∞ = 2 dp 18ηL ( ρ p − ρL )g .27 ⋅ 10 m/s ηL A more general approach is to eliminate v∞ from Eqs.22. Solution Volumetric flow rate Q = 15 m3/h = 4.118 vol% Find Thoughts The minimal required area can be calculated from Eq. Solution For Re < 1. 9. 9.5 ⎠ range. 9.167⋅10-3 m3/s Use Eq. the particle diameter dp can be calculated from the known settling rate. 9. 9.8 m2 v ∞ 3. The easiest solution is to assume that one equation is valid and check the Re number afterwards.8⎞ .3 < 1 Æ Eq. otherwise v∞ would follow from Eq. 9.2·10-3 < 1 (Re OK).22 to calculate the required tank area: A ≥ Q = 15 / 3600 = 11. the sedimentation is unhindered at this low concentration. the terminal settling velocity of this particle ηL = 1⋅10-3 Ns/m2 Thoughts To calculate the terminal settling velocity v∞ of a spherical particle.1 Given Find dp = 70 μm (sphere) ρS = 2600 kg/m3 ρL = 1000 kg/m3 v∞.15.Assume 5 < Re < 500 and solve Eqs.10 or Eq. ⎛C ⎞ ⎛27. Exercise 9. .14 and 9.54 ⋅ 10−4 Note: Probably.Assume 1 < Re < 5 and solve Eqs.14 and 9.12 or 9.10. 9.15.9 and 9. v∞. 9. 9. CD Re 2 = 4 d p ρL ( ρS − ρL ) g (valid for any value of Re) 3 η2 3 and to solve for CD and Re with either Eq.27 ⋅ 10−3 m/s Check Reynolds number: Re = ρL ⋅ v ∞ ⋅ d p −3 = 0.2⎞ . SOLUTIONS TO PROBLEMS 9.10 gives Eq.10: ⎜ D ⎟ = ⎜ ⎟ hence Re < 1 is OK ⎝Re ⎠ ⎝0.11: v∞ = 2 dp 18ηL ( ρ p − ρL )g = (70 ⋅ 10−6 )2 18 ⋅ 10−3 (2600 − 1000) ⋅ 9.3 SOLUTIONS Exercise 9.5 ⎠ range.9 μm and Re = 4.Fundamentals of Industrial Separations. 9.12: ⎜ D⎟=⎜ ⎟ . resulting in Eq. ⎛C ⎞ ⎛83. As the gravitational solids settling rate is given. If Re < 1 then Eq. 9.15. 9.

A≥ vs = 2. 9. Now assume that 5 < Re < 500 and use Eq.818 . D = 1. 9.8 = 0. Qwater / ρwater + Qoil / ρoil the settling can be considered to be hindered.65 gives v s / v ∞ = ε 2 ⋅ ε 2.65 = 0.14 with CD = 18. The volume fraction ε of the fluid is calculated from Eq. Re OK and v ∞ ≡ ρ ⋅ d 34. ηwater The volume fraction of the fluid ε = Qwater / ρwater = 0. Eq. For the settling rate.9 with the appropriate expression for Solution First assume that Re < 1 and use Eq. Combining Eqs. 9.: Thoughts The terminal settling velocity v∞ has to be calculated from Eq.0344 Exercise 9. as given in Eq. 9. 9.22.5 ⋅ 10−4 )2 18 ⋅ 10 −3 (900 − 1000) ⋅ 9. 9. Finally. 9.22: Amin = QV = 18 / 60 = 8.17.001 Pa⋅s Qoil = 1000 kg/h Qwater = 5000 kg/h = 150 μm (oil in water dispersion) Find D. 9. 9.3 Given Find dp = 1 mm η = 1⋅10-3 Pa⋅s ρS = 1200 kg/m3 QV = 18 m3/min ρL = 1000 kg/m3 A.11: v∞ = 2 dp 18η ( ρS − ρL )g = (1⋅ 10−3 )2 18 ⋅ 10−3 (1200 − 1000) ⋅ 9.4 SEDIMENTATION & SETTLING Exercise 9.11): v∞ = 2 dp 18η ( ρoil − ρwater )g = (1. 9. the tank area can be calculated: Qwater / ρwater 2 . The hindered settling rate is smaller by a factor ε2·f(ε). diameter of a settling tank to separate oil from water of the dispersed phase (the oil droplet) have to be calculated.5⋅Re-0.2 ⎞ Re ⋅ η Solve for CD and Re: ⎜ D ⎟ = ⎜ = 0.11 is not valid. the volumetric flow of the continuous phase and the settling rate Solution The unhindered terminal droplet velocity (Eq.4 Re ⎠ ⎝ ⎠ ⎝ L p The required tank area with Eq. Thoughts To calculate the required tank area.13).9. 9.18 Æ Eq.11 may be applied (check Re). 9.16.109m/s Check Re: Re = ρL ⋅ v ∞ ⋅ d p = 109 ηL Æ Eq.6 (Eq. 9. ⎛C ⎞ ⎛2. with Eqs. For a cylindrical tank.22 is used to evaluate the minimum tank area.7 m2 v∞ 0.11 is valid.16 and 9. 9.4 Given ρoil = 900 kg/m3 ρwater = 1000 kg/m3 dp ηoil = 0. the required tank area for this separation CD (see Exercise 9. ρoil ⋅ v ∞ ⋅ d p Check the Re number : Re = = 0.1).9 m min 1 with n = 2. Eq.5 it follows that vs = -5·10-4 m/s. From this settling rate.003 Pa⋅s ηwater = 0.7·10-4 m/s .9 m.8 = −1.16 and 9. 9.393 1 and the hindered settling rate vs = 0. ⎟ .19 vs would be -3.225 ⋅ 10−3 m/s Note that the velocity of the oil droplets is directed upwards (oil is lighter than water).0344 m s-1.482·10-3 m/s. The area A follows from Eq.18 with n = 2.

6 Given Find dp = 8 μm η = 1⋅10-3 Pa⋅s ρp = 1050 kg/m3 rc(entrifuge) = 0. ( ρPbS − ρwater ) ⋅ d x = ( ρquarx − ρwater ) ⋅ dmax Solving for dx gives dx = 12. thus Eq.11 is applicable to all particles.11 leads to 2 2 . Combining vPbS(dx) = vquarz(dmax) and Eq.204 ⋅ 10−3 m / s 18 ⋅ ηwater Hence. Eq.11). 9.81 m/s2 = 0. 9.001 Pa. Eq. Thoughts Eq. Thoughts a. b. Don’t forget to check the boundary condition. Check this for the largest leadsulfide particles: ρ ⋅v ⋅d Remax = water PbS max max with ηwater v PbS max = 2 g ⋅ ( ρPbS − ρwater ) ⋅ dmax = 2. An expression to relate unhindered. Re < 1.11 can be used to Solution Gravitational sedimentation rate: v g∞ = 2 dp 18η ( ρS − ρL )g = (8 ⋅ 10−6 )2 18 ⋅ 10 −3 (1050 − 1000) ⋅ 9. this is the maximum value. Re = 0. 9.2 m ρL = 1000 kg/m3 ω = 5000 rev/min The gravitational and the centrifugional stationary sedimentation velocity v∞. 9. Exercise 9. With v PbS (dmin) = 3.11 is valid.5 Given ρPbS = 7500 kg/m3 g QV = 9. see Eq. 9.055. stationary settling velocity with density and diameter is available (Eq. the settling time balances the residence time: τ↓ = τ → .Fundamentals of Industrial Separations. SOLUTIONS TO PROBLEMS 9. Smallest particle size of heavier species in the first chamber b. The settling time of the smallest PbS particles equals the residence time in the direction of the flow along a distance L1 + L2. The settling time of the smallest PbS particles τ ↓ = The residence time τ → = H (H is the settling height) v PbS (dmin) L1 + L2 (L1 + L2 ) ⋅ w ⋅ H = (w is the width of the settling chambers) u Qwater In the limiting situation that the smallest PbS particles just reach the end of the trajectory L1 + L2.2 m.8 = 1.s dmin = 10 μm ρwater = 998 kg/m3 w dmax = 5.5 Exercise 9. The velocity of the smallest leadsulfide particles (with diameter dx) in the first chamber equals the Solution a. Minimum value of L1 + L2 to prevent settling of the heavier species in the last chamber velocity of the largest quarz particles in the second chamber: vPbS(dx) = vquarz(dmax).6 μm.05 m3/s ρquarz = 2650 kg/m3 ηwater = 0. b. calculate the gravitational sedimentation rate at Re < 1. η .31 applies to centrifugal sedimentation and can be used at Re < 1..74 ⋅ 10−6 m/s Check: Re = ρL ⋅ v g ∞ ⋅ d p = 1. 9.5 ⋅ 10−5 < 1. Eq. 9. 9.11 is applicable only for Re<1.54 ⋅ 10−4 m / s follows L1 + L2 = 28.0 m = 25 μm Find a.22 with A = (L1 + L2)·w.

9.6 SEDIMENTATION & SETTLING Sedimentation rate in the centrifuge: ω = 5000 rev/min = 83.375 / 0. . the Sigma concept is used. the left-hand side represents the Solution First.31 is valid.8 ⋅ 10−5 m/s 0.078 < 1. The right-hand side represents the actual performance of the machine. use Eq.275) → the centrifuge is 3580 / 918 = 3.75 m ηL = 0.4 m3/min ρS = 2800 kg/m3 Find The efficiency of this machine compared to gravitational settling process parameters.90 times more efficient than gravitational settling.75 ⋅ 10−3 m/s Check Re = ρL ⋅ v c∞ ⋅ d p = 0.09 m3/s and Σ g = QV = v∞ For the machine sigma. 9. Eq.8 = 9. v c∞ rc ω 2 = ≈ 5600 times faster v g∞ g Exercise 9.4)2 = 9. η Note that the sedimentation rate in the centrifuge is compared to gravitational sedimentation.375 m r1 = r2 – pool depth = 0.s dcut-off = 10 μm ω = 1800 rpm ρL = 1000 kg/m3 pool depth = 0. 9. this is known as the ‘process’ Sigma. use the right-hand side of Eq.4 m /min = 0. or the machine Sigma. 9.5 rad/s 2 2 Centrifuge volume VC: VC = Lπ (r2 − r1 ) = 1. the centrifuges should produce the same acceleration: Eq. Thoughts To calculate the efficiency.8 ⋅ ln(0.2752 ) = 0.9.306 ⋅ 188.3 rev/s = 523. In Eq. or the desired area (the required ‘performance’ of the machine).5 ⋅ π ⋅ (0.45 = 20 ⋅ = 49 Hz r2 0.075 Exercise 9.3752 − 0.7 Given Find Large centrifuge: D = 0. Solution 2 2 hence ω2 = ω1 ⋅ r1 ⋅ ω1 = r2 ⋅ ω2 r1 0.35.4 rad/s v c∞ = 2 dp 18η ( ρS − ρL ) ⋅ rc ω 2 = (8 ⋅ 10−6 )2 18 ⋅ 10 −3 (1050 − 1000) ⋅ 0.001 Pa.8 Given Tube centrifuge: L = 1.09 9.1 m QV = 5.5 m D = 0. The ratio of the actual ‘area’ and the area required by the process can be used as a measure of efficiency. 9. v∞: v∞ = 2 dp 18η ( ρS − ρL )g = 3 (10 ⋅ 10−6 )2 18 ⋅ 10 −3 (2800 − 1000) ⋅ 9.306 m3 2 2 V ⋅ω 0.11 to calculate the terminal settling velocity (under gravity).9 m. ω = 20 Hz Lab-scale centrifuge: D = 150 mm The rotational speed required in the lab centrifuge to duplicate plant conditions Thoughts To duplicate plant conditions.5 Σ machine = C = = 3580 m2 ⎛r ⎞ g ⋅ ln⎜ 2 ⎟ ⎝ r1 ⎠ 9.275 m ω = 1800 rpm = 30 r/s = 188.27.2 ⋅ (523.35: r2 = centrifuge radius = D/2 = 0.8 ⋅ 10−5 = 918 m2 QV = 5.

05 m r1 = 25/2 mm = 0.0295 m ωlab QV.28 ⋅ 10−4 ⋅ 20902 9.0125 Exercise 9.01 g/s·cm = 0.01 poise D = 0.022 2 = 217 m2 ) 0.28 ⋅ 10 m and ωlab = 20000 rad ⋅ 2π = 2094 60 s ⇒ 50% Σ lab = 2. Σ 50% = lab 2 VC.001 N·s/m2 ≡ 0.lab 2. Eq.011 m ρS = 2600 kg/m3 R-r1 = 0.8 ⋅ = 4. see previous exercise. The maximum flow Q is Solution ηL = 0.lab ⎠ 2 2 −4 3 with VC.lab ) = 2.052 − 0.9 Given L = 0.34 or 9.lab ωplant = 20000 rev/min = 8·10-6 m3s-1 = 15000 rev/min Find a. r2 = 100/2 mm = 0.01252 ) = 4.05 18 ⋅ 10−3 9.10 Given Llab = 0. 9.6 rad/s Qmax follows from Eqs.lab = 0.6 m ω = 200 Hz ηL = 0.35 can then be used directly to calculate the flow rate.47 ⋅ 10−4 m3 /s = 4. 9.11 and 9.Fundamentals of Industrial Separations. Solution a.8 ⋅ ln 0. Note that the viscosity of the liquid is given in poise. Note that the viscosity of the liquid is given in poise.62 ⎝ ⎠ (2600 − 1000) ⋅ 9.022 m ηL = 0.42 ⋅ 10−3 ⋅ 0. 9. The maximum volumetric flow QV.8 ⋅ ln( 2 ⋅ 0.1 m dmax = 1 μm ρL = 1000 kg/m3 weir = 25 mm ρS = 2600 kg/m3 Find The maximum volumetric flow Q to reach this separation obtained if the centrifuge works at 100% efficiency.01 poise ρL = 1000 kg/m3 Lplant = 0.39.0222 . Thoughts a. lab − r1 .plant to reach this separation b.2 m r2.lab = 0.001 kg/s·m = 0.0125 m 2 2 VC = Lπ (r2 − r1 ) = 0. 9.42 ⋅ 10−3 m3 ω = 200 Hz = 200⋅2⋅π rad/s = 1256. The cut size depends on the Stokes terminal velocity v∞.34 or 9.0112 + 0. hence combine Eqs. Eq. The maximum flow is obtained if the centrifuge works at 50% efficiency.001 Pa·s.01 poise = 0. Calculate the effective cut size used directly to calculate the flow rate.35 with a cut-off diameter of 1 μm: ⎡ 2 ⎤ d ω2 Qmax = VC ⎢ max ( ρS − ρL ) ⋅ g⎥ = ⎢ ⎥ ⎣ 18ηL ⎦ g ⋅ ln r2 r1 2 ⎛ ⎜10−6 ⎞ ⎟ 1256.7 Exercise 9. lab ⎟ g ⋅ ln⎜ ⎜r 2 + r 2 ⎟ ⎝ 1.6 ⋅ π ⋅ (0. SOLUTIONS TO PROBLEMS 9.734 m R = 0.lab = Llab ⋅ π (r2.39 can then be b.0521 m 50% collection efficiency r1.lab ⋅ ωlab ⎛ ⎞ 2 2r2. Thoughts The volume of the centrifuge can be calculated from the given dimensions.

9- 8

SEDIMENTATION & SETTLING

50% Σ plant =

VC, plant ⋅ ω 2 plant ⎛ ⎞ ⎜ 2R2 ⎟ g ⋅ ln⎜ ⎟ 2 ⎜ r1 + R2 ⎟ ⎝ ⎠

with VC,plant = 5.08 ⋅ 10−3 m3 and ω plant = 1571

rad s

50% Σ plant =

5.08 ⋅ 10−3 ⋅ 15712 9.8 ⋅ ln( 2 ⋅ 0.05212 0.02262 + 0.05212 )

= 2455 m2

QV,plant = QV,lab ⋅

Σ plant = 9.05 ⋅ 10−5 m3s−1, about 10-times that of the lab centrifuge. Σ lab

b. The cut size depends on the Stokes’ terminal velocity v∞ and the terminal velocity determines the throughput QV: Eq. 9.11 v ∞ = Eq. 9.39 v ∞ =
2 dcut ⋅ ( ρS − ρL ) ⋅ g 18 ⋅ ηw

QV,plant 2 Σ plant ⇒ dcut = 0.15 μm (check that Re < 1)

Eliminate v∞ and solve for dcut

Exercise 9.11

Given

Hydrocyclone: H = 4D dp = 10-4 m ηL = 10-4 Pa.s a. the diameter of the cyclone b. the number of cyclones to process 600 kg/s slurry

vin

ρs ρL

< 3 m/s = 900 kg/m3 = 600 kg/m3

Find

Thoughts a. The performance of a hydrocyclone can be estimated with Eq. 9.53. The inlet area can be
calculated from the cyclone diameter using the ‘rule-of-thumb’ (see context of Eq. 9.49).

b. Calculate the flow in one cyclone (Eq. 9.49). By converting the total mass flow to a total
volumetric flow, the number of required cyclones follows from the ratio of total flow and capacity of one cyclone.

Solution

a. For d0 = 0.1 mm and H = 4D, the cyclone diameter can be calculated:
d0 = 3ηD 2 2 πv f ( ρs − ρ ) H

D=

2 8πv f ( ρs − ρ) (1⋅ 10−4 )2 ⋅ 8 ⋅ π ⋅ 3 ⋅ (900 − 600) d0 = = 0.754 m 3η 3 ⋅ 10−4

b. The maximum volumetric flow rate that can be treated in one cyclone is:
D2 = 0.095 m2 6 Q = v f ⋅ Ain = 3 ⋅ 0.095 = 0.28 m3 /s Ain =

The minimum density of the slurry is the butane density, 600 kg/m3; the total volumetric kg kg flow rate of 600 kg slurry/s equals 600 / 600 = 1.0 m3s−1. s m3 Number of cyclones: 1.0 / 0.28 = 4 cyclones.

Fundamentals of Industrial Separations, SOLUTIONS TO PROBLEMS

9- 9

Fundamentals of Industrial Separations, SOLUTIONS TO PROBLEMS

10-1

Chapter 10: FILTRATION
Exercise 10.1 A slurry is filtered with a laboratory leaf filter with a filtering surface area of 0.05 m2 to determine the specific cake and cloth resistance using a vacuum giving a pressure difference of 0.7 bar. The volume of filtrated collected in the first 5 min was 250 cm3 and, after a further 5 min, an additional 150 cm3 was collected. The filtrate viscosity is 10-3 Pa.s, the slurry contains 5 vol% of solids with a density of 3000 kg m-3. Calculate the specific cake resistance α and the cloth resistance RM. Exercise 10.2 The data given in the table below were obtained from the constant pressure period of a pilot scale plate and frame filter press. The mass of dry cake per unit volume of filtrate amounts to 125 kg/m3, filter area A = 2.72 m2, viscosity η = 10-3 Pa.s, pressure difference ΔP = 3 bar. time: filtrate volume V: 92 0.024 160 0.039 232 0.054 327 0.071 418 0.088 472 0.096 538 0.106 (s) (m3)

Calculate the cake resistance α. Exercise 10.3 Calculate the specific cake resistance α and the medium resistance RM when the same slurry data apply from the following constant rate data obtained on the same pilot scale plate and frame filter press: V: ΔP: Exercise 10.4 Laboratory filtrations conducted at constant pressure drop on a slurry of CaCO3 in water gave the data shown in the following table: Filtrate Volume V (l)
0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0

0.016 0.9

0.032 1.2

0.040 1.35

0.056 1.7

0.064 1.8

0.072 1.85

0.088 2.3

0.096 2.4

0.114 2.7

(m3) (bar)

Test I (0.45 bar) t (s)
17 41 72 108 152 202

Test 2 (1.10 bar) t (s)
7 19 35 53 76 102 131 163

Test 3 (1.95 bar) t (s)
6 14 24 37 52 69 89 110 134 160

Test 4 (2.50 bar) t (s)
5 12 20 30 43 57 73 91 111 133 157 183

Test 5 (3.40 bar) t (s)
4 9 16 25 35 46 59 74 89 107

Liquid density and viscosity as in previous exercise. drum speed = 1 rpm.1 kg of solid (solid density ρS = 2500 kg m-3) per kilogram of water. liquid density ρL = 1000 kg/m3 and viscosity ηL = 0. operational speed and cake thickness required to produce 5 m3/h of filtrate with a 1 m wide horizontal belt filter operating at a pressure difference ΔP = 60 kPa. cake moisture 3.6 A slurry.8*1010 m/kg and medium resistance RM = 3. Exercise 10. Exercise 10. viscosity η = 10-3 Pa.7 A rotary drum filter with 30 percent submergence is to be used to filter an aqueous slurry of CaCO3 containing 230 kg of solids per cubic meter of water.s Exercise 10.1 kg solids/kg slurry.0 800 5. Calculate the thickness of the cake produced when it has a porosity ε = 0. Evaluate the quantities α and RM as a function of pressure drop ΔP. liquid density ρL = 1000 kg/m3.7 400 4. The pressure drop is to be 0. solid density ρS as in Exercise 10. Liquid density ρL = 1000 kg m-3. a.001 Pa.8 140 2. and fit an empirical equation to the results for α. The drum rotates at a speed of one revolution in 6 min and 20 per cent of the filtering surface is in contact with the slurry at any instant. Determine the filtrate and dry solids production rate when filtering with a pressure difference of 65 kN/m2.0*109 m-1.s. The specific cake resistance α = 1. slurry solids concentration cS = 350 kg/m3.9 Calculate the filtration time. b.5 g/L.5. The cake porosity ε = 0.1 210 2. fraction submerged f = 0.4 104 1. liquid viscosity ηL = 0.5 kg wet cake/kg dry cake. obtained from a series of constant pressure filtration experiments: Filtration pressure ΔP : Specific resistance α: Exercise 10.10-2 FILTRATION The filter area A = 440 cm2. liquid viscosity ηL = 0.001 kg m-1 s-1.6 m.6 m and diameter D = 0. the mass of solid per unit volume of filtrate was 23. 70 1. Calculate the filter area required to filter 40 ltr/min of slurry when the filter cycle time is 5 min.3.4.5 Calculate the relationship between the average specific resistance and the filtration pressure from the following data.45 bar. medium resistance RM = 1×1010 1/m. solids density ρS = 2000 kg/m3.s and the temperature 25°C. Specific cake resistance α = 2.001 Pa.6 (kPa) (×1011 m/kg) . The slurry has the following properties: specific cake resistance α = 5×109 m/kg. containing 0. Exercise 10. solids concentration xS = 0. is fed to a rotary drum filter with length L = 0.43.0*109 m-1. required area.8 Calculate the dry solids production from a 10 m2 rotating vacuum filter operating at 68 kPa vacuum and the following conditions: cake resistance α = 1×1010 m/kg.1*1011 m/kg and medium resistance RM = 6.

Exercise 10. solids concentration cS = 150 kg/m3 filtrate. medium resistance RM = 2·109 1/m αav = 7. Of the total 9 m belt length 1.84ΔP-0. Filter data: Cake properties: Filtrate: Exercise 10. viscosity ηL = 0. Solid density ρS = 2000 kg/m3.5 m is available for the filtration stage.11 A tank filter is operated at a constant rate of 25 L/min from the start of the run until the pressure drop ΔP = 3.635 m diameter. and then at a constant pressure drop of 3.53. Given: specific cake resistance α = 1.46 m/kg. a. The cake porosity ε = 0.0·1010 m-1.5 bar.254 m height) rotating at 20 rps. its specific resistance α = 6×109 m/kg.s. Calculate the solids production rate (kg/s). How does the washing rate change when a 5 cm thick supernatant liquid layer is present? width 2 m. liquid density ρL = 1000 kg/m3 and liquid viscosity ηL = 0. What time is required for the passage of two void volumes of wash if there is almost no supernatant liquid layer over the cake. viscosity ηL = 0.001 Pa. linear velocity 0. medium resistance RM = 1.s. solid density ρS = 2350 kg/m3 density ρL = 1390 kg/m3.5 bar until a total of 5 m3 of filtrate is obtained.001 Pa.12 Calculate the washing rate of a filter cake 0.1 m/s.025 m thick deposited on a centrifuge basket (0.Fundamentals of Industrial Separations. εav = 0. b. Assume the cake is incompressible.1·108ΔP0. Calculate the total filtration time required.10 It is proposed to use an existing horizontal belt filter to separate phosphoric acid from a slurry containing gypsum at 30% w/w. 0.8·1011 m/kg. A medium with a resistance of RM = 1·108 m-1 is used to line the perforate basket. SOLUTIONS TO PROBLEMS 10-3 Exercise 10.001 Pa.054. Cake formation at a constant pressure difference of ΔP = 50 kPa is to be followed by displacement washing and deliquoring.s P P .

10-4 FILTRATION SOLUTIONS .

. SOLUTIONS TO PROBLEMS 10-5 In the graph at the following page a plot at each pressure difference is given. The table summerizes the calculated values of αav and RM.Fundamentals of Industrial Separations.

004 0.8 intercept x 109 kg/m·s 1.55 5.79 12.5 .002 0.88 2.26 1.008 Test 1 2 3 4 5 slope x 1011 kg/m7s 6.29 8.98 6.006 V /m3 0.37 8.10-6 FILTRATION ΔP ⋅ t kg m 4s 1 1010 V 8 109 6 109 Test 1 4 10 9 Test 2 Test 3 2 109 Test 4 Test 5 0 0 0.5 α x 1010 m/kg 4.53 8.46 15.88 9.32 7.26 1.89 7.00 3.05 8.80 14.29 RM x 1010 1/m 5.

SOLUTIONS TO PROBLEMS A plot of ln(α) vs ln(ΔP) is presented in the following figure: 26 10-7 lnα 25 24 10 11 12 ln ΔP 13 t vs V ⋅ ΔP n to get a unified plot V Closer inspection of Eqs. 10.15 suggests plotting ΔP ⋅ ΔP ⋅ t.2 0. kg V m 4s 8 109 9 6 10 Test 1 Test 2 9 4 10 Test 3 Test 4 2 109 Test 5 0 0 0.6 V ⋅ ΔP n m įPa 3 n 0.14 and 10.4 0.8 .Fundamentals of Industrial Separations.

10-8 FILTRATION .

Fundamentals of Industrial Separations. SOLUTIONS TO PROBLEMS 10-9 .

10-10 FILTRATION .

SOLUTIONS TO PROBLEMS 10-11 .Fundamentals of Industrial Separations.

10-12 FILTRATION .

SOLUTIONS TO PROBLEMS 10-13 .Fundamentals of Industrial Separations.

10-14 FILTRATION .

0 kg m-3.4 Calculate the osmotic pressure of a solution containing 0. Exercise 11. .0050 kmol m-3.5 The permeability of a membrane is experimentally determined by measuring the flow of an aqueous NaCl solution in a reverse osmosis module at a given pressure difference. The equilibrium constant K = 1. Exercise 11.1 mol NaCl kg H2O at 25°C.Fundamentals of Industrial Separations.2 The concentration of a solute at both sides of a membrane with thickness 30μm is 0. Calculate the permeances for water and sodium chloride. The measured flow rate is 1. The density of pure water at 25°C amounts to 997. The inlet concentration cin = 10 kg /m3 solution with a density of 1004 kg/m3 solution.5 and DA = 7. Exercise 11.1 Show that permeability can be expressed in m2s-1. the membrane area A = 0.1.1 Chapter 11: MEMBRANE FILTRATION Exercise 11.0 10-11 m2 s-1 in the membrane.92 10-8 m3 solution/s at a pressure difference of 54. Calculate the flux and the concentrations at the membrane interfaces inside the membrane. SOLUTIONS TO PROBLEMS 11.39 kg/m3 solution with a density of 997 kg/m3 solution. Compare the result with the experimental value given in Table 11.0020 m2. The mass transfer coefficients at both liquid sides can be considered as infinite.030 kmol m-3 and 0. The product concentration cout = 0.3 Repeat the previous exercise in case that the mass transfer coefficient at the product side amounts to 2 10-5 m s-1. Exercise 11.4 atm.

11- 2

MEMBRANE FILTRATION

SOLUTIONS Exercise 11.1 Show The dimension of permeability can be m2 s-1.
PM,i plays a role similar to that of the coefficient of diffusion.

Thoughts Pick a flux equation such as Eq. 11.3c, with Δc as the driving force. Then the proportionality constant
[N ] ⋅ [δ ] mol m3 m2 = ⋅m⋅ = . Compare with permeance in exercise 11.5. [c] mol s m2 ⋅ s

Solution

[PM,i ] =

Exercise 11.2 Given Find Thoughts Solution cF = 0.030 kmol s-1 KA = 1.5 cP = 0.0050 kmol s-1 DA = 7.0·10-11 m2 s-1

δ = 30 μm
k1 = k2 = ∞

The flux JA and the concentrations at the interfaces inside the membrane, cA,z=0 and cA,z=δ, respectively.
The concentration gradient is depicted in Fig. 11.7; Eqs. 11.3c and 11.12 is applicable (Δc driving force).

The relevant transport equation is given by Eq. 11.12:

D K D 1.5 ⋅ 7 ⋅ 10−11 JA = A (cA,z=0 − cA,z=δ ) = A A (cF − cP ) = ⋅ (0.03 − 0.0050) = 8.75 ⋅ 10−8 kmol s−1 m−2 −6 δM δM 30 ⋅ 10 JA cA,z=0 cA,z=0 = KA·cF = 45 mol m-3; cA,z=δ = KA·cP = 7.5 mol m-3.

cF cA,z =δ cP

δΜ

Exercise 11.3

Given

cF = 0.030 kmol m-3 KA = 1.5 kF = ∞

cP = 0.0050 kmol m-3 DA = 7.0·10-11 m2 s-1 kP = 2·10-5 m s-1.

δM = 30 μm

Find

The flux JA and the concentrations at the interfaces inside the membrane, cA,z=0 and cA,z=δ, respectively.
expression in Eq. 4.6, where also a concentration gradient contributes to the rate of mass transfer.

Thoughts On the feed side simply apply Eq. 11.11. On the product side, see the derivation of the kinetic Solution Feed side: cA,z=0 = KA· cF = 45 mol m-3. No accumulation of matter takes place in the interface between membrane surface and product phase, hence the rate of mass transfer through the membrane equals that through the stagnant film at the product side. The rate expressions according to the film theory:

Fundamentals of Industrial Separations, SOLUTIONS TO PROBLEMS

11- 3

JA =

δM

DA

(cA,z=0 − cA,z=δ ) = kP (cP,z=δ − cP ) or, with Eq. 11.11a

JA =

KA DA

δM

(cF − cP, z=δ ) = kP (cP,z=δ − cP )

Eliminate cP,z=δ by summation of the following two expressions
cF − cP,z=δ = JA J cP,z=δ − cP = A kP

δM

JA cA,z=0

KA DA

giving

⎛ δ 1⎞ cF − cP = JA ⎜ M + ⎟ or ⎝ KA DA kP ⎠ 1 cF − cP 1 JA = = kOL (cF − cP ) with = kOL 1 1 δM δM + + KA DA kP KA DA kP

cF

cA,z=δ cP,z=δ

δΜ

cP

JA = 2.98 ⋅ 10−6 ⋅ (0.030 − 0.005) = 7.45 ⋅ 10−8 kmol s−1 m−2

According to the film theory: JA = kP·(cP,z=δ – cP) = 7.45·10-8 kmol m-2 s-1 Hence, cP,z=δ = 8.72 mol m-3 and cA,z=δ = K· cP,z=δ = 13.0 mol m-3.

Exercise 11.4 Given cNaCl = 0.1 mol / kg H2O

ρw = 997.0 kg m-3.

Find

Osmotic pressure
Note that 1 mole NaCl dissociates into 1 mole Na+ plus 1 mole Cl-. Assume that the density of this very diluted solution equals that of pure water.

Thoughts Apply the Van’t Hoff relation Πosm ≈ cRT (Eq. 11.1) with c in mol ions per unit volume of pure solvent.

Solution

2 ⋅ 0.1 ⋅ 8.31⋅ 298 = 4.938 bar = 4.88 atm . 1/ 997.0 The experimental value is slightly less: 4.56 atm. c=

Exercise 11.5 Given flow rate = 1.92·10-8 m3 s-1 cin = 10.0 kg / m3 solution cout = 0.39 kg / m3 solution Msalt = 0.0585 kg mol-1

Δp = 54.4 atm ρsolution in = 1004 kg/m3 ρsolution out = 997 kg/m3
A = 2.0·10-3 m2

Find

The permeances for water and sodium chloride at 25°C.
The water flow has to be converted into a water flux [kg s-1 m-2] and the osmotic pressures at both sides of the membrane must be calculated (Van ‘t Hoff: π = cRT). Note that the concentration of salt at the product side is sufficiently low to assume that ρpure water = ρsolution out.

Thoughts Eq. 11.03b is applicable for water whereas Eq. 11.3c defines the solute flux.

11- 4

MEMBRANE FILTRATION

From the water flux, the salt flux can be calculated by noting that the product concentration is defined by the ratio of the solute flux and the solvent flux.

Solution

Calculation of the water flux 1.92 ⋅ 10−8 × 997 m 3 solution 1 kg solvent kg water ⋅ ⋅ ≈ 9.57 ⋅ 10−3 1.92·10-8 m3 soln / s ⇒ −3 2 3 s m m solution 2 ⋅ 10 s ⋅ m2 Calculation of osmotic pressure The concentration c to be applied in the Van ‘t Hoff equation is expressed as mol NaCl per m3 pure water. 1 m3 product solution contains 0.39 / 0.0585 mol NaCl and (997-0.39) / 0.39 / 0.0585 997 m3 pure water. Hence, cproduct = = 6.67·10-3 mol NaCl / m3 H2O and (997 − 0.39) / 997 the πproduct = 2·6.67·8.31·298 = 0.33·105 Pa = 0.33 atm. Similarly, 1 m3 feed solution contains 10 / 0.0585 mol NaCl / m3 solution and 1004 – 10 = 10 / 0.0585 994 kg pure H2O with a volume of 994/997 m3. Hence, cfeed = = 171.5 (1004 − 10) / 997 mol NaCl / m3 H2O and πfeed = 2·171.5·8.31·298 = 8.49·105 Pa = 8.38 atm.

It follows for the permeance of water (Eq. 11.3b) 9.57·10-3 /[54.4 – (8.32-0.33)] = 0.207·10-3 kg s-1 m-2 atm-1.
Calculation of the solute flux
cout = Nsolute . Nwater / ρwater

Nsolute = 0.39 ⋅

kgNaCl 9.57 ⋅ 10−3 = 3.74 ⋅ 10−6 997 s ⋅ m2

The permeance of NaCl becomes (Eq. 11.3c): 3.74·10-6 / (10 – 0.39) = 0.390·10-6 m s-1.

12 0.02 0.05 0. applicable for this simultaneous olefin and paraffin recovery from the vent gas? After recovery the olefin/paraffin needs to be separated in two fractions.Fundamentals of Industrial Separations. SOLUTIONS TO PROBLEMS 12-1 Chapter 12: SEPARATION SELECTION METHODS Exercise 12. The composition is given by (1 bar.85 0.68 0.0 0. a. 1-pentene en 1-hexene) in pure state.5 mol% mol % mol % mol % 1-Butene 1-Pentene 1-Hexene 3 mol % 2 mol % 1 mol % Within the R&D department of the company it is explored which techniques may be technically and economically feasible to recover the three olefins (1-butene. b.08 0.5 1. Can you determine which two key components need to be separated (selectivity>1) in order to achieve a full olefin/paraffin separation? c. In other words achieve a selectivity = (x1/y1) /(x2/y2) > 1? A possible alternative for absorption is extraction with a solvent that has a higher affinity for olefins compared to paraffins.4 3.1 The vent gas from several polymer plants contains air.03 0. pentane.05 0. in your opinion.20 0. In principle.0 0.10 0.24 Distribution Coefficient (concentration in solvent/concentration in feed) NMP 0. hexane) and the olefins.15 DEG 0. 25°C): Air Butane Pentane Hexane 91 1. this is possible by selective absorption of the olefins. As a first step they are considering the purification of the air by simultaneous recovery of the olefins and the paraffins. bar) 2. What separation methods are. paraffins and olefins (monomers).25 0.12 DMSO 0. d.06 0. What are the two key components in order to obtain a full olefin/paraffin separation when extraction with a highly polar solvent is applied? e.08 0.04 0. What is the minimal required difference in affinity (activity coefficients) of the absorption liquid towards both key components to achieve this full olefin/paraffin separation. Which of the solvents below are in principle suitable (selectivity>1) for a complete separation of the olefin and paraffin fractions? C4 C4= C5 C5= C6 C6= Vapor pressure(25°C.15 . the paraffins (butane.01 0.10 0.20 0.01 0. The company has decided to approach you as a consultant and prepared several questions for the first meeting.

Consider the mixture to behave (almos)t ideal.2 In a large chemical plant methylcyclohexane is separated from toluene by distillation. for extractive distillation and for extraction to separate this mixture into its four pure constituents? What distillative separation might become problematic and why? e. b.12-2 SEPARATION SELECTION METHODS Exercise 12. A detailed evaluation requires firstly the characterization of the current separation between methylcyclohexane and toluene.5 . d. Which of the arrangements seems. f. bar) Cyclohexane 0. Which of the given solvents might be feasible to enhance the relative volatility sufficiently to make extractive distillation economically attractive? c. the most economical solution. For the construction of a new plant it is considered whether the use of extractive distillation or extraction could provide economically more attractive options. Why is the counting of the number of operations sufficient to get a first impression about the most economical route? What effects are not taken into account? Benzene Vapor pressure (80°C.39 Activity coefficient at infinite diliution NMP 1. a.54 Toluene 1. Besides methylcyclohexane (45%) and toluene (45%) the feed also contains 5% of cyclohexane as well as benzene. What would be the optimal arrangement of separation steps for distillation. Calculate from the given data the relative volatility for the separation of methylcyclohexane and toluene by distillation.01 0. considering the number of operations (columns). Assume that the solvents and the methylcyclohexane/toluene mixture are (almost) immiscible.5 DMSO 4 DEG 7 NMF 1.5 7 25 41 10 8 30 60 10 2 4 10 2. The same question for extraction.99 Methylcyclohexane 0.

Solution a) A sharp separation of the olefin/paraffin fraction from the vent gas is required.05 0.5 mol% mol% mol% mol% 1-Butene 1-Pentene 1-Hexene 3 2 1 mol% mol% mol% The vapor pressures of the pure components are given as: C4 Vapor pressure (25 C.85 C6 0.15 (a) what separation methods are in your opinion applicable for the simultaneous olefin and paraffin recovery from the vent gas.4 o C4= 3.15 0.10 0. the less soluble component will be 1-butene.01 C5= 0.01 C6= 0.03 0.0 C5 0.0 0.10 0.1 Given The composition of the vent gas at 1 bar and 25oC: Air Butane Pentane Hexane 91 1. (e) which of the given solvents are in principle suitable (selectivity>1) for a complete separation of the olefin and paraffin fractions. cryogenic distillation and chemical adsorption (see section 12.20 C6 0.20 C6= 0.68 C5= 0.04 0.08 0. (d) what are in your eyes the two key components in order to obtain a full olefin/paraffin separation when extraction with a highly polar solvent is applied. .Fundamentals of Industrial Separations.05 0. Thoughts In this problem. absorptive and extractive separations are compared on basis of the expected selectivities as discussed in chapters 3 (absorption) and 5 (extraction).12 0.5 1. The best soluble component of the paraffin fraction will be hexane.06 0. At high flows of the vent gas. (b) The olefin and paraffin fractions have to be separated between the key components which are the most difficult separable components of both fractions. During the absorption of the olefin fraction.25 C5 0. physical absorption and cryogenic distilation seem to be the most applicable separation methods. adsorption. (c) what is the minimal required difference in affinity (activity coefficients) of the adsorbing liquid towards both key components to achieve this full olefin/paraffin separation. which is undesired as a product in the extracted olefin mixture.4).08 0. bar) 2.12 0. SOLUTIONS TO PROBLEMS 12-3 SOLUTIONS Exercise 12. The separation methods that can be used to obtain a sharp separation are physical absorption.02 C4= 0. (b) can you determine which two key components need to be separated (selectivity>1) in order to achieve a full olefin/paraffin separation.24 The distribution coefficients (concentration in solvent/concentration in feed) of the components in three solvents: NMP DMSO DEG Find C4 0.

For the three given solvents.2): Substitution gives: Selectivity = o ∞ γ1 −butene ⋅ P1−butene ∞ γ hexane o ⋅ Phexane >1 ⇒ > P1o −butene o Phexane = 3.005 0.05 = = 0.10 K bu tan e K 1−hexene 0. these selectivities were calculated and summarized in the table below.10 = = 2.00 = 15.3: K Selectivity = β 1−butene. the less polar (due to the larger molecule) – and thus less soluble – component will be 1-hexene.20 Thus.0 0. (f) The selectivity of 1-hexane compared to butane during the extraction with a solvent that has a higher selectivity for olefins can be calculated by using Eq.hexane K 1−hexene 0.12-4 SEPARATION SELECTION METHODS (c) The selectivity of the absorption of 1-butene compared to hexane is given as: ⎞ ⎛ x1−butene ⎜ y 1−butene ⎟ P1−butene Phexane ⎠ ⎝ ' = α1 Selectivity = −butene.15 = = 7. The most polar – and thus best soluble – component of the paraffin fraction will be butane. 5.hexane = 1−butene K hexane Suitable solvents are characterized by a selectivity above 1. the minimal required difference in affinity of the absorbing liquid towards the ∞ ∞ key components must be of a factor 15: γ hexane > 15 ⋅ γ 1 −butene .50 0. Solvent β1-butene.hexene = x1−butene x hexane ⎞ ⎛ x hexane ⎜ y hexane ⎟ ⎠ ⎝ ∞ o P1−butene = γ 1 − butene ⋅ P1− butene ⋅ x1−butene ∞ o Phexane = γ hexane ⋅ Phexane ⋅ x hexane ∞ γ hexane ∞ γ1 −butene with Raoults law (equation 3.02 K bu tan e Remarks not suitable NMP DMSO suitable DEG best suitable of the three given solvents . (e) During the extraction of the olefin fraction.05 K bu tan e K 1−hexene 0.00 0.

(c) which of the given solvents might be feasible to make extraction economically attractive.6: o γ M PM γ with the enhancement factor = M ⋅ γT Po γT T ' αM .01 Cyclohexane 0.2 Given The vapor pressures of the pure components are given as: Benzene Vapor pressures (80oC. What distillative separation might become problematic and why? (e) which of the arrangements seems. The calculated enhancement factors and separation factors (α’M. extractive distillation (chapter 2 and 3) and extraction (chapter 5) are being discussed in this problem on basis of the enhancement of the selectivities when different solvents are being used.99 Methylcyclohexane 0.5 Cyclohexane 7 25 41 10 Methylcyclohexane 8 30 60 10 Toluene 2 4 10 2.T = The relative volatility will be enhanced with increasing enhancement factor.T = o PM o PT = 0.39 (b) The relative volatility for non-ideal mixtures is given by Eq.39 Activity coefficients at infinite dilution: Benzene MP DMSO DEG NMF 1. the most economical solution.T) are summarized in the following table: .Fundamentals of Industrial Separations. 1. Solution (a) The relative volatility for ideal mixtures is given by Eq. bar) 1.38 0. (d) which three arrangements of separation steps would be optimal when distillation.54 Toluene 0.5 4 7 1. 1.5: α M .5 Find (a) calculate the relative volatility for the separation of methylcyclohexane (MCH) and toluene (T) by distllation. (b) which of the given solvents might be feasible to enhance the relative volatility to make extractive distillation economically attractive. extractive distillation or extraction is chosen as the first step to separate this mixture into its four pure components. considering the number of operations (columns). (f) why is counting of the number of operations sufficient to get a first impression about the most economical route? What effects are not taken into account? Thoughts Distillation (chapter 2).54 = 1. SOLUTIONS TO PROBLEMS 12-5 Exercise 12.

52 NMP γM 8 = =4 2 γT γ M 30 = = 7.02 0.T ⎛γM ⎜ ⎜γ ⎝ T ⎞ ⎟ ⎟ ⎠ EXTRACT ⎛γ M Assuming that ⎜ ⎜γ ⎝ T ⎞ ⎟ is constant during the extraction. However. because their enhancement factors are > 5 (see Fig.5: ⎛γ M ⎞ ⎜ γT ⎟ ⎝ ⎠ EXTRACT with the enhancement factor = = ⎛γ M ⎞ ⎜ γT ⎟ ⎝ ⎠ RAFFINATE β M . (c) The selectivity of the extraction process is given by Eq.4 DEG 8.99 (e) The distillative separation.T = 1. The distillative separation of benzene (B) from cyclohexane (CH) might become problematic due to the insufficient difference in boiling point of both components.52 DMSO will be the most economically attractive solvent of these four.T > 2 for αM.1 to 12. all solvents obey the requirement (see figure 12.4) that α’M. it may be stated ⎟ ⎠ RAFFINATE that the enhancement factor equals the factors as summarized in the table above. DMSO and DEG are economically attractive solvents.28 NMF 5. energy requirements and product stability. 5.T 5. Sepns.01 = 1. (f) Neglected are.3 on the next two pages. (d) The optimal arrangements are shown in Figs. for instance effects like the difficulties of the separations (column dimensions). The relative volatilities are almost equal: α B. 12. 12.4 in Fund. Ind.5 γT DMSO 10. .12-6 SEPARATION SELECTION METHODS Solvent Enhancement factor α’M. consisting of three columns seems the most economical solution when compared to extractive distillation and extraction.).C = o PB o PC = 1. because the economical enhancement factor for DMSO is the largest.38. 5 4 γT γM 60 = =6 10 γT γM 10 = =4 2 .

T Extractive Distillation Distillation B. MCH. T Figure 12. MCH Distillation MCH S B. SOLUTIONS TO PROBLEMS 12-7 B B.T B B.Fundamentals of Industrial Separations. Extractive distillation .CH. MCH.T Distillation MCH.1.2.S Distillation T Figure 12. Distillation CH CH.T.CH.CH Distillation CH MCH Distillation T B.

CH.T. MCH.T Extraction S B Distillation B. MCH CH Distillation S.12-8 SEPARATION SELECTION METHODS CH.S Distillation T Figure 12. Extraction . MCH Distillation MCH B.3.T B.CH.

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