Process Engineering

Department

Chemical Engineering Lab

Binary Distillation
LEARNING OUTCOMES FOR DISTILLATION LAB
At the end of this course, students will be able to:

1. Knowledge and Understanding

 Identify key process variables in the operation of the distillation plant
 Use standard operating procedures to start up and shut down the distillation plant
 Differentiate between steady state and transient operation
 Identify process upsets during operation

2. Cognitive skills
 Monitor process variables to identify deviation from steady state operation
 Conduct material and energy balances in unit operations

3. Practical and Professional skills

 Develop operational skills
 Trace process lines and perform pre –start up checks
 Conduct start-up, normal operation and shutdown of distillation unit
 Monitor and manipulate process variables using a Distributed Control System
 Collect samples and perform basic quality control checks

4. Transferable and Key skills

 Apply theoretical knowledge and operation skills to correct upsets in a process and
achieve desired product specifications
 Use technical report writing skills to produce laboratory reports

1|Page
 Binary Distillation
Objectives:

 Familiarization with Prestart up procedure

 Adjust operating variables, e.g. temperature, pressure, feed rate, energy input rate
and reflux rate to produce nearly pure methanol and water products from a mixture
of methanol and water
 Create flooding conditions in the tower, observe and control by adjustment of
process variables
 Test the feed, top and bottom products to determine the percentage of methanol in
each stream
 Shut-down the distillation column
 Perform material and energy balances

Principles of Distillation

Distillation is an example of a mass transfer operation. In distillation, the separation of a liquid

mixture into its individual components or into groups of components is achieved via a series of
condensation and vaporization stages. Differences in boiling points or volatility is the basis of
separation of components via distillation, as differences in boiling points will directly influence
the distribution of the various components between a vapour phase and a liquid phase. Volatility
is a measure of how easily a liquid can change phase to vapour (i.e. ease of vaporization).

A volatile liquid vaporizes easily since it has a low boiling point and a high vapour pressure. A
binary mixture will be separated via distillation in to a more volatile component (MVC) and a less
volatile component (LVC). The LVC requires more energy to vaporize since it has a lower vapour
pressure than the MVC. (Question: In cooling a binary mixture of vapours, which component
would condense first, LVC of MVC?)

The creation of the vapour phase in distillation is achieved by boiling of the liquid mixture using
a heating medium such as steam or an electrical heating element in a reboiler which is located at
the base of the column or external to the column. Since the heat is supplied to the column from the

2|Page
base, a temperature gradient exists within the column whereby the hottest temperature exists at the
bottom of the column and the lowest at the top of the tower. This decrease in temperature ascending
the column allows the vapour that flows upwards to become richer in the MVC while the liquid
flowing down the column becomes richer in the LVC. This occurs since as temperatures decreases,
the LVC will be condensed out and separated from the rising vapours and fall downwards to the
base of the column as a liquid, leaving the rising vapours richer in the MVC. Thus, the vapour
phase will contain more of the MVC and the liquid phase will contain more of the LVC.

Binary Distillation

The simplest case of continuous distillation is binary distillation, whereby a single liquid feed
mixture of two components is separated into two separate products. The product withdrawn from
the top of the column is known as the overhead product or top product or distillate, and the product
drawn from the base of the column is known as the bottoms product or simply, the bottoms. The
separation of a mixture of methyl alcohol and water into its components is a typical example of
binary distillation.

3|Page
 Figure 1

Continuous Fractionating Column with Rectifying and Stripping Sections

(Reference: Unit Operations of Chemical Engineering, 5th Edition, McCabe, Smith, Harriott)

A conventional distillation column has a feed stream, an overhead product and a bottom product,
a condenser and a reboiler. The liquid feed enters the distillation column after it is preheated. The
Column A is fed at or near its midpoint with a definite flow of feed of known composition. The
plate on which feed enters is called the feed plate. All plates above the feed plate constitute the
rectifying section, and all plates below, including the feed plate itself, constitute the stripping
section. The feed flows down the stripping section into the bottom of column in which a definite
level of liquid is maintained.

4|Page
The liquid flows to the Reboiler B, which is an electric heated vaporizer. The reboiler provides
the initial vaporization of liquid phase to create the vapour phase. Part of the liquid in the reboiler
is vaporized and the vapour is returned to the distillation column. At one end of the reboiler is a
weir and the bottoms product is withdrawn from the pool of liquid on the downstream side of the
weir and flows through the Cooler G. Heat exchange occurs in cooler G, whereby the heated
bottoms product exchanges heat with the cooler incoming feed stream and thus preheats the feed.

The vapours rising through the rectifying section leaves as overhead vapours and are completely
condensed in Condenser C. The condensate from Condenser C is collected in Accumulator D, in
which a definite liquid level is maintained. Part of the liquid from the overhead Accumulator D
is withdrawn as the distillate or top product and the rest is returned to the column as reflux liquid.
Reflux Pump F takes reflux from the Accumulator D and delivers it to the top tray of the tower.
The reflux liquid flows down the column, combining with the feed stream in the column, and the
combined liquid continues to flow down the column. Without the reflux, no rectification would
occur in the rectifying section and the concentration of the overhead product would be no greater
than that of the vapor rising from the feed plate. Condensate not picked up by the reflux pump is
cooled in Heat Exchanger E, called the product cooler, and withdrawn as overhead product.

Inside the column, the down-flowing liquid comes into contact with the up-flowing vapour. The
distillation column is equipped with trays and/or packings that facilitate the intimate contact
between the phases. During the vapour-liquid contact, the vapour is enriched further in MVC (and
stripped of LVC) while the reverse is true for the liquid.

In the lab a mixture of methyl alcohol and water is separated into nearly pure methyl alcohol and
water products.

The column has plates or trays which provide the vapor liquid contact the same way as the packing
in a packed tower. The three most common type of trays are shown in figure below (column in
the lab has bubble cap trays):

5|Page
 Figure 2

Cross-Sectional View of Finite-Stage Contactor Tower in Operation showing a Sieve Tray, a

Valve Tray, and a Bubble-Cap Tray

(Reference: Elementary Chemical Engineering, 2nd Edition, Max Peters)

6|Page
 Figure 3
Vapor Flow Through Trays
(Reference: Surface Production Operations, 2nd Edition, Arnold, Stewart)

Sieve Trays:
 Is the least expensive tray option.
 If vapor velocity is much lower than design, the liquid will begin to flow through
perforations (a condition known as weeping). For this reason, sieve trays have poor
turndown ratio.
 Have high capacity, high efficiency.

7|Page
Valve Trays:
 Are essentially modified sieve trays.
 Have holes punched in the tray floor but they are much larger than those in the sieve
trays. Each of these holes is fitted with a device called a valve.
 At low vapor rates valves are closed. As the vapor rate increases the valve opens
up accordingly.

Bubble Cap Trays:

 Are more expensive
 Have lower capacity
 Have higher pressure drop than valve or sieve trays
 Don’t weep unless they are damaged. For this reason they have very good
turndown ratio.

8|Page
 Figure 3
Cross-Sectional View of Bubble-Cap Plate Tower (one plate shown)
(Reference: Elementary Chemical Engineering, 2nd Edition, Max Peters)

9|Page
PFD of Distillation Trainer

10 | P a g e
P&ID of Distillation Trainer

11 | P a g e
STARTUP PROCEDURE
Outside Control Room
1. Turn on the power to the control panel and select whether operation is to be from the local
panel or DCS. If DCS control is selected, ensure that the local controllers are switched to
automatic (red light off).
2. Turn on the power to the reboiler panel.
3. Open instrument air supply valve.
4. Turn on the cooling water flow through the overhead condenser, and bottom product cooler by
opening the block valves.
5. Select feed tray (usually tray 5).

Inside Control Room

6. Ensure all valves are closed.
7. Ensure level in reboiler is 4-6 inches (10-15 cm).
8. Turn on the power supply (PIC-105) to the reboiler. Allow reboiler to heat up, while tracing
the process flow lines for the column.

Notes: >If the column is going towards flooding conditions, reduce power immediately.

9. When the glass accumulator fills to the point that the low accumulator level alarm cancels,
start the feed flow and stabilize the stripping section of the column.
The feed flow rate should normally be in the range of 30 to 50% of full-scale, with feed going
to tray 5 in the column. Keep the feed flow rate steady. Only adjust it if it deviates by itself
from the initial steady value.

Notes: >all pumps to be started against closed valves

>always check visually for correct flow

10. After the stripping section has stabilized, start the reflux flow and visually check for flow at
top of column and observe impact on temperature. Stabilize rectifying section.

12 | P a g e
11. The column is now operating but must be adjusted to attain a steady-state operation with
reasonable top and bottom product flows. Operating variables that can be adjusted
independently are:

(a) Amount of reboiler power

(b) Reflux flow
(c) The amount of the feed
(d) Position of feed.(fixed to tray 5 for this experiment)

Notes: >If a flow rate has gone to zero, stop the pump immediately.

Observe column temperatures, reasonable operation results in a good spread of temperatures in the
tower (trays 1 to 10, the overhead vapor to the condenser, and the reboiler temperature). The
temperature spread on the trays between the reboiler (close to 100 ºC, the boiling point of water)
and the condenser (close to 65 ºC, the boiling point of methanol).

DATA COLLECTION:

When reasonable operation has been achieved, obtain samples of feed, top product, and bottom
product and determine the percent methanol in each, to determine if a reasonable separation is
being attained. (See attached graph to convert specific gravity to % methanol).

1. Record the temperature of each sample.

2. Using a hydrometer, measure the specific gravity of each sample and convert it to percent
methanol.
3. Repeat the analysis of feed, top product, and bottom product for final purities.
4. Create flooding conditions in the tower by reboiler rate and feed flow rate to the tower.
Make observations and record them.
**Screen shot of DCS to obtain values for calculations.

13 | P a g e
SHUTDOWN PROCEDURE:

1. Shut off power to the reboiler by first reducing the output of PIC-105 to zero then turning
off the switch on the reboiler panel.
2. Stop reflux flow to column and save for later cooling down.
3. Continue to circulate cold feed to cool down column.
4. When reboiler temperature reaches a fairly low temperature (= or < boiling point of
methanol), stop feed flow by closing feed valve and turning off pump.
5. Re-start the reflux flow into the column for further cooling.

Notes: >Do not empty accumulator to zero, leave approximately 4inches of reflux
to avoid damaging pump.

6. Turn off reflux flow by closing valve and stopping pump.

7. Ensure all control valves via the control panel are closed and all pumps are off before
leaving control room.
8. Close instrument air valve, cooling water valves and feed tray.
9. Switch to local control and turn off power to the control panel.

14 | P a g e
Material Balance Calculations
Calculation of Mass Flow Rates

1. Use the dimensions of circumference and wall thickness taken for each cylinder (top
product, bottom product and feed cylinders) and calculate the internal diameter of each
cylinder.
2. Use the dimensions of recorded height of liquid in each cylinder and the internal diameter
to calculate the volume of liquid in each cylinder.
3. Calculate the respective volumetric flow rates for top, bottom, and feed streams using the
calculated liquid volumes and the times recorded for the liquid to accumulate in the
cylinder to the recorded height.
4. Convert the volumetric flow rates for each stream into a mass flow rate by using the specific
gravity measurements that were obtained from the hydrometer.

Overall Material Balance

1. Once the flow rates of the top, bottom and feed streams are calculated, conduct the overall
material balance for the column using the relationship:

Mass in = Mass out

F=D+B
Where:
F = Feed
D = Distillate (top product)
B = Bottoms (bottom product)

If F  D+B, suggest possible reasons.

Individual Component Balance: (Methanol and Water Balance)

1. Using the percentage purity values read off from the weight % of methanol vs. specific
gravity chart, conduct the component balance using the relationship:

Methanol in = Methanol out

Water in = Water out

15 | P a g e
 F x f  D xD  B xB

Where:
xf = mass fraction methanol or water in feed.
xD = mass fraction methanol or water in distillate
xB = mass fraction methanol or water in bottoms

If F x f  D x D  B x B , state possible reasons.

Heat Balance Calculations

Calculation of Heat Input into Column

1. Calculate the heat input (in kW) into the column from the reboiler using the following
relationship:
100% Reboiler output = 30 kW
30  Re corded Re boiler Output %
Heat Input to Column = , in kW
100

Calculation of Heat Load

1. Calculate the heat load in E-101, E-102 and E-103.

For example to calculate the heat load in E-102:
Q = mcp∆T
Where:
Q = heat output in J
m = mass flow rate (kg/s) in bottoms product cooler (obtained from material balance
calculations)
cp = Specific heat of water 4.184 kJ/kgºC
∆T = Change in temperature in bottom product cooler (Temperature of bottoms product
entering heat exchanger -Temperature of bottoms product leaving heat exchanger), ºC
Use the cp of methanol as = 2.53 kJ/kgºC

16 | P a g e
Overall Heat Balance in Column

1. Conduct an overall heat balance in the column using:

Heat In = Heat Out

If Heat In  Heat Out, give any possible reasons.

Calculation of Cooling Water Flow Rates

1. Calculate the cooling water flow rates in E-102 and E-103.

For example to calculate the cooling water flow in E-102:
Q = mCp∆T
Q = Heat output by E-102 (obtained from heat load calculations above)
m= mass flow rate (kg/s) of cooling water
cp = Specific heat of water 4.184 kJ/kgºC
∆T = Change in temperature in cooling water (Temperature of cooling water entering heat
exchanger -Temperature of cooling water leaving heat exchanger), ºC

17 | P a g e
18 | P a g e