Chemical Engineering Practical 1

2023 Experiment Guideline

(CEP2601)
DISTILLATION

Semester 1 and 2

Department of Chemical Engineering

IMPORTANT INFORMATION:

This practical guideline is to be followed all the time when operating the pilot plants
in the laboratory

Open Rubric
DISTILLATION

1.1 INTRODUCTION
The multi-stage distillation is a basic unitary operation of chemical industry.
The liquid-vapour separation (L-V) is a process which has been used for many years
and many are the methods and devices developed in to obtain the balance (equilibrium)
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 designed to obtain the
maximum interface area.
With constant liquid and vapour 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 (equilibrium) of the system, which represent the
100% of efficiency.
The combination of factors such as the production of contact devices, the operating
conditions, the characteristics of the system rarely take the system to an efficiency of
100%. (In practice, 100% efficiency is impossible).
The separation process is usually carried out in columns which consist of devices
enabling the continuous or discontinuous liquid-vapour contact.
The plate columns are the examples of discontinuous balance states, while the filling
(packed) columns are the example of continuous liquid- vapour contact.
The first ones cause a variation of the liquid and vapour concentration on plates, each
of which represents a balance state. The mass transfer, of course, occurs also in
the part between the plates: between liquid in the shape of little drops and vapour and
between vapour and liquid in the shape of foam.
The actual mass transfer is attributed to the contact between the two phases on the
plate or very near it.
The plate column is different from a filling column because the first has its own “downfall”
to keep a liquid state on the plate and it has a downward pipe (downcomer) taking the
liquid from the upper to the lower plate.
The filling columns make the continuous mass transfer between phases possible
for the whole height of the column.

The main difference between filling column and plate ones lies in the fact that in the
first one (packed column) the liquid and vapour mus pass in countercurrent through
the same passages, while in the second (plate column) the two phases continue taking
two separate ways except when these are in contact between them on the plate.
You can have plate columns without the downwards pipes and so the two phases must
cross the same passages; these columns are considered filling and must
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be treated as such.

2. DESCRIPTION OF EQUIPMENT

2.1 Description of the equipment

•AISI 304 stainless steel framework with castors
•6 litres reboiler, borosilicate glass execution
•Quartz pre-heating resistance, P=1000W, code J1 with borosilicate glass
container, code J1
•Quartz heating resistance, P=2500W, code J2
•Distillation column, DN 80, h = 1500mm, borosilate glass execution, with 10 bubble
cup plates, code C1
•Shell and tube overhead condenser, stainless steel execution, exchange surface
0.4m2, code E1
•Tube-tube heat exchangers for bottom product cooling, AISI 316 stainless steel
execution, code E1
•15 litres feeding tank, borosilate glass execution, code D1
•5 litres tank for distillate product, borosilicate glass execution, code D2
•5 litres tank for condensed product, borosilicate glass execution, D3
•5 litres tank for bottom product, borosilicate glass execution, D4
•Metering feeding pump, PP execution, flow rate 0 -16l/h, adjustable with 4 -
20 mA signal, code G1
•Liquid ring vacuum pump, P =0.7kW, code G2, with solenoid valve on inlet water
pipe, code EV2, air/water separator, AISI 304 stainless steel execution, code D5
•8 RTDs double Pt 100, AISI 316 stainless steel sheath
•8 electronic temperature indicators
•2 metering pumps for the control of reflux ratio, PVDF execution, range 5l/h at
5bar, code G3 and G4
•Electronic flow meter, variable area type, range 25 -250l/h, output signal 4-20 mA,
AISI 304 stainless execution, code FI1
•Electronic differential pressure transmitter for the condensate level measure, range
0-500 mmH20, AISI 316 stainless steel execution, output signal 4-
20 MA, code LT1
•Electronic level indicator, range 0-100%, code LI1
•Electronic absolute pressure transmitter, range 0-1000 mbar, AISI 316 stainless
steel execution, output signal 4-20 mA, code PT1
•Pneumatic control valve for overhead condenser cooling water, Cv =2.5, AISI
316 stainless steel execution, code PV1
•2 PID digital controllers, 4 control loops complete with RS485 cards
•Connecting lines and valve in AISI 304-316 stainless steel
•IP55 electrical switch board, according with CE standards, complete of plant synoptic
and E.L.C.B
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2.2 Brief Description of Controller Digitric 5000
This plant is equipped with 2 controllers Digitric 500, multi-loops PID type.
Each controller is complete of RS-485 cards for the connection with PC (by means of
a RS-485/232 converter included in the serial cable).
The configuration of the controllers is the following:
2.3 Controller no.1
•1st loop: control of flow rate of overhead cooling water, code FIC1 range 0-
100% proportional to 0-250l/h, output controlling valve FV1; measure of
temperatures TI2, TI3 and TI4
•2nd loop: residual pressure control, code PIC1, range 0-100% proportional to
0-1000mbar, output controlling valve FV2
•3rd loop: output controlling pump G3, range 0-100% proportional to 0-5 l/h
•4th loop: level control, code LIC1, range 0-100% proportional to 0-500 mbar, output
controlling pump G4

2.4 Controller no.2

•1st loop: pre-heating temperature control, code TIC1, range 0-1000C, output
controlling J2
•2nd loop: measure of differential pressure PdI1 and of temperatures TI5, TI6;
TI7 and TI8; output controlling resistance J2, range 0-100% proportional to 0-
2500W
• 3rd loop: output controlling pump G1, range 0-100% proportional to 0-16l/h
Display Indications

•1st line: text line where the indications of menu and submenus appear
•2nd line: process variable
•3rd line: display of set-point (SP) value, error; out, %, bar. That can be
selected with the key Ind
•4th line : indication of the current loop
Description of frontal panel
•Key Loop it enables to select the desired loop
•Key Ind: it enables to vary the parameter appearing in the third line of the
display, or to set the parameters as it will be explained in the next page.
•Key Esc/Menu: it enables to enter the menu or to exit from the menu and
submenus without storing the variations carried out
•Key Enter: it enables to enter the menu and submenus and to confirm the
variations carried out
•Key M/A/C: it enables to switch from the automatic mode to the manual mode
•Keys ▼▲: they enable to increase or reduce the set point value, the value of the
parameter selected in the programming or to run the menu and submenus

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• Key SP-w: it enables to display the set-point value in the third line

Setting the parameters

The parameters are set in the submenu Parameter that can be entered according to
the following procedure:
•Enter the main menu by pressing the key Esc/Menu; position on the submenu
Parameter running (scrolling) the list of submenus with the keys
▼▲; then enter the submenu pressing the key Enter
•Choose the parameter to be modified running the list with the keys ▼▲ and press
the key Enter to select
•Modify the value of the parameter by pressing the key Enter and then the keys
▼▲; press the key Ind and shift to the digits of the number to be modified; pressing the
key Ind for 3 seconds shifts the decimal point
•Exit without confirming by pressing the key Esc/Menu
•Confirm the variation by pressing the key Enter
Example: Modify the value of the GAIN (Proportional band), integral and
derivative action
• Press the key Esc/Menu
• Run the list of submenus with the keys ▼▲ up to the parameter
• Press the key Enter
• Position on the loop of interest with the keys
• Press the key Enter, GAIN is displayed on the first line
• Press the key Enter
• Position on the digit to be varied pressing the key Ind
• Increase or reduce the value with the keys ▼▲
• Confirm the variation pressing the key Enter
• Vary the integral action (RESET TIME Tn) operating as in the case of GAIN
• Vary the derivative action (RATE TIME Tv) operating as in the case of GAIN
For further information on the instrument DIGITRIC 500 refer to the
instructions manual

3. START UP AND RUNNING THE PLANT IN AUTOMATED MODE

3.1 Services
Hereafter follows a series of the services necessary for the good
operation of the continuous distillation pilot plant mod. CA/EV

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• Power phase,50 HZ, max. power 6 kW
supply: 380 V • Water: max. consumption 1000 l/h
three • Compressed air at 6 bar, max consumption 10 Nm3/h
3.2 Brief description of the cycle
The continuous distillation plant is mainly composed of a bubble-cap column, bottoms
boiler with electrical sensor, a condenser and a feed pump.
The binary mixture, stocked in the proper tank, is fed with a pump after it has been pre-
heated by an electrical resistor.
Once the boiler has been filled, the solution is heated with the bottom resistor.
Once the solution reaches the boiling point and the column is at steady state the distillate
can be taken, keeping the reflux ratio as fixed, and then it can be fed.
3.3 Setting the continuous distillation plant ready to start in automated mode
at atmospheric pressure.
•Shut of valves V2, V3, V5, V6, V11, V15, V16, V17, V18, V19, V20, V21, V24, V27,
V28 and V29.
•Open valves V1, V4, V7,V8, V9, V10, V12, V13, V14, V22, V23, V25, V26 (partially)
•Fill the boiler, with the mixture to be distilled (e.g. : 10% water- methanol or water-
ethanol), until the electrical resistor J2 is completely plunged
• Fill tank D1 with the mixture to be distilled
• Set all switches to 0
• Connect the plant to the electrical supply
•Connect the pressure reducer under the electrical switchboard to the laboratory
compressed air line (using the pipe with quick connections provide) and adjust the
pressure at 1.5 bar
•Connect the plant to the water system as in the synoptic (valve V7 and valve V26)
with the rubber pipe provided, using metal hose clamps to fix it to the hose connector
•Connect the water outlet to a floor drain with the rubber pipe provided, using
metal hose clamps to fix it to the hose connector
• Turn the switch AUTO-PC to AUT

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 • Switch on the E.L.B.C
• Push the start button
• Select the 1st loop FIC1 (Controller no. 1) with pushbutton Loop
• Set the control mode of the 1st loop FIC1 (controller no. 1) to
manual mode with pushbutton M/A/C (red led on)
• Open the control valve FV1 and set the flow rate at 40% for
example (select the indication Out with pushbutton Ind and
increase or decrease it with pushbutton ▼▲)
• Adjust the set point (push the button SP-w increase or decrease its
value with the push button ▼▲) at 40% for example
• Set the 1st loop FIC1 to automatic mode with pushbutton M/A/C
(green led on)

Objectives:

• To calculate mass balance and energy balance for the distillation column
• This will help the student to understand the effects of variable such as feed
composition, reflux ratio and calibration curve of the composition binary mixture
using refractometer
3.4 Start up
• Set the switch of the resistor J1 to 1
• Power the electrical resistor using the output 4-20 mA of the 2nd
loop of the controller no. 2, proportional to 0-2500 W (Select the 2nd loop
with pushbutton Loop and then the indication Out with pushbutton
Ind, finally increase or decrease its value with pushbutton ▼▲)
at 100% for example.
• Take the mixture to the boiling point
• Wait about 15 – 20 minutes to reach steady state
• Wait for steady state condition (temperature TI4 constant), once TI4
is constant reduce J1 to 70%
• Turn the switch of the pump G1 to the position 1 (If not getting flow
to J2, open plastic valve on pump G1)
• Feed e.g. 8 l/h of mixture using the output of the 3rd loop of the
controller no. 2 (select the 3rd loop (G1) with pushbutton Loop and then
the indication Out with pushbutton Ind, finally increase or decrease
its value with pushbutton ▼▲)
• Wait until the container of the preheating resistor J2 is filled
• Switch on J2
• Select the 1st loop (TIC1) of controller no. 2
• Adjust the set point (push the button SP-w increase or decrease its
value with pushbutton ▼▲) at 55oC for example
• Set the control loop TIC1 to automatic mode with pushbutton M/A/C
(green led on)

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•When the distillate level in tank D3 is sufficient, control it automatically:
select 4th loop LIC1 of controller no. 1 with pushbutton Loop, select the
setpoint pushbutton SP-w, increase or decrease its value with pushbutton ▼▲ at 40%
for example; switch the loop in automatic mode with pushbutton M/A/C (green led on)
 Open V17 and V18
•Switch on pump G4 (4th loop of controller no. 1)
•Switch on pump G3 (reflux pump) and set the flow rate in function of the ratio desired:
select the 3rd loop (G3) of controller no. 1 with pushbutton Loop, select the output with
pushbutton Ind, increase or decrease its value with pushbutton ▼▲ (NB: all this is
done in manual mode)
 Start the stop watch once the droplets of sample is obtained in tank D2 and open
V21 immediately.
 Take sample every five minutes from D2 and D4 and record mass and volume
as well as temperatures.
3.5 Shut-off of the plant
•Set the switch of the pre-heating resistor J2 to 0
•Stop pumps G1, G3 and G4
•Set the switch of the heating resistor J1 to 0
•After about 3-5 minutes close the water inlet to the top condenser
(take the output of the control loop FIC1 to 0)
•For long stop drain completely tanks D1, D2, D3, D4 and the reboiler
3.6 Running anomalies
•If the distillate cannot be condensed, check if there is water across the condenser
•If the column tends to go flooding, drop the power to the boiler or reduce the feed
flow rate
•If the distilled concentration is lower than the required one, increase the reflux ratio
3.7 Emergency
•Push the emergency button

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4. RESULTS AND FINDINGS

Table1: Product composition

Xd Xd

Time Mass (g) Volume Density (mass (mole

(ml) fraction) fraction)
(kg/m3)

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Table1: Bottom composition

Xw Xw

Time Mass (g) Volume Density (mass (mole

(ml) fraction) fraction)
(kg/m3)

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Equilibrium Data

Molar Fraction of Ethanol in Molar fraction of Ethanol in the

the liquid vapour
0 0
0.00565 0.0424
0.0229 0.0147
0.0346 0.205
0.059 0.301
0.123 0.468
0.194 0.573
0.273 0.649
0.360 0.708
0.458 0.758
0.567 0.809
0.692 0.967
0.836 0.931
1 1

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