Automated Distillation Pilot Plant (mod.

DCA/EV)

Addis Ababa Science and Technology

University
College of Engineering
Chemical Engineering Department
Mass Transfer Unit Operation Laboratory

Automated Distillation Pilot Plant

(mod. DCA/EV)

November 2023
 Automated Distillation Pilot Plant (mod. DCA/EV)

Table of Contents Page No

1. Experiment Name........................................................................................................................................1

2. Introduction.................................................................................................................................................1

2.1. Concentration Diagram............................................................................................................................2

3. Technical Specifications..................................................................................................................................2

4 Controller Description.................................................................................................................................4

5 Operating Instruction........................................................................................................................................5

5 Experiment..................................................................................................................................................7

5.1 Determining The Composition Of A Mixture With The Refractometric Method.......................................7

5.2 Determination Of Total Reflux (Rt)............................................................................................................8
5.3 Perform Material And Energy Balance......................................................................................................9
6 Discussion (By Student)............................................................................................................................12

7 Conclusion (By Student)...........................................................................................................................12

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1. Introduction
The multi-stage distillation is a basic unitary operation of chemical industry. The liquid-vapor separation
(L-V) is a process which has been used for many years and many are the methods and devices developed
in the meantime to obtain the balance between the phases in contact. The mass transfer increases in
proportion with the contact area between the phases and this is the reason why the devices have been
planned to obtain a maximum interface area. With constant liquid and vapor flows, the contact time
between the two phases is constant so when the contact area increases, so does the mass transfer and with
it the possibility to reach the balance of the system, which represent the 100% of efficiency. The
combination of factors as the production of contact devices, the operative conditions, the characteristics
of the system rarely take to an efficiency of the 100%. The separation process is usually carried out in
columns which consist in devices enabling the continuous or discontinuous liquid-vapor contact.
The contact can be made either using a packed column or plate column. Plate towers exhibit
larger pressure drops and liquid holdup at higher gas flow rate. While, packed towers are not appropriate
for very low liquid flow rates. Packed column is the preferred choice than a plate column to handle toxic
and flammable liquids due to lower liquid holdup to keep the unit as small as possible for the sake of
safety. Plate columns are normally suitable for fouling liquids or laden with solids. They are easier to
clean and could handle substantial temperature variation during operation. Packed towers are more
suitable for foaming and corrosive services. It is easier to make the provision for the installation of
internal cooling coils or withdrawal of side streams from a plate column.
In a continuous distillation, the system is kept in a steady state or approximate steady state.
Steady state means that quantities related to the process do not change as time passes during operation.
Such constant quantities include feed input rate, output stream rates, heating and cooling rates, reflux
ratio, and temperatures, pressures, and compositions at every point (location). Unless the process is
disturbed due to changes in feed, heating, ambient temperature, or condensing, steady state is normally
maintained. For a distillation process using a distillation column, at steady state, if the feed rate and feed
composition are kept constant, product rate and quality are also constant. However if there is change
(disturbance) to one of the variables such as, feed pre-heating temperature, reflux ratio, feeding flow rate,
reboiler heating power, feeding composition, and residual pressure the quality of the product will be
changed. For a set of variables a desired product quality can be obtained by appropriate design of a
distillation column (for example by determining the required number of plates). The desired production
rate and quality determines the amount of energy required during a distillation process.
In this laboratory work the effect of the stated variables on the top and bottom product quality
will be investigated. The theoretical number of plates will be calculated for a set of operating variables.
Energy and material will also be performed. For this study a continuous distillation pilot plant (mod.

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 Automated Distillation Pilot Plant (mod. DCA/EV)

DCA/EV) (Fig. 1) will be employed. The distillation column is completely made of glass and it consists
of a reboiler, of a column with packing of steel mesh and of a condenser with reflux valve and head. The
bottom product and the distillate are collected into two glass tanks after being cooled by two heat
exchangers. The pilot plant is equipped with two PID controllers being able to control the flow rate of
cooling water crossing the condenser, the vacuum degree of the plant and the feeding pre-heating
temperature, automatically.

Fig. 1: Continuous distillation pilot plant (mod. DCA/EV)

2. Objectives of the experiment

2.1. General objective
 To understand a continuous distillation process of binary mixture and study the effect of
distillation variables on the performance of a distillation column.
2.2. Specific objectives
 To perform energy and material balance as a function of reflux ratio and reboiler heating
power
 To determine the minimum reflux ratio and minimum number of theoretical plates for a
specified distillation process conditions

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3. Theory
3.1. Components of a distillation column
A typical Continuous Distillation Column has several components to facilitate the overall process. These
four main components are:

 Column (incorporating the enriching and stripping sections), where the liquid/gas phase
separation takes place.
 Reboiler (heat exchanger), which provides the heat energy to partially vaporize the columns input
feed (liquid) for the separation (distillation) process to take place. The input feed flows into the
center of the column and down through the stripping section to the base, before entering the
reboiler where the feed liquid is heated to generate the feed vapor (through evaporation). This
feed vapour travels up through the column by convection, to continue the feed components
separation process.
 Condenser, which cools and condenses the separated and enriched feed vapour at the top of the
column before it enters the reflux drum.
 Reflux drum, which collects the condensed feed vapour (as a liquid), and splits it into two
streams, 1. the distillation process output (distillate) and 2. the reflux drums recycled liquid
(reflux), which is fed back into the top of the column, to further enrich and purify the distillate.

Enriching
column

Depletion
column

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Fig. 2: Continuous distillation column sections

3.2. Hypothesis of the ideal condition

The following simplificative hypotheses refer to ideal binary mixtures.

 Each stage of the column corresponds to an ideal stage of the process: the liquid and the vapor
leaving each stage are in thermodynamic equilibrium.
 The column is adiabatic (there is no heat exchange with the outside).
 Reflux occurs at the boiling point.
 The molar flow rates of liquid and vapor are constant along the column.
 Molar specific heat and molar heat of vaporization do not depend on the composition.

3.3. Concentration diagram

Start studying the distillation of a binary mixture plotting the (y) vs. (x) diagram (Fig. 3). This diagram
can be plotted according to several methods (in ideal mixtures), that is:
 through the values of equilibrium - (x, y) vs. (T) - of a certain mixture;
 through Antoine equation and the application of RAOULT's and DALTON's laws (boiling
and drew-point curves);
 through the value of relative volatility of the mixture and the application of BROWN's
equation:

(1)

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Fig. 3: Isobaric concentration diagram

3.4. Calculating the number of theoretical stages

Using the simple Mc-CABE-THIELE diagram (y) vs. (x) allows calculating the number of ideal (or
theoretical) stages required to obtain ascertain fractionation of a certain mixture with a certain reflux
ratio.
3.4.1. Enriching column
Refer to the Fig. 4 (a) and consider the following balances.
a) overall balance between the plates N+1, N and the condenser:
(2)
b) balance of the weak component N+1, N and the condenser:

(3)
If the indices of the equation (3) are omitted, the result is:

(4)
Eq.3 can be rearranged as

(5)
Then substitute the Eq.2 in the formula Eq. 5 and divide by D: the result is:

(6)

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L/D is the reflux ratio (r) and Eq. 6 can be written as

Enriching column operating line (7)

Fig. 4: (a) system boundaries of material balance for enriching and depletion columns, and (b)
theoretical number of stages for enriching section using Mc-Cabe-Thiele diagram for feed at
boiling point.
3.4.2. Depletion column
Similar to the enriching column, from material balance for the depleting column (Fig 4 a) an
operating line for depleting column (Eq. 8) can be derived.

(8)
This is the operating line of the depletion column intersecting the point (yR = xR, xR)
If the slope for the operating line of the depletion column (L’/V’) is known the number of plates can
be determined graphically (Fig. 5).

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Fig.5: Mc Cabe-Thiele diagram for calculating the number of theoretical plates in the depletion
column feed at the boiling point

However, if these data are not known, the operating line of the depletion column can also be drawn
through the method of the feed line and the known degree of vaporization.
3.4.3. Feed stage considerations
In determining the operating lines for the rectifying and stripping sections we needed the bottoms and
distillate compositions and reflux and reboil ratios. The compositions can be independently specified, but
r and VR = V’/R are related to the vapor to liquid ratio in the feed

V < V’ V = VA + V’
V = V’

A A A

V’ L’ = L+LA V’
L’ > A+ L L’ = A+ L V’

V = A + V’ V > A + V’

A A

L’ = L V’ L’ < L V’
Fig. 6: Possible feed conditions

Consider the cases where the feed is not a supercooled liquid or a superheated vapor:

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Mass balance around the reboiler:

Mass balance around the condenser:

Mass balance around the column:

Vapor entering the enriching column (rectifying section):

Liquid entering the depletion column (striping column):

Substituting this into the column balance:

In other words, the vapor entering the rectifying section is the vapor entering the condenser minus the
feed vapor flow rate.
So except in the cases where the feed is a supercooled liquid or superheated vapor the boilup is related
to the reflux by the material balance:
(9)
Dividing by R gives the boilup ratio:

(10)
Distillation operations can be specified by the reflux ratio or boilup ratio although the reflux ratio (or
r/rmin) is most often specified.
3.4.4. The q line
First, we define the parameter q by:

(11)
Where; hv is molar specific temperature of feeding at its dew temperature
hA is molar specific temperature of feeding at operative conditions and
hl is molar specific temperature of feeding at its boiling (bubbling) temperature
Subtracting the two operating lines:

Gives (12)
Using a material balance in the light key component (ethanol):

Using a material balance around the feed stage to eliminate vapor flow rates:

 (13)
Simplifying and using the definition of q results in the q-line:

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the q line. (14)

At , implying the q-line has slope q/(q-1) and intercepts the 45 degree line at y = ZA

3.4.5. Operating conditions of the column

Now what explained above makes drawing the operating line of the depletion column easier. In fact this
line meets the point I of intersection of the operating line of the enriching column with the feed line (q-
line): both these lines can be determined when the following parameters: feed titer, distillate titer,
residue titer, reflux ratio, thermal condition of feed (degree of vaporization), are known the Fig. 7 shows
how these three lines can be drawn according to these parameters.

q
q 1

xD
1 r

Fig. 7: Construction Lines for McCabe-Thiele Method

3.4.6. Number of theoretical stages

The number of theoretical stages can be calculated graphically through the McCabe-Thiele diagram
(Fig. 8). Start from the upper part where the composition of the top vapor is known: y1 = xD
(hypothesis of total condensation). The composition x1 of the liquid flowing from the first plate (in
equilibrium with the vapor of the composition y1) corresponds to the abscissa of the point 1 on the
equilibrium curve of ordinate y1. The composition y2 of the vapor which crosses the liquid of the
composition x1 corresponds to the ordinate of the point of abscissa x1 on the operating line. So, the

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point 2 = (y2, x2) is determined on the equilibrium curve. Then it is possible to fix the point (y3, x3) on
the operating line and so on. The number of steps between operating lines and equilibrium curve
corresponds to the number of theoretical (or ideal) stages required to obtain a distillate of
composition xD and a residue of composition xR starting from a mixture of composition Z A with a
degree of vaporization (feed condition) and a reflux ratio r.

Fig. 8: Graphical construction of the number of theoretical plates

3.4.7. Material balance

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Refer to the Fig. 9. Generally the following data

are available:

A = flow rate of feed

ZA = feed composition

D = flow rate of distillate

xD = composition of distillate
= degree of vaporization

Fig. 9: General diagram of a distillation column

Consider these two overall material balances:

(15)
(16)

The formulae (15) and (16) are two simultaneous equations with two unknown quantities (R and χR): the solution
is easy. Furthermore, from a material balance of the condenser it is possible to get:

(17)
that is:

(18)

When V, L and the degree of vaporization are known, the flow rates V' and L' can be calculated through
the equations (10) and (11):

(19)

(20)

3.4.8. Heat balance

The fig. 10 is a symbolic representation of the heats involved in the continuous distillation. The balance

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equation states that the sum of the heat flows in inlet must be equal to the sum of the heat flows in outlet,
that is:

(21) Where:
JA = specific enthalpy of feed (cal/mol)
A = flow rate of feed (mol/h)
Qr = heat delivered by the reboiler (cal/h)
Qc = heat subtracted from the condenser (cal/h)
JD = specific enthalpy of the distillate (cal/mol)
D = flow rate of the distillate (mol/h)
JR = specific enthalpy of residue (cal/mol)
R = flow rate of residue (mol/h)

Fig. 11: Symbols of the various types of heat involved in distillation

The general equation of the heat balance (21) can be written as follows:

(22)
where:
CPA,l = molar specific heat of feed (cal/mol)
TbA = boiling point of feed (°C)
CPD,l = specific heat of the distillate (cal/mol)
CPR,l = specific heat of residue (cal/mol)
TD = temperature of distillate (°C)
TR = temperature of residue (°C)
The value of can easily be calculated from the diagram (x,y) vs. (T), through the lever method (Fig.
12):

N.B.: The reference temperature for enthalphies is 0 °C.

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Fig. 12: Determination of for a temperature TA and a composition Z

The next paragraphs explain how the various terms of the Eq. 22 can be expressed versus the operating
data and conditions of the plant.

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4. Procedure
4.1. Composition determination using the refractometric method (calibration curve
preparation)
 Clean properly the refractometer
 Prepare ethanol-water mixtures at known molar compositions (0%, 25%, 50%, 75%, and 100%
ethanol)
 Record the values of the refractive index versus the composition of the mixtures, on a table
(Table 1)
 Plot the index of refraction versus the mole fraction, on a chart, and extract the equation of the
calibration line
 Repeat the operation to obtain a calibration line more accurate for low concentrations of ethanol
in water (Table 2)

Table 1: Refractive index vs. mole fraction

Mole fraction (%) 0 25 50 75 100
Index of refraction

Table 2: Refractive index vs. mole fraction to be more accurate for calibration curve at low
ethanol concentrations
Mole fraction (%) 0 5 10 20 25
Index of refraction

4.2. Operating instruction in automated mode

Before starting the operation in automated mode ethanol to water mixture should be prepared with a mole
fraction of 10 %.

4.2.1. Start up at atmospheric pressure

 Connect the plant to the electrical main power
 Shut off valves V2, V3, V4, V5, V7, V8, V9, V10, V11, V12, V14, V21, V23, V26 and V27

 Open valves V1, V13, V15, V16, V17, V18, V19, V20, V22 and V24
 Valve V6 is permanently opened to avoid overpressure in the feeding line Open partially valve V25
 Open valve V5 to feed over the intermediate plate.

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 Fill the boiler, with the mixture to be distilled (water-ethanol, 10% mole fraction.), until the electrical
resistor J2 is completely plunged.
 Fill the tank D1 with the mixture to be distilled (water-ethanol, 10% vol.)
 Push the “Start” pushbutton
 Open the Connected tap water of the plant and set the water flow rate to 150 l/hr.

4.2.2. Study the effect of reboiler heating power

 Set the resistor J2 to 90 % then switch on the heater by clicking the red light to green.
 Take the mixture to the boiling point of ethanol and then decrease the heating power to 80 %.
 Let the column to total reflux for about 5 minutes (until the temperature TI6 is stable).
 Turn the switch off the pump G1 and set the flow rate to 40% (5 l/hr)
 Wait until the container of the pre-heating resistor J1 is filled and then Adjust the set point
50°C. Note the pre-heating temperature must be less than the boiling point of the mixture.
 Switch on the heater J1 to green.
 To select the reflux ratio, set the timer “START” at 2 sec and the timer “STOP” at 20 sec
 Set the switch “Reflux” to green.
 Start operating the distillation process, record all the temperatures of the sections, and take 5 ml of
samples of distillate and residue (bottom product) and determine their composition.
 By using the McCabe–Thiele method, determine the minimum number of theoretical plates, and
perform energy and material balance.
 Repeat the experiment with a heating power of 80 % to 60%.

Composition of Composition of bottom product

Test Test
distillate xd xb
1 1
2 2
3 3
Average xd Average xb=
Minimum number of theoretical plates (N) =

4.2.3. Study the effect of reflux ratio

 Set the resistor J2 to 90% then switch on the heater by clicking the red light to green.
 Take the mixture to the boiling point of ethanol and then decrease the heating power to 60 %.
 Let the column to total reflux for about 5 minutes (until the temperature TI6 is stable).

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 Turn the switch off the pump G1 and set the flow rate to 40% (5 l/hr)
 Wait until the container of the pre-heating resistor J1 is filled and then Adjust the set point
50°C. Note the pre-heating temperature must be less than the boiling point of the mixture.
 Switch on the heater J1 to green.
 To select the reflux ratio, set the timer “START” at 4 sec and the timer “STOP” at 40 sec
 Set switch “Reflux” to green
 Start operating the distillation process, record all the temperatures of the sections, and take 5 ml of
samples of distillate and residue (bottom product) and determine their composition.
 By using the McCabe–Thiele method, determine the minimum number of theoretical plates, and
perform energy and material balance.
Test Composition of distillate xd Test Composition of bottom product xb
1 1
2 2
3 3
Average xd Average xb=
Minimum number of theoretical plates (N) =

4.3. Shut down

 Set the switch of the pre-heating resistor J1 to re
 Stop the pump G1
 Set the switch of the heating resistor J2 to red
 Set the “Reflux” switch to red
 After about 3-5 minutes close the water inlet to the overhead condenser (set the output of the control
loop FIC1 to 0)
 Drain the tanks D2, D3 and D4
4.4. Emergency

 Push the emergency red pushbutton

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5. Result and Discussion

5.1. Material and Energy Balance Data

SN Time Xd % T1 T2 T3 T4 T5 T6 T7 T8 T9 T10 T11 T12

Composition 1
of distillate 2
(%) 3
Average Xd
N
SN Time Xb %
Composition 1
of reboiler 2
(%) 3
Average Xb
N

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