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Chemical Engineering Laboratory III
Date of Performing Date of submission
"This report is made due to the request of chemical Engineering Department to study the effects of varying the reflux ratio on the Distillation Column efficiency"
Table of Contents:
4- Equipment…………………………………………………………… 11
5- Procedure……………………………………………………………. 13
Discussion of Results………………………………………………… 20
10- References…………………………………………………………… 24
11- Appendices…………………………………………………………… 25
This separation process is studied by varying the reflux ratio between the reflux stream and the product stream. The Distillate composition (with higher volatility material) rises with the reflux ratio. Equilibrium relations besides two methods: McCabe & Thiele and Panchon & Savarit methods. were used to obtain the Theoretical Number of stages required.Summary: The Distillation Column is an apparatus which separates two substances with difference in their relative volatilities. Also the number of stages loaded inside the column affects the performance of the separation process. which is called "murphee plate efficiency". and so the efficiency of each plate or stage loaded. As a main results. and so the composition of the distillate coming out also varies. Theoretical number of stages was unable to be calculated with neither of the two methods… 4 .
Our experiment is carried under Continuous column section.feed contains more than two components • the number of product streams they have multi-product column .where the extra feed appears in the bottom product stream azeotropic distillation .Introduction: Distillation is an operation whereby the vaporization of a liquid mixture yields a vapor phase containing more than one component. extractive distillation . binary column .column has more than two product streams • where the extra feed exits when it is used to help with the separation. it's a process in which a liquid or vapor mixture of two or more substances is separated into its component fractions of desired purity. Or in another way. which can be further classified according to: • the nature of the feed that they are processing. so they classify into: Batch columns & Continuous columns.where trays of various designs are used to hold up the 5 .where the extra feed appears at the top product stream • the type of column internals tray column . Distillation columns are classified on the basis of how they're operated. and it is desired to recover one or more of these components in a pure state. by the application and removal of heat.feed contains only two components multi-component column .
2.where instead of trays. 'packings' are used to enhance contact between vapor and liquid This experiment is done to: 1. 3. hence better separation packed column . Demonstrate the effect of variation of reflux ratio upon distillate composition. which is the composition of the desired product. 6 . Find the murphee plate efficiency of one plate.liquid to provide better contact between vapor and liquid. Determine the number of theoretical plates within the column using the methods of McCabe-Thiele & PanchonSavarit.
depending on the concentrations of the components present.Theory: Separation of components from a liquid mixture via distillation depends on the differences in boiling points of the individual components. the liquid mixture will have different boiling point characteristics. and following equation are derived: An overall material balance around the entire column states that the entering feed of (F) must equal the distillate (D) plus the bottoms (W) in: F=D+W A total material balance on component (A) gives: 7 . Also. A total material balance gives: Vn+1 + Ln-1 = Vn + Ln A component balance on one material (A) gives: Vn+1 yn+1 + Ln-1 xn+1 = Vnyn + Lnxn As the feed is from the bottom of the tower. then the whole sections is considered to be enriching section. Mathematical-graphical methods for determining the number of theoretical trays or stages needed for a given separation of a binary mixture of A and B has been developed by: 1) McCabe-Thiele method: The main assumption made in this method is that there must be equimolar overflow through the tower between the feed inlet and the top tray and the feed inlet and bottom tray.
8 . with the upper equation gives: y n +1 = x R xn + D R +1 R +1 2) Ponchon-Savarit Method: This method. Making a total material balance around the upper three stages: Vn+1 = Ln + D Making a balance on component (A): Vn+1 yn+1 = Ln xn + D xD Solving for yn+1. so y1 = xD. it obviates the need for the constant phase-ratio flow assumptions.F xF = D xD + W xW The vapor form the top tray having a composition y1 passes to the condenser. Since equimolal overflow is assumed. L1 = L2 = Ln and V1 = V2 = Vn = Vn+1. The reflux stream L and distillate D have the same composition. the enriching section operating line is: y n +1 = Ln D ⋅ xD xn + V n +1 V n +1 Ln R = V n +1 R +1 Since V n +1 = Ln + D . where it's condensed so that the resulting liquid is at the boiling point.
Vn-2 enter and the equilibrated streams Vn-1. which then separates into two equilibrium vapor and liquid phases Vn-1. Ln-1 that are connected by a tie line through z. as shown in fig (b). The vapor Vn-2 and liquid Ln are mixed to give overall composition z. 9 . Ln-1 leave. stage n-1 of the column shown in fig (a) is a mixing device where streams Ln.Start numbering the stages from the top as n.
the calculations can be done on per mole or per pound basis. Since it is unnecessary to assume constant molal overflow. By making material and enthalpy balances about the portion of the enriching section of the column in fig (a) enclosed with the dotted line: For the more volatile component: Yn-2 Vn-2 = xn-1 Ln-1 + DxD Total material balance: Vn-2 = Ln-1 +D And the enthalpy balance: qD D + Hn-2 Vn-2 = hn-1 Ln-1 + hDD 10 .The ponchon diagram embodies both enthalpy and material balance relationships as well as phase equilibrium conditions.
By solving the material balance equations for Ln-1/D: L n −1 x − y n −2 = D D y n −2 − x n −1 And by simultaneous solution of the upper two equations: L n −1 ( h − q D ) − H n −2 = D D H n −2 − hn −1 Which these two equations represent the operating line for two passing streams Vn-2 and Ln-1 by the equation: ( hD − q D ) − H n −2 H − hn −1 = n −2 x D − y n −2 y n −2 − x n −1 11 .
2 (steam) Reflux control: Variable area flow meters infinitely variable Safety: Graphite rupture discs.Equipments: As shown on fig(C) : • • • • • • • • • • Bubble cap column: 1500mm x 80mm dia fitted with 8 type 316 SS bubble cap trays Condenser: 100mm dia x 0. 4. 12 . A vertical shell where the separation of liquid components is carried out.2 Boiler: 150mm dia x 0.5ft. element temperature sensor. pressure gauge Process: Reflux controller. a re-boiler to provide the necessary vaporization for the distillation process a condenser to cool and condense the vapor leaving the top of the column a reflux drum to hold the condensed vapor from the top of the column so that liquid (reflux) can be recycled back to the column 2.2ft. 3. two temperature indicators Vacuum: Control valve. zener barriers (intrinsically safe electricals) Water: Control valve. Column internals trays/plates which are used to enhance component separations.5ft.2 Product cooler: 40mm dia x 0. flowmeter. control valve. pressure gauge Steam: Reducer. pressure gauge. 5. fifteen temperature indicators The major components with their duties are: 1.
Fig(C) 13 .
Procedure: Starting the cooling water pump and slowly adjusting the flowrate of cooling water to about 4L/min on flow meter. The pressure of steam should not exceed 1. open the valve that leads to the flowmeters. 14 . Vapor generated in the re-boiler rises through the column and is condensed in a Vertical water-cooled condenser. When distillate liquid is seen on top of the column. The condensed product leaves the column and passes into an infinitely variable reflux ratio controller incorporating variable area flowmeters. The pressure should not exceed 2 bars Open slowly the steam inlet valve and also the (steam trap by- pass).5 bar.
Vapor and liquid compositions throughout are determined by temperature measurement. 15 . Calibration of the flow rate should be done by the flowmeter controllers. When done. which allows product removal while operating under vacuum. Taking the temperature readings across the column. and the flowrate of the reflux stream. or back to the boiler. Reflux is returned to the column and product passes through a cooler and graduated pipe section and can be passed either to a receiving vessel. Repeating the experiment for different reflux ratios. adjusting the flowrate of the Product stream.
7216 Table(5): reflux ratio vs. composition of distillate reflux ratio 2.1628 35.20 37.20 2.790 16 .793 xD 0.915 1.Results: Table (4): Rotameter reading and the actual reading. Reflux Rotameter reading 3.75 3.76 43.385 1.70 Actual reading ml/min 65.00 1.96 41.403 30.960 0.00 2.06 Product rotameter reading 1.40 Actual reading ml/min 27.232 1.60 2.35 57.20 1.6824 41.980 0.835 0.20 2.000 0.202 46.00 1.915 0.
70 17 .
which is desirable and more profitable with the product distillate stream to be high concentrated. separation efficiency is always reduced. because. and the following effects may occur: o Foaming Foaming refers to the expansion of liquid due to passage of vapor or gas. Whatever the cause. it means that the reflux flowrate that goes back to the column will go for further separation through the stages. but the only convincing reason for that is: when first the steam pressure if so high that cause a large amount of vapor to pass through the stages. foaming may be so bad that the foam mixes with liquid on the tray above. when using the McCabe-Thiele method to get the number of theoretical stages. because the utility of the rotameter will be much better and easier for the user to calculate by interpolation the flowrate of the streams. and so for further concentrating for the distillate and the bottom streams. the relation of the Reflux Ratio and the distillate composition is direct. than if it was non linear. 21 . Although it provides high interfacial liquid-vapor contact. but is sometimes due to tray designs and condition. and of course it should be that. which is unbelievable. In fig (5). Whether foaming will occur depends primarily on physical properties of the liquid mixtures. the result was infinity. excessive foaming often leads to liquid buildup on trays.Discussion of Results: It's apparent that the relation between the rotameter scale readings and the actual flowrate is a direct linear relation. In some cases. And that is logically correct. when the reflux ratio is high. And that is the target of the experiment.
Flooding is detected by sharp increases in column differential pressure and significant decrease in separation efficiency. The increased pressure from excessive vapor also backs up the liquid in the downcomer. Also the effects will hit the Panchon-Savarit method when calculating the theoretical number of stages in the same way. causing liquid to be entrained in the vapor up the column.o Entrainment Entrainment refers to the liquid carried by vapor up to the tray above and is again caused by high vapor flow rates. Depending on the degree of flooding. and the liquid of stage n-1 due to flooding or any other effect will approach the stage n and so differs it's really efficiency. 22 . Due to these effect the efficiency of the plate will by undetermined. the maximum capacity of the column may be severely reduced. It could also contaminate high purity distillate. It is detrimental because tray efficiency is reduced: lower volatile material is carried to a plate holding liquid of higher volatility. o Flooding Flooding is brought about by excessive vapor flow. causing an increase in liquid holdup on the plate above. Excessive entrainment can lead to flooding. because the temperature of the liquid and the vapor above the stage will be the same.
Recommendation: 23 .
Nomenclature: Em R T xD y x x rota Murphee plate efficiency in vapor terms Reflux Ratio Temperature composition of distillate @ top of column mole fraction of methanol in vapor phase mole fraction of methanol in liquid phase rotameter reading Actual flow rate composition of vapor at stage n composition of liquid at stage n the composition of the bottom vapor in the tower Composition in the hypothetical vapor phase that would be in equilibrium with liquid composition leaving the actual stage ml/min % % % Co % % % y Act Xn Yn XB y*n % 24 .
References: 1. 3. McGraw-Hill 2. sixth edition.Geankoplis.D. PTR PH " Unit Operations of Chemical Engineering" _ McCabe & Smith & Harriott.Henley & J. John Wiley " Transport Processes and Unit Operations" _ Christie J. " Equilibrium-Stage Separation Operations in Chemical Engineering"_ Ernest J.unknown edition. 1993.seader . 25 . 2001. Third Edition.
arbitrarily X (mole fraction of methanol in liquid) values are chosen from the x-axis.2 Rotameter reading for product = 1.68 m m • And so fig (1') is generated… The reflux ratio: R= reflux product flow rate flow rate 43.96 35.799(1. Rotameter reading for Reflux = 2. the actual flow rates of obtained rotameter readings are gathered.604 l in = 35. table no. reading its actual flow rate.96 m m = 13.Appendices: _ Sample of Calculations: Trial no.2) + 13.6 Actual flow rate for Reflux = y Act (1) = x = x rota (1) rota (2) Actual flow rate for Product = y Act (2) = 13. 3 will be chosen as a sample: • From the given data.68 R =1.(1) of rotameter. then 26 . fig(1) is drawn.799(2. going vertically from there.604 l in = 43.604 By interpolation. fig(2).6) + 13. till hitting the liquid saturation curve.799 ( x ) +13 .232 R= • from the T-x-y diagram . with an equation: y = 13 .
232 0. after that moving downward to the x-axis to read the value of Y (mole fraction of methanol in vapor) • • The Xn. yn + 1 = 0.232 +1 1.915 To calculate XB (the composition of the bottom vapor in the tower).217 • o Using McCabe-Thiele Method:_ The operating line equation is y n +1 = y n +1 = 1. Yn data form the x-y equilibrium curve. XB = 0. Locate the temperature of the top of tower.(which is for the vapor phase) at the y-axis. the temperature is 68oC.217 then horizontally going to the y-axis.41 Drawing the operating line from the 45o reference line @ XD=Yn=0.232 +1 R x xn + D R +1 R +1 y n +1 = 0. To calculate XD (the composition of the distillate @ the top of the column). the same procedure is taken as above @ T= 92oC.going vertically to the right till hitting the saturated vapor cure.915 till the y-axis by setting Xn=0 on the operating line equation. 27 .915 xn + 1. the q-line starts from the 45o line @ XB = 0. the T-x-y diagram is used. and then vertically tot eh x-axis to read XD = Yn = 0.55197 xn + 0. then going horizontally till the saturated vapor curve . fig (3).41 As the feed stream is from the bottom and is a saturated vapor.
the theoretical no. fig (4).928cm.Savarit method: From the given data in table (4). To get the Theoretical no. of stages required. [b]: represents the liquid flow rate. Starting drawing horizontally from 45o line @ XD till the equilibrium line @ (Vn. Locating [∆ D] from the saturated vapor curve by a distance 4. [a]: represents the distillate flow rate at the top of the column. o Using Panchon . the enthalpy diagram for methanol-water system is drawn. locate the composition of the distillate & bottom @ the x-axis. then going vertically till the operating line @ (Ln. R is 1.928cm. the distance ratio a/b = R = L/D.72 on the saturated liquid curve. Vn-1 is located @ Yn-1. from this pint going on a straight line toward [∆ D]. we get Ln @ Xn=0. From lever Rule. of stages . the distance between the saturated liquid & vapor curves is [a]. going upward vertically from XD. Ln) . [a] is measured by a ruler to be 4.232= 4. so b = a*R = 4.4*1. when crossing the saturated vapor curve. the distance from the saturated vapor till an unknown point [∆ D] is [b].4cm. of stages is infinity ∞. 28 . Starting at point (Vn) on fig(4) and using the equilibrium curve fig(2).232. As shown in fig (3). and so on in the same way till reaching XB or step off it. Vn-1). The number of triangles made between the equilibrium line & the operating line are the Theoretical no.
of stages required.217 *100 % 0.195 − 0.1 37.6 3 flow rate mL/min 25.Completing in the same way to get a number of tie lines (lines that represents the equilibrium between the two outgoing phases from a stage).217 − 0.2 1.9 2.5 1.7 28 30.5 35.217 =∞ Given Data: Table(1): Calibration curve data: RI/(B+1A) 0. It's obviously seen that also the Theoretical number of stages is ∞.2 50.6 Table(2): Equilibrium data xM 0 29 yM 0 . these tie lines indicate the Theoretical no.1 55. o The Murphee plate efficiency: Ev = yn − yn−1 *100% * yn − yn−1 = 0.1 1.8 1.
729 0.929 3.887 3.579 0.30 0.954 x 0.625 45.273 0.379 39.665 0.60 0.871 37.916 0.804 3.45 0.40 0.453 30 .418 0.267 4.620 37.10 0.70 0.95 1.723 4.05 0.984 1 Table(3): Enthalpy data for methanol/water mixture HL KJ/g.1 0.72 0.681 42.915 0.958 0.2 0.90 0.089 40.825 0.979 1.6 0.mole 6.779 0.0.9 1 0.mole 47.50 0.80 0.00 y 0.000 0.331 37.5 0.144 43.3 0.00 0.870 0.334 38.009 41.15 0.20 0.804 3.804 3.8 0.000 HV KJ/g.804 3.835 39.138 3.678 42.846 3.4 0.803 0.26 0.832 38.389 4.871 0.517 0.95 0.62 0.7 0.816 3.061 5.
60 31 .
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