University of Jordan Faculty of Science & Technology Department of Chemical Engineering

Chemical Engineering Laboratory III

"Distillation Column"

Date of Performing Date of submission

: :

4/4/2005 19/4/2005

"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:
13 Summary

2-

Introduction.. 4

36

Theory..

4- Equipment 11

5- Procedure. 13

6-

Results.. 15

7-

Discussion of Results 20

8-

Conclusion 22

9-

Nomenclature 23

10- References 24

11- Appendices 25

Summary:

The Distillation Column is an apparatus which separates two substances with difference in their relative volatilities. This separation process is studied by varying the reflux ratio between the reflux stream and the product stream, and so the composition of the distillate coming out also varies. Also the number of stages loaded inside the column affects the performance of the separation process, and so the efficiency of each plate or stage loaded, which is called "murphee plate efficiency". Equilibrium relations besides two methods: McCabe & Thiele and Panchon & Savarit methods; were used to obtain the Theoretical Number of stages required. As a main results, The Distillate composition (with higher volatility material) rises with the reflux ratio. Theoretical number of stages was unable to be calculated with neither of the two methods

Introduction:

Distillation is an operation whereby the vaporization of a liquid mixture yields a vapor phase containing more than one component, and it is desired to recover one or more of these components in a pure state. Or in another way, 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, by the application and removal of heat.

Distillation columns are classified on the basis of how they're operated, so they classify into: Batch columns & Continuous columns.

Our experiment is carried under Continuous column section, which can be further classified according to:
the nature of the feed that they are processing, binary column - feed contains only two components multi-component column - feed contains more than two components the number of product streams they have multi-product column - column has more than two product streams where the extra feed exits when it is used to help with the separation, extractive distillation - where the extra feed appears in the bottom product stream azeotropic distillation - where the extra feed appears at the top product stream the type of column internals tray column - where trays of various designs are used to hold up the
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liquid to provide better contact between vapor and liquid, hence better separation packed column - where instead of trays, 'packings' are used to enhance contact between vapor and liquid

This experiment is done to: 1. Demonstrate the effect of variation of reflux ratio upon distillate composition, which is the composition of the desired product. 2. Determine the number of theoretical plates within the column using the methods of McCabe-Thiele & PanchonSavarit. 3. Find the murphee plate efficiency of one plate,

Theory:

Separation of components from a liquid mixture via distillation depends on the differences in boiling points of the individual components. Also, depending on the concentrations of the components present, the liquid mixture will have different boiling point characteristics. 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. 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, 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:
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F xF = D xD + W xW The vapor form the top tray having a composition y1 passes to the condenser, where it's condensed so that the resulting liquid is at the boiling point. The reflux stream L and distillate D have the same composition, so y1 = xD. Since equimolal overflow is assumed, L1 = L2 = Ln and V1 = V2 = Vn = Vn+1. 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, 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 ,

with the upper equation gives:

y n +1 =

x R xn + D R +1 R +1

2) Ponchon-Savarit Method: This method, it obviates the need for the constant phase-ratio flow assumptions.

Start numbering the stages from the top as n, stage n-1 of the column shown in fig (a) is a mixing device where streams Ln,Vn-2 enter and the equilibrated streams Vn-1, Ln-1 leave.

The vapor Vn-2 and liquid Ln are mixed to give overall composition z, 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 ponchon diagram embodies both enthalpy and material balance relationships as well as phase equilibrium conditions. Since it is unnecessary to assume constant molal overflow, the calculations can be done on per mole or per pound basis. 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
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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

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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 0.5ft.2 Product cooler: 40mm dia x 0.2ft.2 Boiler: 150mm dia x 0.5ft.2 (steam) Reflux control: Variable area flow meters infinitely variable Safety: Graphite rupture discs, element temperature sensor, zener barriers (intrinsically safe electricals) Water: Control valve, flowmeter, pressure gauge, two temperature indicators Vacuum: Control valve, pressure gauge Steam: Reducer, control valve, pressure gauge Process: Reflux controller, fifteen temperature indicators

The major components with their duties are:

1.

A vertical shell where the separation of liquid components is carried out. Column internals trays/plates which are used to enhance component separations. 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.

3.

4.

5.

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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 should not exceed 2 bars Open slowly the steam inlet valve and also the (steam trap by-

pass). The pressure of steam should not exceed 1.5 bar. 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, open the

valve that leads to the flowmeters. The condensed product leaves the column and passes into an

infinitely variable reflux ratio controller incorporating variable area flowmeters.

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Calibration of the flow rate should be done by the flowmeter

controllers. When done, adjusting the flowrate of the Product stream. Taking the temperature readings across the column, and the

flowrate of the reflux stream. 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, which allows product removal while operating under vacuum, or back to the boiler. Vapor and liquid compositions throughout are determined by

temperature measurement. Repeating the experiment for different reflux ratios.

15

Results:

Table (4): Rotameter reading and the actual reading. Reflux Rotameter reading 3.75 3.20 2.20 2.00 1.70 Actual reading ml/min 65.35 57.76 43.96 41.20 37.06 Product rotameter reading 1.00 1.20 1.60 2.00 2.40 Actual reading ml/min 27.403 30.1628 35.6824 41.202 46.7216

Table(5): reflux ratio vs. composition of distillate reflux ratio 2.385 1.915 1.232 1.000 0.793 xD 0.980 0.960 0.915 0.835 0.790

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70
17

18

19

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Discussion of Results:

It's apparent that the relation between the rotameter scale readings and the actual flowrate is a direct linear relation, and of course it should be that, because the utility of the rotameter will be much better and easier for the user to calculate by interpolation the flowrate of the streams; than if it was non linear.
In fig (5), the relation of the Reflux Ratio and the distillate composition is direct. And that is logically correct, because, when the reflux ratio is high; it means that the reflux flowrate that goes back to the column will go for further separation through the stages, and so for further concentrating for the distillate and the bottom streams, which is desirable and more profitable with the product distillate stream to be high concentrated. And that is the target of the experiment.

when using the McCabe-Thiele method to get the number of theoretical stages, the result was infinity; which is unbelievable, 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, and the following effects may occur:
o

Foaming Foaming refers to the expansion of liquid due to passage of vapor or gas. Although it provides high interfacial liquid-vapor contact, excessive foaming often leads to liquid buildup on trays. In some cases, foaming may be so bad that the foam mixes with liquid on the tray above. Whether foaming will occur depends primarily on physical properties of the liquid mixtures, but is sometimes due to tray designs and condition. Whatever the cause, separation efficiency is always reduced.

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Entrainment Entrainment refers to the liquid carried by vapor up to the tray above and is again caused by high vapor flow rates. It is detrimental because tray efficiency is reduced: lower volatile material is carried to a plate holding liquid of higher volatility. It could also contaminate high purity distillate. Excessive entrainment can lead to flooding.

Flooding Flooding is brought about by excessive vapor flow, causing liquid to be entrained in the vapor up the column. The increased pressure from excessive vapor also backs up the liquid in the downcomer, causing an increase in liquid holdup on the plate above. Depending on the degree of flooding, the maximum capacity of the column may be severely reduced. Flooding is detected by sharp increases in column differential pressure and significant decrease in separation efficiency.

Also the effects will hit the Panchon-Savarit method when calculating the theoretical number of stages in the same way. Due to these effect the efficiency of the plate will by undetermined, because the temperature of the liquid and the vapor above the stage will be the same, 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.

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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

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References:

1.

" Equilibrium-Stage Separation Operations in Chemical Engineering"_ Ernest J.Henley & J.D.seader ,unknown edition, John Wiley " Transport Processes and Unit Operations" _ Christie J.Geankoplis, Third Edition, 1993, PTR PH " Unit Operations of Chemical Engineering" _ McCabe & Smith & Harriott, sixth edition, 2001, McGraw-Hill

2. 3.

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Appendices: _ Sample of Calculations:

Trial no. 3 will be chosen as a sample:

From the given data, table no.(1) of rotameter, reading its actual flow rate, fig(1) is drawn; with an equation:
y = 13 .799 ( x ) +13 .604

By interpolation, the actual flow rates of obtained rotameter readings are gathered. Rotameter reading for Reflux = 2.2 Rotameter reading for product = 1.6 Actual flow rate for Reflux = y Act (1) = x = x
rota (1) rota (2)

Actual flow rate for Product = y Act (2)

= 13.799(2.2) + 13.604 l in = 43.96 m m = 13.799(1.6) + 13.604 l in = 35.68 m m

And so fig (1') is generated The reflux ratio:

R= reflux product flow rate flow rate

43.96 35.68 R =1.232 R=

from the T-x-y diagram , fig(2), arbitrarily X (mole fraction of methanol in liquid) values are chosen from the x-axis, going vertically from there, till hitting the liquid saturation curve, then
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going vertically to the right till hitting the saturated vapor cure; after that moving downward to the x-axis to read the value of Y (mole fraction of methanol in vapor)

The Xn, Yn data form the x-y equilibrium curve, fig (3). To calculate XD (the composition of the distillate @ the top of the column); the T-x-y diagram is used. Locate the temperature of the top of tower;(which is for the vapor phase) at the y-axis; the temperature is 68oC, then going horizontally till the saturated vapor curve , and then vertically tot eh x-axis to read XD = Yn = 0.915 To calculate XB (the composition of the bottom vapor in the tower), the same procedure is taken as above @ T= 92oC, XB = 0.217

o Using McCabe-Thiele Method:_

The operating line equation is

y n +1 =
y n +1 =

1.232 0.915 xn + 1.232 +1 1.232 +1

R x xn + D R +1 R +1

y n +1 = 0.55197 xn + 0.41

Drawing the operating line from the 45o reference line @ XD=Yn=0.915 till the y-axis by setting Xn=0 on the operating line equation.
yn + 1

= 0.41

As the feed stream is from the bottom and is a saturated vapor, the q-line starts from the 45o line @ XB = 0.217 then horizontally going to the y-axis.
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Starting drawing horizontally from 45o line @ XD till the equilibrium line @ (Vn, Ln) ; then going vertically till the operating line @ (Ln, Vn-1), and so on in the same way till reaching XB or step off it. The number of triangles made between the equilibrium line & the operating line are the Theoretical no. of stages required. As shown in fig (3); the theoretical no. of stages is infinity .

o Using Panchon - Savarit method: From the given data in table (4); the enthalpy diagram for methanol-water system is drawn; fig (4).

To get the Theoretical no. of stages ; locate the composition of the distillate & bottom @ the x-axis, going upward vertically from XD; the distance between the saturated liquid & vapor curves is [a]; the distance from the saturated vapor till an unknown point [ D] is [b]. From lever Rule; the distance ratio a/b = R = L/D, R is 1.232, [a] is measured by a ruler to be 4.4cm, so b = a*R = 4.4*1.232= 4.928cm. Locating [ D] from the saturated vapor curve by a distance 4.928cm. [a]: represents the distillate flow rate at the top of the column. [b]: represents the liquid flow rate.

Starting at point (Vn) on fig(4) and using the equilibrium curve fig(2), we get Ln @ Xn=0.72 on the saturated liquid curve; from this pint going on a straight line toward [ D]; when crossing the saturated vapor curve; Vn-1 is located @ Yn-1.

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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); these tie lines indicate the Theoretical no. of stages required.

It's obviously seen that also the Theoretical number of stages is .

o

The Murphee plate efficiency:

Ev = yn yn1 *100% * yn yn1

0.195 0.217 *100 % 0.217 0.217

=
Given Data:
Table(1): Calibration curve data: RI/(B+1A) 0.8 1.1 1.2 1.5 1.9 2.6 3 flow rate mL/min 25.7 28 30.5 35.1 37.2 50.1 55.6

Table(2): Equilibrium data xM 0 29 yM 0

0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

0.26 0.45 0.62 0.72 0.803 0.871 0.916 0.95 0.984 1

Table(3): Enthalpy data for methanol/water mixture HL KJ/g.mole 6.061 5.267 4.723 4.389 4.138 3.929 3.846 3.804 3.804 3.804 3.804 3.816 3.887 3.954 x 0.00 0.05 0.10 0.15 0.20 0.30 0.40 0.50 0.60 0.70 0.80 0.90 0.95 1.00 y 0.000 0.273 0.418 0.517 0.579 0.665 0.729 0.779 0.825 0.870 0.915 0.958 0.979 1.000 HV KJ/g.mole 47.625 45.144 43.681 42.678 42.009 41.089 40.379 39.835 39.334 38.832 38.331 37.871 37.620 37.453

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60
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