Fractional Distillation Experiment - ChE

DISTILLATION
You should plan and carry out this project as if you received the following memo from the head of your
engineering research and development division.
To: Group Leader

From: Head, Process R & D Unit
Subject: Experimental Fractional Distillation Apparatus
We are in the process of calibrating and testing our small-scale fractional distillation column so that it
may be used later for the separation of mixtures that occur in processes under consideration by Process
Development.
The binary methanol-water system has been selected as the test system based on the following
considerations:
(1) Both methanol and water are available in high-purity and at low cost, and
(2) The properties of the pure components and of their mixtures are readily available in the literature.
Please do the following:
(a) Obtain mathematical models describing the operations of the column (material and energy
balance). Your knowledge of Process Dynamics will come handy here.
(b) Record the temperatures of the column stages (T1 – T6) at different times. This will be used to
determine the compositions of the methanol vapour at the different times (NOTE: Use Antoine
equation for methanol-water system. The column operating pressure is assumed to be 760
mmHg).
(c) Suppose the column is to be used for continuous operation such that the feed concentration is xF
and the distillate concentration is xD (obtain these concentrations for the system at steady state).
For the operating conditions chosen by your group,
i. What is the condenser heat duty?
ii. Determine the enthalpies of the feed, distillate and bottoms. What is the feed quality (i.e.
“q”)?
iii. Determine the number of stages at total reflux. Does this correspond to the actual number
of stages on the equipment?
(d) Determine the overall column efficiency and the Murphree efficiency of each plate. For these
purposes you should operate the column at steady state with total reflux.
(e) Compare your results with what would be obtained using a process simulation package such as
HYSYS or CHEMCAD. Comment on your findings.
As you know, the literature on binary distillation and the McCabe-Thiele method of analysis is vast.
Among the convenient references is the textbook by McCabe et al. (2005, Chapter 21).
Attached sheets give a summary of the manufacturer’s description of our distillation apparatus, including
a schematic diagram, and operating procedures.
Please note that methanol is a toxic material. Liquid is absorbed by skin contact. Vapor is mildly toxic on
inhalation. Its main toxic effect is on the nervous system, particularly the optic nerves and possibly the
retinas, which can progress to permanent blindness.
Vapor-Liquid Equilibrium Data for the Methanol-Water System
(In the following table, x and y are the mole fractions of methanol in the liquid and vapor phases,
respectively. T is the temperature in degrees Kelvin.)
The Apparatus
Figure 1 presents a schematic diagram of the fractional distillation apparatus.
• Feed Tank Reservoir. The feed tank has a capacity of about 10 gallons with a sloping bottom for proper
drainage. The reservoir is fitted with a liquid-level sight glass.
• Still Boiler. The boiler tank (capacity approximately 5 gallons) is fitted with a quick disconnect coupling
inlet, a pressure measurement port and a sight glass for visual liquid level indication. The main heating
element is a stainless steel sheathed bayonet-type cartridge heating element. This element has a
continuously-variable control and is rated at 2500 Watts. Precise liquid level control is obtained by means
of a float-type control element that actuates a solenoid-operated valve which recycles excess liquid from
the still boiler to the feed reservoir. The boiler also has a dial-type temperature indicator.
• Condenser. The condenser is a shell-and-tube heat exchanger which contains the equivalent of 1.5 sq. ft.
of spiral-tube heat exchange surface. The tube side coolant is water for this project. Countercurrent
coolant flow through the tube is metered by means of a rotameter. For pressure safety, a spring-loaded
relief valve (set for 1.0 psig) is connected to the shell side of the condenser. The shell side condensate
drains through a 3/8-inch line to the distillate receiver.
• Distillate Receiver. Condensate enters from the condenser through a 3/8-inch stainless steel tube into the
top of the receiver. The top flange also contains a spring loaded pressure relief valve set at 1.0 psig. From
the bottom are three connections: a valve drain, a valve inlet to the reflux pump, and an overflow stand-
pipe return to the main feed reservoir.
• Instrumentation and Control Panel. The panel includes a voltmeter and ammeter for power input and
indication, a boiler liquid level control switch for automatic operation (not in use at this time), a boiler
thermal-overload indicator, on-off electrical switches for feed and reflux pumps, and a continuously
variable control element for the main boiler heater. The main system power is controlled by means of a
circuit breaker, on-off switch, and indicator light. In addition, indicator lights are on circuits for the feed
and reflux pumps.
• Thermocouples. The system includes twelve thermocouples: one in the still boiler, six in the column
(one for each sieve plate tray), two on the condenser inlet and outlet lines, one for the distillate line, and
one for each preheater.
• Rotameters. The calibration for the reflux rotameter (calibrated with water at 21 oC over the range 20 to
100 on the tube scale) is given by:
F = 2.04 R - 13.2
where F is the flow rate in cm 3/min, and R is the rotameter reading. For the feed rotameter (calibrated
with water at 17 oC over the range 10 to 100 on the tube scale)
F = 1.99 R - 14.4.
• Column. The column consists of 6 sieve plate sections, each assembled from a 5- inch-long, 3-inch ID
glass pipe section, and a stainless steel process ring with four connections. Each section contains fittings
for feed, pressure measurement, liquid and vapor sampling, and weir-downcomer adjustment. The plate
column, when assembled, is approximately 30 inches in height. On each plate the weir and downcomer
are readily accessible for adjustment purposes.
• Plates. Each plate in the column is perforated with 36 holes of 3/32-inch diameter, with center-to-center
spacing of 0.265 inches (square pitch). The plate thickness is 0.125 inches; the space between plates is 6
inches. The opening for the downcomer has a diameter of 0.534 inches.
Start-up Procedure
1. Charge the feed reservoir tank through the spring-loaded opening C1 with 8 gallons of the mixture to
be distilled.
2. To charge the boiler, connect the flex-tubing feed line to the boiler top through the quick-disconnect
coupling Q1
3. Trace the feed line from the reservoir tank through the pump and feed rotameter, opening valves F1
and bypass F3, closing the drain valve D-1 and rotameter valves F2 and F4.
4. Turn the main power switch on, then the feed pump switch. Pilot lights should indicate that these units
are on.
5. Observe the liquid level as it rises in the boiler sight glass. When the liquid approaches the 3/4-full
mark, shut bypass F3 and open valves F2 and F4 to meter the remaining charge through the rotameter.
6. Begin the heating cycle. Check both the thermocouple and sample port tube fitting connections to
insure that they are properly sealed on each plate location.
7. Turn the boiler power switch on; a pilot light should indicate heat input.
8. Start a flow of water through the condenser. Set this rotameter at a low value. As the boil-up proceeds,
adjust the rotameter until the top section of the condenser near the vapor inlet line is just warm to the
touch.
9. Set the proportional power control switch for the boiler to the desired heating rate value to expedite the
start-up. Generally, it is best to turn full power on until boiling begins, but be sure to throttle back to the
desired value when boiling begins.
10. Monitor constantly the boiler temperature with the bimetallic thermometer T13, attached to the boiler
front.
11. While the system is heating up, open the distillate receiver overflow valve R2 to permit venting back
to the reservoir tank. The distillate drain valve R3 should be closed, and the distillate line valve R1,
leading to the suction side of the reflux pump, should be closed, and the recycle pump should be off.
12. Observe the temperature as distillate begins to collect in plates above the boiler. Steady-state
operation should obtain in roughly 30 minutes.
13. As distillate collects in the distillate receiver, turn on the reflux pump and maintain a reflux rate, using
valve R4, at a value sufficient to control the level (manually) in the distillate receiver.
14. Pressure relief valves (PRV) are located at the top of the distillate receiver and on the shell side of the
condenser. These are set to open at approximately 1.0 psig.
15. It is necessary periodically to monitor the liquid level in the boiler. If for any reason the liquid level
were to drop below the electrical heating coils in the boiler, a thermal overload switch, set to respond at
240 degrees Fahrenheit, would interrupt the line power. This overload switch is in the 250-Watt auxiliary
heater located on the right hand side of the boiler. The thermal overload switch is the red button located in
the center of this module. This device is manually reset and cannot be reset until the boiler temperature
drops below the trigger value.
Shut-down Procedure
1. Turn off the boiler power switch.
2. When condensate no longer collects in the distillate receiver, turn off the reflux pump, close valve R1,
and open valve R3. Leave valve R3 open so the system remains vented.
3. Turn the main power control switch off.

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DISTILLATION

To: Group Leader

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