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Distillation is the MOST common separation technique in chemical process industry, accounting for 90-95% of the separation operations This is why more than a half of this course is devoted to “distillation” or “column distillation”, which includes Binary-mixture distillation Multi-component distillation Extractive & azeotropic distillation Batch distillation
3.1 Distillation Cascade
Students have already been introduced to the “flash distillation” and how to perform the calculations for flash distillation
Although flash distillation is a very simple (probably “simplest”) separation technique, it produces a limited amount of separation (i.e. it cannot yield a product with a desired purity)
From the Examples in Chapter 2, it is clear that the flash distillation yields liquid and vapour phases that comprise more than one substance (i.e. the liquid and vapour streams are not pure)
In order to obtain a single-species product for each of liquid and vapour phases, a separation technique called the distillation cascade is employed; the details of this technique are as follows Let’s consider the separation of such a binary mixture as ethanol (EtOH)-water system, in which EtOH is more volatile (i.e. has a higher vapour pressure or a lower boiling temperature); thus, for this system, water a less volatile species From the flash distillation, it is evident that the vapour product contains a high concentration of more volatile species; on the other hand, the liquid product has a high concentration of less volatile component(s)
In order to produce a vapour product with a higher concentration of more volatile species, the vapour product must be condensed to liquid and, subsequently, passed through the flash column for another flash distillation
Alternatively, the vapour stream is pressurised (to yield a higher-pressure vapour stream) and then sent to another flash tank; note that the pressure of the second flash tank is higher than that of the first one
At the other end (i.e. the liquid product), in order to obtain a liquid product with a higher (or pure) concentration of less volatile species, the liquid stream is passed through an expansion
valve (to reduce its pressure) and, then, sent to another flash column, operating at a lower pressure (than the first one) Figure 3.1 illustrates the configuration of the above description, which is, in fact, the simple distillation cascade; note that the first column (or the feeding flash column) is denoted as “3” the higher-pressure column is denoted as “2” the lower-pressure column is denoted as “4” Note that a pump or a compressor is used to increase the pressure of the vapour product
1: The configuration of a simple distillation cascade The vapour product from the flash column # 2 contains an even higher concentration of more volatile component(s) 6 .V2 2 L2 Pump or Compressor V3 Feed stream L3 Expansion valve 3 V4 4 L4 Figure 3.
more higherpressure flash columns and the accompanying pumps or compressors are added on top of the flash column # 2 Likewise. more lower-pressure flash columns and the accompanying expansion valves are added to the bottom of the flash column # 4 7 . to obtain a higher concentration of less volatile species in the liquid phase.At the other end. the liquid product from the flash column # 4 has an even higher concentration of less volatile component(s) To obtain a higher concentration of more volatile species in the vapour phase.
The system that comprises the multiple flash columns with an increasing pressure from the lowest column to the highest one (or with a decreasing pressure from the top-most column to the lowest one) is called the “distillation cascade”.2. while the final liquid product.. which can be illustrated by Figure 3. P1 > P2 > P3 > P4 > P5 By using this distillation cascade. note that. e.g.g. L5. the final vapour product. in Figure 3.. V1. is very rich (or even pure) in more volatile component(s).2. is very rich (or pure) in less volatile species 8 . e.
3: The distillation cascade 9 .V1 1 L1 Pump or Compressor V2 2 V3 Feed stream L3 Expansion valve L2 3 V4 4 L4 V5 5 L5 Figure 3.
L1. V4. and V5. that.It should be noted. although we obtain the final vapour product with a very high concentration of the more volatile species and the final liquid stream containing a very high concentration of the low volatile component. not pure or contain both more and less volatile species) How could we deal/how should we do with these intermediate streams? Let’s start with the stream L2 10 . we also get the intermediate products/streams (e.) with the intermediate concentrations (i. however. L2.e..g.
in turn. comes from the vapour stream of the column # 3 (or the feeding column). which. the vapour product of the column # 4. the stream L2 can be fed back into the flash column # 3 Next. consider the stream V4.Since the stream L2 is the liquid product of the column # 2. as it is condensed once (in the flash tank # 3) and vaporised once (in the flash tank # 4). its concentration should be similar (but NOT equal) to that of the feed stream (as it is vaporised once and condensed once) Thus. its concentration should be close to that of the feed stream 11 . once again.
this stream can also be fed back to the column/tank # 3 The ways to deal with the streams L1 and V5 are in the similar manner as per the streams L2 and V4. respectively The resulting new configuration of the distillation cascade.Hence.3 Note that there are no intermediate products in the “counter-current distillation cascade” 12 . which is commonly called the “counter-current distillation cascade”. is shown in Figure 3.
V1 1 L1 V2 2 L2 V3 Feed stream 3 L3 V4 4 L4 V5 5 L5 Figure 3.3: A counter-current distillation cascade 13 .
the vapour and liquid products with very high concentrations of (or even pure) more volatile and less volatile components. the distillation cascade with each cascade operating at different pressure (but the whole system is at nearly constant temperature) is NOT practical. respectively. which are rather expensive. can be obtained Unfortunately. the effect of pressure on the vapour-liquid equilibrium is not so significant (on the contrary. as it requires a number of compressors.By using the counter-current distillation cascade. the effect of temperature on the equilibrium is rather strong) 14 . however. additionally.
while the pressure of the whole system is kept constant (or nearly constant). whereas the bottom (lower) part is concentrated with less volatile species.Hence. which boils at low temperatures. to be more practical. is proposed The principal idea of this configuration of distillation cascade is that the top (upper) part of the cascade contains high concentrations of more volatile components. the distillation cascade that operates such that the temperature of each cascade is varied. which boils at higher temperature 15 .
the operation or the design of the temperature-varying distillation cascade is as follows: 16 .Additionally. heat/energy must be provided to the system) and vapour is condensed to liquid is an exothermic process (i.e. heat/energy is released from the system) Accordingly.e. we have learned previously that the phase changes in which liquid becomes vapour is an endothermic process (i.
4) Note that the bottom product that is not vaporised is the end product. using a condenser. The top or vapour product is totally condensed. which is denoted as B. stream V6 in Figure 3. the end product is normally liquid 17 .e. and then split into 2 streams: one is the product stream. to liquid. and then fed back (as vapour) to the cascade (i. which is called the reflux and denoted as Lo The bottom product is partially vaporised. which is called the distillate and denoted as D. using a re-boiler. another one is the stream that is returned to the cascade.
The configuration of the temperature-varying counter-current distillation cascade is illustrated in Figure 3.4 Figure 3. 2007) The ratio between the reflux (Lo ) and the distillate (D ) is the reflux ratio 18 .4: The temperature-varying countercurrent distillation cascade (from “Separation Process Engineering” by Wankat.
while the liquid phase. it is evident that. is partially vaporised The condensation of the vapour phase (to liquid) provides heat required for vaporising the contacting liquid phase 19 .From Figure 3. particularly the more volatile components. especially the less volatile species (whose boiling temperature is relatively high). is partially condensed. between each stage.4. the vapour phase. the vapour and the liquid phases are in contact with each other During the contact of the liquid and the vapour phases.
this section is called the “stripping” section The practical distillation column widely used in chemical process industry is exemplified in Figure 3. resulting from the fact that the more volatile components are stripped out of the liquid phase by the rising vapour phase.With reference to the more volatile species. it is called the “enriching” or “rectifying” section Meanwhile. since the section above the feeding point is enriched with more volatile components. the section below the feeding point is concentrated with less volatile species.5 20 . hence.
5: An illustration of the distillation column (from “Separation Process Engineering” by Wankat.6 21 . 2007) The contact between the liquid and the vapour phases within each stage (which is practically called “tray”) is illustrated in Figure 3.Figure 3.
org) 22 .Figure 3.6: An illustration of the contact between the liquid and the vapour phases within each stage of the distillation column (from http://wikipedia.
as illustrated in Figure 3. in order to enhance the contact time between the liquid and the vapour phases 23 .7 Note that a weir (ที่กน) is used to control the ั้ flow rate of the liquid phase by detaining liquid to a certain level. which is one among many types of tray of the distillation column The simplest type of tray is the sieve tray.The tray shown in Figure 3. which is a metal plate with several holes.6 is called a bubble-cap tray.
Figure 3. the space between trays (or the height of each stage) varies from 2 to 48 inch (~5-135 cm) 24 . 2007) Normally.7: An illustration of a sieve tray (from “Separation Process Engineering” by Wankat.
the contact between the vapour and the liquid phases is low. thus. the vapour phase is rapidly rising through the liquid phase. the liquid phase is close to being stagnant (นิ่ง) with only small bubbles rising through it In this regime. depending on the flow rate of the rising vapour stream (gas phase): Bubble regime: the vapour flow rate is low. thus yielding a relatively high stage efficiency 25 . hence. there are 4 flow regimes.Within the distillation column. thus resulting in a low stage efficiency Foam regime: the vapour flow rate is higher (than the bubble one). which causes a good mixing between the vapour and the liquid phases.
8: An illustration of the foam regime. in which the bubbles (or the vapour phase) are rising through the stagnant foam 26 .It should be noted.9 Figure 3.8 and 3. and this phenolmenon is called “flooding” The foam regime in the distillation column can be exemplified by the foam at the top of a glass of beer in Figures 3. that if the foam is too stable or if there is too much foam. the foam may fill the gap or space between each tray. however.
9: An illustration of the thickness of the foam layer Forth regime: the vapour flow rate is even higher (than the foam one).(a) When the foam is at normal level (b) When the foam is too thick (flooding) Figure 3. and some splashing may also be observed 27 . thus causing the surface of the liquid phase to is boil violently.
which. the contact or the mixing between the liquid and the vapour phases is excellent. most of the commercial distillation columns are operated in this regime Spray regime: the vapour flow rate is very fast (too fast) until the liquid phase. thus lowering the contact time between the liquid and the vapour phase. through which the vapour is passed.In this regime. yields a low column efficiency 28 . thus resulting in a very good column efficiency Accordingly. in turn. becomes small droplets.
it contains a high amount of more volatile components On the other way around. the rising vapour phase (V ) exchanges both mass and energy (or heat) with the down-coming liquid phase (L ) k k -1 As described previously. the liquid phase flowing down from the top is a result of the con- densation of the rising vapour phase. the rising vapour phase is from the vaporisation of the liquid phase from the bottom part.Let’s get back to Figure 3. hence.6 Between each stage. it contains very higher amounts of less volatile species 29 .5 or 3.
the less vola- tile components in the vapour phase condense 30 . the boiling is an endothermic process) The heat for boiling liquid is provided by the rising vapour phase When the heat comes out of the rising vapour phase (i.e.The more volatile species in the down-coming liquid phase boil at low temperatures In order for liquid to boil. heat or energy is required (i.e. an exothermic process).
e. the net Q is 0) In addition to an exchange in heat or energy between the liquid and the vapour phases. at each stage.Normally. it is reasonable to assume that the process is adiabatic (i. the condensation of 1 mole of a less volatile component essentially provides the heat just enough for vaporising 1 mole of a more volatile component This implies that. as the latent heat of vaporisation (ความร้อนแฝงของการกลายเป็นไอ) per mole is approximately constant with reference to tempearture. mass transfer of the species also takes place 31 .
the top product contains very high concentrations of more volatile components. through the whole distillation column.The more volatile components in the down- coming liquid phase that boil and thus become vapour migrate (ย้ายไป) into the vapour phase Meanwhile. stage-by-stage. after passing. and the bottom product comprises very high concentrations of less volatile species 32 . the less volatile species in the rising vapour phase that condense and thus become liquid transfer into the liquid phase Eventually.
for a EtOH-water binary mixture. since EtOH is more volatile than water (i. while the bottom product consists of a high concentration of water In addition to the boiling point. the fraction of such 33 .For example.e. if the component (species) is more volatile. the following technique is employed From the flash distillation. we have learned that. the boiling point of EtOH is lower than that of water). the top product contains a high concentration of EtOH. when it enters the column. in order to determine which component would tend to be vapour when it enters the distillation column.
species that becomes vapour is higher than the fraction that becomes liquid. 3.1 gives æ y öV ç i÷ >1 ç ÷ çx ÷ L ç ÷ è ø i (3. Eq.1) Re-arranging Eq. 3. from Eq.3) 34 . yi xi = Ki Thus. which can be implied mathematically as follows yV > x i L i (3.2 becomes V Ki > 1 L (3.26. 2.2) but.
3 implies that. for the same V and L. the components with higher values of K i tend to be more vapour than liquid when they enter V the distillation column. 3.Eq. and the same given temperature and pressure. given that K i >1 L 35 .
the following variables are usually specified: Column pressure (which sets the equili- brium data) Feed flow rate (F ) Feed composition (z i ) Feed temperature or enthalpy or quality (i.e.3. the ratio between the mass of the vapour phase and the total mass of the feed) Reflux temperature or enthalpy (usually the reflux is a saturated liquid) 36 .2 Specifications of the Distillation Column For both design (to design a new distillation column) and operation or simulation (to operates the existing column) problems.
For the design problems. N Column diameter 37 . D and B Heating and cooling load. Lo/D Optimal feed plate B D or B xD or xB Reflux ratio Optimal feed plate B or D xB or xD QR and QC N & Nfeed Column diameter The variables that engineers have to calculate Distillate and bottom flow rates. QR and QC. xD Mole fraction of more volatile component in bottom. the specified (given) variables and the variables that engineers have to calculate for each case of problem (A–D) are summarised as follows Case A The specified variables Mole fraction of more volatile component in distillate. xB Reflux ratio. respectively Number of stages (plates).
Case C The specified variables xD and xB Boil-up ratio. V/B Optimal feed plate The variables that engineers have to calculate D and B QR and QC N & Nfeed Column diameter D Fractional recoveries of a component in distillate (FRi)D Fractional recoveries of a component in bottom (FRi)B Reflux ratio Optimal feed plate xD and xB QR and QC N & Nfeed Note that the optimal feed plate is the feed location/stage that gives the fewest number of total stages (plates) of the distillation column 38 .
the specified (given) variables and the variables that engineers have to calculate for each case (A–D) are summarised as follows Case A The specified variables N & Nfeed xD and xB Column diameter The variables that engineers have to calculate Reflux ratio B and D QR and QC Check if V > Vmax B N & Nfeed Reflux ratio xD or xB Column diameter C N & Nfeed xD or xB Column diameter (set V = a fraction Vmax) 39 xB or xD B and D QR and QC Check if V > Vmax Reflux ratio xB or xD B and D QR and QC .For the simulation problems.
Case D The specified variables N & Nfeed QR xD or xB Column diameter The variables that engineers have to calculate xB or xD B and D QR and QC Check if V > Vmax Note that Vmax is the maximum allowable amount of the volume of the vapour phase in the feed for the given temperature and pressure 40 .
the external material balances can be formulated as follows Overall mass (mole) balance F = B +D (3.3.4) Note that the bottom (or the bottom product: B ) and the distillate (D ) are both liquid 41 . the column is adiabatic).10. shown in Figure 3. is specified.3 External (Mass & Energy) Balances of the Distillation Column When the pressure of the distillation column. and with the assumption that the column is well insulated (thus.
xB. zi hF (TF) Vk+1 Vj+1 f Lj Lk-1 k N VN+1 QR LN B.10: A distillation column Species balance (for more volatile species) z i F = Bx B + Dx D (3.V1 1 V2 D.5) 42 . hD Lo. xo L1 j F.QC h1. y1. hB Figure 3. xD.
P ) reflux B 43 (3.5 can be solved simultaneously for B and D Once B and D are obtained..When x B and x D .6) Note that QC and QR are treated as the heat input. the energy balance can be carried out as follows hF F + QR + QC = hD D + hB B (3.7a) (3. sat. T .7b) (3. P hD = hD hB = hB D ( ) (x . liq.4 and 3. as well as z i and F. are specified.7c) . TF . P ) (x . Eqs 3. the enthalpy of each stream can be specified as follows hF = hF z i . the resulting sign (+ or –) indicates the direction of the heat transfer Normally.
9) . the stream V1 enters the condenser with the composition of y1 and is then condensed and separated into 2 streams: the streams D (the distillate) and Lo (the reflux) with the compositions of x D and x o .10.8) Performing a mass (mole) balance around the condenser yields V1 = D + Lo 44 (3. respectively Since there is no chemical reaction at the condenser. the composition does not change (only phase change is taken place).In Figure 3. it results in the fact that y1 = x D = x o (3.
10) Note that = reflux ratio Re-arranging Eq. 3.Dividing Eq.11 45 . 3. and D (the amount of the distillate) is obtained from solving Eqs.9 with D results in V1 D Lo D = 1+ Lo D (3. 3. the reflux ratio is known (given).4 and 3.5 Thus. the value of V1 can be computed using Eq. 3.10 gives æ Lo ö ÷ V1 = ç1 + ÷ D ç ç ÷ ç D÷ è ø (3.11) Normally.
an energy balance around the condenser can be performed as follows hV1 + QC = hD D + ho Lo 1 (3. then. from Eq.hV1 1 46 .12. it results in the fact that hD = ho (3. 3.12) Since the streams D and Lo are both liquid and has the same composition (i. Eq. 3. x D = xo ).Once V1 is obtained.14) but.9. becomes hV1 + QC = hD (D + Lo ) 1 (3.14 can be re-arranged as follows hV1 + QC = hDV1 1 QC = hDV1 . V1 = D + Lo Hence.13) Eq. 3.e.
liq. P hD and y1 = x D Accordingly. since hD < h1 . the latent heat of vaporisation of the liquid with the composition of x D at a given pressure Note that. h1 . in fact.hD is. vap. P ) 47 . meaning that it is an exothermic process (at the condenser) D D ( = h (x ) .. h1 = h1 y1. sat.h1 ) (3. sat.15) Normally..QC = V1 (hD . QC is negative.
respectively.hB ) (3. 3. and hN +1 .6) Note that.hB is the latent heat of vaporisation of the liquid with the composition of x B at a given pressure Note also that QR is positive (i. by performing similar material and energy balances around the re-boiler. the value of QR can then be calculated using Eq. the equation that can be used to compute QR is obtained as follows QR = VN +1 (hN +1 .16) where hN +1 and hB are the enthalpies of the streams VN +1 are B.6: hF F + QR + QC = hD D + hB B (3.Once QC is obtained. the heat transfer at the re-boiler is endothermic) 48 .e.
and QR Given hD = 60 kcal/kg. and the desired bottom composition (x B ) and distillate composition (x D ) are 0.000 kg/h The reflux ratio (Lo / D ) is 3. QC . counter-current. respectively Find D. hB = 90 kcal/kg.Example A steady-state.05 (weight fraction of EtOH) and 0. hF = 30 kcal/kg.0.80. operated at 1 atm. staged distillation column. B. is to be used to separate EtOH from water The feed comprises 30 wt% EtOH and the remaining water at 40 oC and has a flow rate of 10. and h1 = 330 kcal/kg 49 .
000) = (0.17) Species balance (for EtOH) z i F = Bx B + Dx D (0.8) D (3.3)(10. 3.17 and 3.05) B + (0. 667 kg/h D = 3. 333 kg/h Performing the mass balance around the condenser gives 50 .18 simultaneously yields B = 6.18) Solving Eqs.Overall balance F = B +D 10. 000 = B + D (3.
QC can then be computed using Eq.V1 = D + Lo (3.19) Combining Eqs.9 and 3.19 together yields V1 = D + (3.330) . 3.0D ) = 4. 332)(60 .9) Lo D It is given that the reflux ratio.h1 ) 51 = (13. 332 kg/h Thus.0 (3. is 3. 333) V1 = 13.0D (3. Lo = 3.15 as follows QC = V1 (hD .0 Thus. 3.0D = 4.
3.6: hF F + QR + QC = hD D + hB B (3. 333) + (90)(6.8 is 60 . 600. 599. 000) .(30)(10. 640) QR = 4.(-3. 640 » -3. 000 kcal/h Note that the latent heat of vaporisation of liquid with x EtOH = 0. QR can be calculated using Eq.hF F .000 kcal/h 52 . 650 kcal/h » 4. 667 ) . 599.QC = -3.330 = 270 kcal/h Eventually.QC = (60)(3. 099.6) as follows QR = hD D + hB B .100.