Experiment: Reactive Distillation Column

Abstract

Reactive distillation column used to separate a mixture in continuous process. This

experiment used the distillation column to separate mixture of 0.3 mol of Ethanol
and 0.7 mol of water. Using the Refractometer to identify the refractive index of the
solution and the McCabe-Thiele’s method, the number of theoretical and actual
number of trays able to be identified. The actual number of trays required for the
solution is 5.8 trays and one reboiler respectively. The overall efficiency of the
distillation column is 58%. The theoretical trays that required for the distillation is 5.7
trays and one reboiler with the overall efficiency of 57%. This experiment can be
improved by repeating the experiment by several times in order to get the average
values which are nearer to the theoretical data.

1.0 Introduction

Distillation is a method for separating the various components of a liquid solution which
depends on the distribution of these components between a vapor phase and a liquid
phase. In the distillation process, all the components are present in the two phases, vapor
phase going up and liquid phase going down. The vapor phase is formed by vaporization of
the liquid phase at the boiling point of the corresponding component. For a binary system,
the more different the boiling points of the two substances, the more complete the
separation will be and the better separated product we will get.
Distillation is widely used in industrial production in the case of miscible liquids. For
instance, in the mixture of alcohol and water, we use the different volatilization of alcohol
and water to improve the purity of alcohol and other operations. And another important
application in industry is the separation in petroleum industries, which is almost the most
complicated distillation process.

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 Figure 1: FractionaliDistillation ofiCrudeiOil

Continuous distillation is a good choice to separate a mixture, the mixture fed into
distillation column and then separated product are exclude continuously as outcome. The
top section and bottom section are divided by feed tray. The reboiler will collect the feed in
liquid phase, which is flowing down to the bottom, and the condenser will cool the feed in
vapor phase, which is traveling up to the top. Finally, the liquid from the condenser is
removed from the system, which is called as the distillate or top product.
A mixture is separated by distillation process, it is true that between the composition of
boiling liquid mixture and vapor mixture, liquid and vapor from either tray are in
equilibrium. So, for an ideal liquid mixture with a low-pressure vapor at a given
temperature, the partial pressure of any species will be equal to the vapor pressure of the
species in the pure state multiplied by its mole fraction in the liquid mixture for an ideal
mixture, which is known from Raoult’s law (Geankoplis, 2014). According to Dalton’s law
which states that the total pressure of a gas mixture equals the sum of the partial pressures
of gases that make up the mixture. So, for a component i,
Psat
i
y i=x i (Eq.1)
P
If it is non-ideal situation, there are additional terms to modify the [Eq.1]:
γ i Psat
i
∅ i y i=x i (Eq.2)
P
Where γ i is known as activity coefficient and should be calculated using the two-parameter
Margules modle.

2.0 Objectives
2.1 To carryiout the vapour-liquid separationiprocess using a reactiveidistillationicolumn
(Bubble Cap Tray type).

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 2.2 Toiexamine the sampleifor the distillate and bottom product by usingiRefractometer.
2.3 To identifyithe number of theoreticalitrays withiMcCabe-Thiele method.

3.0 Methods
3.1 Pre-experiment 1: Refractive Index (RI) vs Composition
1. A set of mixturesacontaining ethanolaand waterawas prepared within a
specificirange of compositionibetween pure wateriand pureiethanol.
2. The refractiveaindex (RI) readings for each set ofamixture was obtained using a
refractometer.
3. A plot of refractive index (RI) againstiethanol mole fraction wasiprepared for the
whole range ofimixtures.

3.2 Pre-experiment 2: Pump Flowrate vs Pot.Post

1. A calibrationicurve for the refluxipump and dischargeipump flowiwas prepared by
the following data:

Figure 2: Data Used To PrepareiCalibrationiCurve for Pump.

3.3 Experiment 1: Continuous Distillation with Bubble Cap Tray Column
1. Theiequipment was switchedion by followed the GeneraliOperatingiProcedures.
2. The valve was setiaccording to the Table 1 foriTray columniexperiments.

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3. V12 was closed.
4. The Feedstocki2itank was filled with 5 litres ofiethanol and water mixture (0.7
v/v)*.
5. A sampleawas taken from theainitial feed and the ethanolaconcentration was
measurediusingiRefractometer.
6. Theifeed temperature setpoint, SV was set to 60°C.
7. Pump 2iwas turned on atia maximumiflowrate and the feediwas sent into the tray
columniuntil theiliquid level in the reboileririse higherithan the electricaliheater
and theilevel switchiindicating light changed toiorange.
8. Pump 2iwas stoppediand the V2 and V13 were closed.
9. Theireboiler heater was started, and theitemperature set pointiwas set to 70°C.
10. The time isiallowed toiwait until the vapourireached to the topiof the column and
liquidistarted to accumulate in theirefluxidrum.
11. Data wasistarted toirecord at the intervalsiof 5 minutes.
12. V2iwasiopenediand Pump 2iwasistartediati30 ml/min.
13. Theilevel ofireflux drum wasimonitored. The refluxipump was turnedion when the
refluxidrum levelireached to half. Theiflow was setiin a way toimaintain the liquid
level in the refluxidrumiconstant at half. The system wasiallowed to runiunder
total refluxifor a minimumiof 10 minutes. This allowedithe upperisections of
theicolumn was sufficientlyiheated and reachedito theisteady state.
14. V13iwas opened afterithe initialiheating period.
15. The refluxiratio was setito 2 by adjustingithe refluxiand discharge pumpiflowrate
to a properivalue. Reflux ratioiis defined as theiratio of theiliquid amountireturned
to the columnirelative to theiliquid removedias product.
16. V14iwas openedato produceathe bottom product from theacolumn. Flowrateaof
bottom productishould be set in a way to prevent accumulation of chemical in the
column.
17. Samplesiof the top and bottomiproducts wereitaken and analysediby using the
Refractometerievery 5 minutes.
18. The processiparameters and temperaturesiwere monitored.
19. The process wasiallowed to runiuntil steady state, the productsiin the topiproduct
tank andibottom productitank were accumulated.

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 20. Theidata was noticollected when the topiand bottomiproduct reachedisteady
state.
21. Pumpi2 and DosingiPump were stopped. V1 and V5 wereiclosed.
22. GeneraliShut-downiproceduresiwere performed.

3.4 Result Analysis

1. A table wasiprepared to tabulateidata foristeady-state condition.
2. A x-y equilibriumidiagram foriethanol-waterisystem wasiused and markedithe top
and bottomicomposition foristeady-state condition.
3. The theoreticalanumber of platesacorresponding to theaexperimental top and
bottomiproduct compositioniwas determinediusing theiMcCabe-Thiele method.
4. The topianditrays concentrationiwasifound by using theaMcCabe-Thieleamethod
andiexperimental resultsiwere compared with theicalculation.
5. The actualinumber of trays wasicompared with the theoreticalinumberiof stages
by McCabe-Thieleimethod to estimateithe efficiencyiof the distillation column.

4.0 Results
Table 1: Relationship for composition of ethanol and refractive index (RI)

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 Figure 1.1: Graph of RI vs x

Figure 1.2: T-x-y graph for ethanol in water

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 Table 2: Experimental data for distillate and bottoms

Sample Calculations
 5 litres of ethanol-water mixture: 1.5L of ethanol and 3.5L of water
For the Feed: Refractive index (RI):1.3495
By using the equation from the graph, y=−0.0312 x 2 +0.0619 x+1.3321
 Compositions: At the top: xD = 0.752
At the feed: xF = 0.30
At the bottom: xB = 0.0396
 Using the feed line equation for subcooled liquid,
C❑ p , L (T b−T F )
q=1+ (Eq. 3)
λ

0.143(78.4−60)
q=1+ 3
=1
39× 10
 Feed line equation,
Slope ¿−q /(1−q) = ∞
 Rectifying Operating Line (ROL)
Using the ROL equation,
R xD 2 0.752
y n+ 1= xn + = x n+
R+1 R+1 2+ 1 2+ 1
y n+ 1=0.667 x n+ 0.251

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 Figure 1.3: Graph for determining the number of theoretical trays required

Number of theoretical trays required: 5.7 trays + 1 reboiler

5.7
Overall Efficiency of the distillation column: ×100=57 %
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Table 3: x and y data for real ethanol-water mixture

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Sample Calculations
At 95.5°C, the vapor pressures of ethanol and water are calculated using the Antoine
equation.
B 1554.3
For ethanol, Psat 1=10( A− T +C ) =10(8.04494− 95.5+222.65 )=1443.805 mmHg
B 1668.21
For water, Psat 2=10( A− T +C ) =10(7.96681− 95.5+228 )=645.737 mmHg

Using modified Raoult’s law: Ptot =x 1 γ 1 Psat 1+ x2 γ 2 P sat2 (1)

Using equations for two parameter Margules Model:
ln γ 1=x 22 ( A 12+ 2 ( A 21−A 12 ) x 1 ) (2)

ln γ 2=x 21 ( A 21+ 2 ( A 12−A 21 ) x 2 ) (3)

Combining (2) and (3) into (1) with data at 95.5°C gives,
2 2
x 1 (0.3781+0.6134 (1− x1 ))
760=1443.805 x 1 e( 1−x ) (0.6848−0.6134 x )¿ ¿+645.737 ( 1−x 1 ) e
1 1

x 1=0.058 , x 2=0.942 , γ 1=1.778 , γ 2=1.003

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 Figure 1.4: Graph for determining the number of actual trays required for real mixture

Number of actual trays required: 5.8 trays + 1 reboiler

5.8
Overall Efficiency of the distillation column: ×100=58 %
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5.0 Discussions
For our experiment, a mixture of ethanol and water was prepared as the feed at fixed
composition. There were some preparations before the actual reactive distillation took
place. Firstly, the mixture of liquid was pumped to the reboiler until approximately half the
reboiler was filled. Next, the reboiler was started to generate vapour, which would then be
condensed into liquid to fill up the reflux drum.

A refractometer was used to calculate the refractive index of the mixture of ethanol and
water which consisted of different composition. The purpose of the refractive index being
obtained was to find out the mole fraction of ethanol.

From figure 1, the value of refractive index , RI, increases as the composition of ethanol
increases. This shows a direct proportionality between RI and ethanol composition. Based
on table 2, as time passes, the RI for the distillate composition, x D and the bottom

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composition, xB show very minor decrease while both xD and xB gradually decrease. There
were some errors associated with the readings taken from the refractometer.

Moving on, after performing several calculations as proposed in the sample calculation part,
figure 3 was obtained. From the plot, the number of theoretical trays that were required to
perform the distillation of ethanol and water mixture was calculated to be 5.7, with addition
of 1 reboiler and the approximate efficiency of the reactive distillation column was about
57%.

Comparing table 1 and table 2, the RI values do not seem to have similar properties. This is
because the RI values in table 1 were directly obtained by using refractometer with varying
ethanol compositions from which were not involved in distillation. Whereas for table 2, the
RI values were obtained using refractometer but involving the distillate with composition of
xD and bottom product of composition x B which were both products of the reactive
distillation. As mentioned earlier, RI values in table 1 showed gradual increment as
composition of ethanol increased, however RI values in table 2 did not show obvious
deterioration as the composition of ethanol decreased. This might due to the errors
associated with the refractometer device. Also, the temperature in the reboiler and
distillate was not constant with time.

Other than that, as time passed, the composition of distillate and bottom , x D and xB did not
decrease steadily, instead they were kind of fluctuating. This caused the reading of RI to not
show obvious changes. And the reason as to why this occurs is probably due to the
approximation of the feed concentration. The efficiency was improved with the inclusion of
the activity coefficient in the Raoult’s law and subsequently plotting McCabe Thiele diagram
using the results gave an efficiency of 58%.

6.0 Conclusion
Objectives of the experiment had achieved where the reactive distillation column used
to undergo vapour-liquid equilibrium and the Refractometer used to identify the refractive
index of the solution. The solution of 0.3 mol of ethanol in 0.7 mol of water being separate
in the reactive distillate column and the mole fraction of distillate and the bottom product
are 0.752 and 0.0356 respectively. By using the McCabe-Thiele’s method the actual stages
or trays that required for this experiment is determined which is 5.8 trays and one reboiler

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while the theoretical trays required is 5.7 trays and one reboiler. The identified overall
efficiency of the distillation column is 58% while the theoretical overall efficiency of the
distillation column is 57%. The accuracy of this experiment can be improved by repeating it
for several times and taking the average reading. It is also recommended to test the
Refractometer before using it. Last but not the least, the solution level of the reflux drum
needs to be considered from time to time.

7.0 References
Geankoplis, C.J. (2014). Transport Processes and Unit Operations (4 th Eds). Prentice-
Hall.

Appendices
1. The apparatus set-up

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2. General Operating Procedures
1. Switch ON the equipment’s electrical panel power switch

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 2. Boot up the PC and run the DAQ software.
3. During the start-up, insert the maximum feed flowrate for Pump 2at 250mol/min.
4. Once the liquid level in the reboiler is at adequate level which is above the heater,
turn off the pump first to allow reboiler preheating. (Level switch indicating light
change to orange color means level is high, green color means low level).
5. Set the reboiler heating temperature based on the heater power percentage.

3. General Shut-down Procedures

1. Stop the reboiler heater (adjust heater power to 0%) and the feedback pre-heater
(adjust heating temperature SV to 0°C).
2. Stop running the software.
3. If there are still remaining solution inside the buffer tank and tray, run the reflux
pump and discharge pump at maximum until the solution is fully drain.
4. Drain out all the remaining solution in the feedback tank at the bottom section
(V9), inside the reboiler (V14), in the top product tank and inside the preheater
tank (V17).
5. Stop the refrigeration chiller.
6. Shut down the software and PC.
7. Switch off electrical power source.

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