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Distillation|Views: 9|Likes: 0

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https://www.scribd.com/doc/84828187/Distillation

03/10/2012

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The separation of liquid mixtures into their various components is one of the major operations in the process industries, and distillation, the most widely used method of achieving this end. In processing, the demand for purer products, coupled with the need for greater efficiency, has promoted continued research into the techniques of distillation. In engineering terms, distillation columnshave to be designed with a larger range in capacity than any other types of processing equipment, with single columns 0.3–10 m in diameter and 3–75 m in height. Designers are required to achieve the desired product quality at minimum cost and also to provide constant purity of product even though there may be variations in feed composition. A distillation unit should be considered together with its associated control system, and it DISTILLATION COLUMNS A distillation column consists of a cylindrical structure divided into sections bya series of perforated trays which permit the upward flow of vapour. The liquid reflux flows across each tray, over a weir and down a downcomer to the tray below. The vapour rising from the top tray passes to a condenser and then through a reflux drum and a reflux divider, where part is withdrawn as the overhead product D, and theremainder is returned to the top tray as reflux R. The liquid in the base of the column is frequently heated by an external reboiler. The vapour generated in the reboiler is returned to the bottom of thecolumn with a composition y , and enters the bottom tray where it is partially condensedand then revaporised to give vapour of composition y1. This operation of partial condensationof the rising vapour and partial vaporisation of the reflux liquid is repeated on eachtray. Vapour of composition ytfrom the top tray is condensed to give the top productD and the reflux R, both of the same composition yt. The feed stream is introduced onsome intermediate tray where the liquid has approximately the same composition as thefeed. The part of the column above the feed point is known as the rectifying section andthe lower portion is known as the stripping section. The vapour rising from an ideal traywill be in equilibrium with the liquid leaving, although in practice a smaller degree ofenrichment will occur.

**Methods and experimental data
**

This design is required to concentrate ethanol from a water–ethanol mixture. The pressure of the column will be designed at atmospheric pressure and the feed to the column will be saturated liquid with 20% w/w ethanol with a total mass flow rate of 20kg/sec. The distillate product must be at least 95% w/w ethanol, with no more than 1% w/w ethanol at the bottom.However distilling a water-ethanol mixture to produce such high purity ethanol has deemed difficult because the ethanol forms an azeotropewhen mixed with water. To overcome this problem, the azeotrope can be eliminatedby the addition of diaminoethanal at concentrations between 2.26 to 4.6 kmol/m3(Kumar, S. 2010). For this specific design, the distillation column is based on a binary system, and the chosen concentration of diaminoethanal is 4.6 kmol/m3. The performance of a distillation column depends on its sizing, therefore the following systems werestudied, and specifications of each of them were obtained: • • Column Insulation of the column

which assumes constant molar overflow. which applies that: • • • constant molar heat of vaporisation no heat losses no heat of mixing The molar concentrations of ethanol (Kumar. Column Reflux ratio and number of trays To determine the number of trays and the reflux ratio (R).5 in intervals of 0.1 to 1. at 4. as our actual reflux ratio dependson the minimum reflux ratio.• • • Condenser Reboiler Pump The results were analysed and the optimization parameters of the systems wereestablished. intersecting zf. The actual reflux ratio (R) was obtained by: R=fRmin Where f is a factor that was varied from 1.1 for further analysis. xd (pure liquid) and the y axis.766 was determined from this equation. were used to plot a vapor-liquid equilibrium curve. The following plots and values were obtained: f R Theoretical Actual number of . and a 45° line was added as follows: The operating line for getting Rmin was drawn. 2010).6 kmol/m3diaminoethanal. the Mcabe-Thiele graphical approach was used. S. The intercept with the y axis is equal to: xDRmin+1 Rmin = 1.

472 2. xB=0. The following equations were used to obtain B and D: F=B+D zfF=xBB+xDD The equations used to obtain Vn and Ln were: R=LnD Vn=D+Ln As there is no vapour in the feed: Vn=Vm Lm=B+Vm Giving the following vales Stream Feed Distillate Bottom Top Vapour Top Liquid Bottom Vapour Bottom Liquid Stream Label F D B Vn Ln Vm Lm Molar flow rate (mol/s) 975.number of trays trays (Theoretical number of trays / 0. T=98.1 1.5 1.1285846 299.8454106 94.4 1.71682598 881. D.295.6) 19 15 14 14 12 1. Material Balance The flow rates (F.3 1. Vm.1157365 204. The optimization of these values will be discussed later.649 11 9 8 8 7 The value of R used for designing the distillation column was 2. B.1157365 1180. Ln.3989105 299.244321 Height of the column The temperatures at the top and the bottom need to be determined.942 2. giving 14 trays.85°C which were obtained from the data table(Kumar. .2 1.295 2.Vn.0039.119 2. Lm) were determined by doing an overall material balance around the distillation column. S. At the bottom.

The volumetric flowrate (Q. The diameter (d) of the column was calculated by: d=4Q.43m.bottom=9.top=8.51kg/m3 and ρvbottom=0. The equation used to calculate the height of the distillation column was: h=2d4+2+3+n of trays0.8 m/s and Ubottom=1.88 was obtained by interpolation giving a T=81. at the top and the bottom.) was calculated by: Q. The actual vapor velocities (U) were obtained by multiplying the Um by 80%. The temperature at the top.04g/s. Heat loss without insulation The resistances were determined for the wall of the distillation column and for the air using the following: R=1UA=tλ(Am cylinder+hemisphere)+1A0 cylinder+A0 hemisphereh0 Am=Ao cylinder+Ao hemisphere-Ai cylinder+Ai hemisphereln (Ao cylinder+Ao hemisphereAi cylinder+Ai hemisphere) Acylinder=2πrH Ahemisphere=3πr28 .8m3/s and Q.52kg/m3 It was assumed that the vapors behave as ideal gases.27L-0.16m3/s.5m.047. Insulation The heat loss (Qloss) was determined without insulation. and by adding the skirt we obtained an actual d of 13.31 m/s. xD=0.72m and dbottom=2. were determinedusing Perry’s handbook data and using the following equation: 1ρl=meρe+mwρw Giving values ofρltop=742.65kg/m3.2010).πU dtop=3.09g/s and MWavbottom=20. The densities of the liquids.36m. and then the insulation was added. These MW were used in: p MWρ=RT To get ρvtop=1. The values obtained wereUmtop=1 m/s and Umbottom=1. The densities at the top and at the bottom were obtained by using the average molecular weight as follows: MWav=yBeMWe+yBwMWw Giving values ofMWavtop=44.25kg/m3 and ρlbottom=853. as a larger d gives a lower vapor velocity and prevents splashing. and using a plate spacing (L) of 0.=mρv Obtaining Q.99m were obtained. Iteration was conducted to obtain the optimum thickness of the insulation.17L2-0.63 m/s. The densities were used to get the values of the maximum vapor velocity (Um): U=Kρlρv Where K=0.5 The height without the skirt obtained was 11. The largest d was used for further calculations. The results obtained were Utop=0.83°C.

The Qloss was calculated from the equation: Qloss=ΔTR The Qloss obtained was 161.74 10.cw was obtained from: Q. The Q was used in: Q=mcwCpcwΔT To obtain mcw=230.05 15.00058 K/W.The R obtained was 0. The Q lost was 14434.5 13.67 kW.35 kJ/s.025 28.075 10. Thickness (mm) Qloss (kW) Temperature outside the distillation column with insulation (°C) 0.6 0.075 thickness because is the one with the less heat loss. it is a one time investment that will not be that high when comparing it with the operating cost throughout the years. for the wall of the insulation and for the air. and Cpcw was obtained from the Perry’s handbook. Even though it will be an expensive fixed cost. the duty (Q) needs to be calculated as follows: Q=-mmixtureΔHev mixture mmixture=methanol+mwater Where mmixture=12.cw=mcwρcw .76 kg/s and ΔHev mixture =270 kcal/kg was obtained from Perry’s handbook.85°C was used as it is the temperature at the bottom of the distillation column. Condenser For designing the condenser. For calculating the Qloss the To=5°C (winter) was assumed and Ti=98. using the following: R=1UA=tλ(Am cylinder w+hemisphere w)+tλ(Am cylinder i+hemisphere i)+1A0 cylinder+A0 hemisphereh0 The same temperatures as the Qloss without insulation were used to obtain a Qloss with insulation at different thickness values.11 20.9 0.37 kg/s where we assumed that ΔT=15°C.9 We will use the 0. different from the one without insulation due to an increase in the area by the insulation. Heat loss with insulation The resistances were determined for the wall of the distillation column. The Q.

and as we can only choose between 2. the following steps were followed.79 kJ/s.232 m3/s where the ρcw=992. Reboiler For obtaining the reboiler duty and the volumetric flow rate of steam produced.27 kW/Km2.The cooling water is entering the condenser at 20°C and leaving at 35°C. obtaining a value of 9. and a value of Q = 8950. The overall heat transfer coefficient (U0) was calculated from: 1U0=D0Di1hi+D0DiFi+D02λlnD0Di+F0+1h0 Where hi=0.64 m.44°C.8[Cpμk]0.21 kg/m3 was obtained from Perry’s handbook at 27. and the water and ethanol mixtures enters and leaves at 81. By dividing the mass flowrate of vapor entering the column we can obtain the volumetric flow rate of steam produced by the reboiler. Method 1 The optimum diameter of the pipe was calculated by: di=0.34.cw=0.37 kg/s and ΔHev mixture =100 kcal/kg was obtained from Perry’s handbook. The A0 found was 212. the selected diameter was 110 mm.)0.75°C. .232 m2. the 2. To calculate the theoretical number of tubes inside the condenser.Q.44 m and 3. as it is shown: Where F is the correction factor and it is equal to 1. the cross sectional area was calculated first: Ac=Q. The theoretical number of tubes equation used was: n=4Acπdi2 The theoretical number of tubes obtained was 1810. .3°C. As there are no pipes of this diameter available.8(Q. The duty (Q) was calculated with the same formula as the one for the condenser. From this value we can obtain the length of the tubes inside the condenser by: L=A0nπD0 The value obtained was L=2. With this in mind we calculated the ΔTm by: ΔTm=ΔT0-ΔTLlnΔT0ΔTL Obtaining a value for ΔTm =53. Pump The pressure drop of the pump was calculated my the following method.023[ρUdμ]0. Where in this case mmixture=21. The two fluids entering the condenser are in counter flow . giving a value of di=108 mm.cwU U was assumed to be 1 m/s.5 Being Q the volumetric flowrate of Vn.04 m/s was calculated.66 m. A0=QU0ΔTmF The U0 and ΔTm were used to calculate the A0.22 m3/s.4λd Finding a value of U0=1.44 m tube was selected and the actual U=1. and the Ac found was 0.

26. from literature. the accepted pipe velocity for a water-ethanol mixture is in the range of 1. Literature says it should be less than 0. Our velocity was calculated from: Ac=Q. The material chosen for the pipes was iron cash. It is said that the optimum velocity of a at a density of 800 kg/m3 should be around 2. The friction loss in the pipeline was calculated by: ΔPf=8fLρU22di The value obtained was ΔPf=3000 Pa.1 atm. The total length of the pipeline was assumed to be around 24 m.0028.5 m/s. Using Moody Diagram we extrapolated our friction fanny factor f = 0. with an absolute roughness of 0. The energy balance was conducted by: Δzg-Δpρ-ΔPfρ-W=0 W=-121. The maximum difference in elevation (z1-z2) was around 12 m. And using this work we get a pump power of 30 kW.The velocity accross the pipe was obtained next. and a relative E=2. And the pressure difference (p1-p2) was assumed to be around 0 Pa. which is an accepted value.5 to 3 m/s.6 J/kg was obtained. Also.4.98 m/s Reynolds numer was calculated using the following data: ρ=742.cwU Where: Ac=πdi24 Giving us a U of 1.25 kg/m3 and μ=5*10-4. .

We take the mole fraction of ethanol as the vapour is always more richer in the volatile component The flow rates of liquid and vapour leaving a tray are labelled asVn and Ln respectively. Were we are assuming that • • • There are no heat losses from the column The difference in temperature between adjacent trays is negligible The latent heat of the two components are equal in other words for every mole of vapour condensed.Thus theses three streams. one more flows liquid flows from that tray( they are in equilibrium) The vapour from the condenser is completely condensed so that the resulting liquid has the same compostion. the vapour leaving the top tray and the top product and the reflux all have the same composition Xd. one mole of vapour boils off and thus for every mole of liquid flowing to a tray.D= molar flow rate of the distillate B = the molar flow rate of the bottom F= feed flow rate Xd= mole fraction of liquid ethanol y= mole fraction of vapour ethanol xb= mole fraction of ethanol at the bottom xf= mole fraction of ethanol in the feed. This liquid is split to produce the top product and to provide liquid for the top tray. .

Thus the distance between the equilibrium curve and ioperating line is at its minimum. At first we need to determine the minimum reflux ratio. xb= 0.The minimum reflux conditions represent the theoretical opposite of total reflux and infinite number of ideal separation stages. As a result operation cost will increase. However. Sou you cannot step past the feed point. Therefore we need to optimise the number of trays to the heat exchanger. and therefore there s no gap between equilibrium cuvre and the intersection point.089 we can determine the Reflux ratio: R=Ln/D The reflux ratio is used to calculate the number of trays in the column by applying the Mcabe-Thiele graphical approach which assumes constant molar overflow.As the condenser at the top of the column is a total condenser the vapour flow rate is equal to the sum of the reflux and the distillate flow rate: Vn=D+Ln At the feed tray the vapour and liquids flow rates in this section are denotes as Vm and Lm this section is called the stripping section. This allows us to apply two operating lines above the feed (enrichment section): Which we can relate to Reflux by substituting Ln and Vn by the relations Ln= RD and Vn=(1+R)D Giving And below the feed (stripping section) Initially we determine minimum number of trays. . IN this case the intersection of the operating line lies on the equilibrium line. the stepping triangles become very small.88. as our actual reflux ratio will be chosen in relation to the minimum reflux ratio. • no heat losses • no heat of mixing.004 and zf= 0. Where Vm = Vn And Lm= Ln+F Determining the Number Of Trays Now that we know xd = 0. which will effect component cost. less trays means a higher reflux ratio and so a larger condenser and more reboiling. which applies that: • constant molar heat of vaporisation.

K. and • no heat of mixing. . • no heat losses.16 Kmol m^-3 Mention m q= 1 as its saturated liquid feed Results and Discussion: Optimization of reflux ratio Quantitative analysis: First we would want to explain the true physical meaning of the reflux ratio “R”. Experimental data concentration of diaminoethanal = 4. It assumes constant molar overflow and this implies that: • constant molar heat of vaporisation. 2010). and its inverse relation to the number of trays in the distillation column. The reflux ratio is fraction of condensed ethanol vapour sent back to the column to achieve total separation of the two components. l • Which lead to a constant molar vapour flow and a constant molar reflux Our VLE plot was taken from experiment date shown below (Kumar.To determine the number of trays we will apply the McCabe-Thiele graphical approach.

our R was unknown. there exist a specific number of plates that gives total separation. We must therefore evaluate the trade-off between reflux ratio R. and the minimum condenser cooling capacity. and the number of trays N. At the start. for which the total cost.Therefore. correspond to an infinite number of trays (separation is impossible at this point). and an infinite reflux ratio. the operating cost is at minimum because we are handling a minimum amount of liquid. we are increasing the purity of our distillate. such as condenser cooling water. will result in a better separation. reboiler. by increasing the reflux ratio. so we needed to calculate the Rmin and then get our reflux patio by iteration. intuitively. hence improving our process. the number of trays required start decreasing until reaching the conditions of Total reflux. The R minimum. which corresponds to the minimum number of trays needed. our reflux ratio R should correspond to the optimized. There are two components of total cost: fixed capital costs fc(such as the cost of purchasing the distillation column. Fixed capital cost: - Number of trays Size of distillation column . Increasing the number of trays. describing a return of a minimum amount of liquid to the column. This point is referred to as the pinch point. So this is the stage of the minimum reboiler heat duty. So for each reflux ratio. or the most economical. vapour steam…). Another factor affecting the quality of the separation is the number of trays used. But the fixed capital cost is at maximum due to the infinite number of trays required. condenser…) and the operating cost fo (costs associated to operating the plant. At the minimum reflux ration Rmin . So in our design. By increasing R. will be the least.

larger equipments are required. and insurance and effluent treatment Operating capital costs - Steam Cooling water Electricity NB: raw material is also included in the operating costs nut it does not vary the change in R. Now.- Size of reboiler Size of condenser Size of the pump Piping and instrumentation (tubes) Insulation Maintenance operating labor supervision plant overheads and laboratory facilities taxes. one would assume a linear continuous decrease of the fixed cost as R increase due to the decrease in the number of trays. In the first approach to analyze the trend of the fixed capital costs variation with the increase R. As R start increasing. and the duties of the reboiler and the condenser start increasing gradually with the increase of the overhead product back to the column as reflux and reboiling all bottom products. we can see . if we take a deeper look at our fixed capital cost.

taxes. Therefore. and insurance and effluent treatment - y: number of trays z: distillation column. and therefore heat loss. although y is at a minimum. fc falls into a minimum then rise again to infinity.that our fc is a function of three variables that react independently and correlates differently with fc . y decreases but our z start increasing. As for the operating cost fo . supervision. insulation. we have an infinite number of trays and a minimum duty on the heat exchanger. the effect of the cost of trays is negligible. dz >>> dy. plant overheads and laboratory facilities. These cost much more than tray does. dx≈ 0 At minimum R. so we can assume it to be constant and has no effect on our economical analysis. we would need larger heat exchangers. pump. Quantitative analysis: . we are dealing with. reboiler. it will continue to increase with increasing reflux ratio. fc = fc (x.z) - x: piping maintenance. At small values of R. larger pumps and bigger insulation to account for the larger amount of liquid. condenser x varies minimally as R increases. So the variation of fc as R increases is set by the effect of component y since it is clear that dy >>> dz As R continue increasing. So our fc starts increasing again governed by the increase of z. operating labor. At high values of R. Hence.y. fc starts decreasing due to the decrease in y (since the trend is governed by the effect of y).

4% from the total heat loss through the distillation column (heat loss through heat exchanger is 23385 kW).8 2 2.119 15 2.2 R efluxra R tio 2.6 2. We now that the highest operating cost. is that of the heat losses.295 14 2.74kW) represent 0.8 3 Next. Heat loss through insulation (10. So our operating cost of will be a function of the duty of the condenser Qc and duty of the reboiler Qr).4 2. R Actual num of trays ber 1. and we extrapolate.649 12 At R= Rmin the numbers of trays y = ∞ As R 30 28 26 24 22 20 18 16 14 ∞.472 14 2. we will analyze the effect of the varying the reflux ratio R on the operating cost fo .9426 19 2. .6 R in m 1.y Rmin s y a t f o r e b m u N 12 10 8 6 4 2 0 1.First we will plot the variation of the number of trays versus the reflux ratio.

Taking a ratio of 2Q To R1 and R2 Qc∞ D(R1+1) Qc∞ D(R2+1) Q1cQ2c=(R2+1)(R2+1) We can say that the duty of the condenser is a function of one variable. ΔHev mix Constant SoQc∞ R+1.Relationship between condenser duties and reflux ratio The duty of the condenser: Qc= -mmixtureΔHev mixture mmixture= -Vn MW Vn=D+Ln R=LnD Vn=D+RD=D(R+1) Qc=-DR+1MWΔHev mix We have D.Mw. R. Duty on the reboiler: QR= mmixtureΔHev mixture Mmixture=LmMW QR=LmMWΔHev mixture Lm=FL+Ln=FL+RD QR=F+RDMWΔHev mixture ∴=FLMW Δ Hev mixture+DMW Δ Hev mixtureR Let: A=FLMWΔHev mixture andB=DMWΔHev mixture y=a+bx Now we will take the ratio of Q1c to Q2c Q1RQ2R=F+R1DMWRΔHev reboilerF+R2DMWRΔHev reboiler Assume MWR constant (assume pure water at the bottom) Q1RQ2R=F+R1DF+R2D .

792201 5718. The reflux ratio at this minimum total cost. and that this is a linear relationship between Reflux rate (R) and the duties across the heat exchangers.1Rmin 1. we will do a rough estimation of the R optimum from data gathered.295 14 2.76845 5036.Now lets get a relation for Q1+Q (Duty across heat exchangers) QR+QC=-mC mixΔHev condenser+mR mixΔHev reboiler=-DR+1MWCΔHev condenser+(F+RD)MWRΔHev reboiler Assume: MWC=MWE MWR=MWW Set the constants A=-D MWE ΔHev ethanol B=F MWR ΔHev reboiler C=D MWR ΔHev mixture QR+QC=A+AR+B+CR=RA+C+(A+B) Set: A'=A+B C'=A+C QR+QC=A'+C'R So we can say that ΣQ is a constant for a specific reflux. R 1.544517 .5Rmin R Num of trays ber 1.3Rmin 1. is our optimum reflux ratio. Our total cost fT. fo that increases linearly with r. and fc and passes through a minimum.9426 19 2.472 14 2.203737 4358. Since we do not have enough data for an economical analysis. and the fixed capital cost trend.649 12 Qr+ Qc 3679. So now we have both of the operating cost.4Rmin 1.119 15 2. We will plot the variation of Qc+Qr versus the reflux ratio.2Rmin 1. which is the sum of the two costs.668359 6400. must therefore pass through a minimum.

Now we are left with 1.4Rmin is neglected because with the same number of trays.3Rmin.5Rmin has a real high reflux ratio. It is clearly not 1. Hence we can conclude that our optimum reflux ratio is R= 1.2Rmin and 1. if given all the data.After finding our Rmin. Since the capital cost is governed by the number of trays at this stage.1Rmin and 1. 1. and can be therefore neglected. is fitted to the following curve: .5Rmin.3Rmin has a lower reflux ratio and hence a smaller operating cost. we can say that dfcdR = 0 at R=1. the change in the capital cost to change in reflux ratio should be zero. a rule of thumb is that the optimum R is between 1.1Rmin because of the high number of trays which will lead to the high fixed cost. At a minimum. 1.3Rmin since a variation in R at this point will give the same number of trays.295 Our total cost curve versus our reflux ratio. Also. 1. Our optimized reflux ratio will correspond to the minimum on the fixed capital cost curve.3Rmin = 2.

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