BATCH DISTILLATION

Experiment #1:
To determine the pressure drop over the distillation column
for various boil up rates.

Theory:
Batch distillation
Type of distillation where the entire batch of liquid feed is placed into the still
at the start of the process and then heated. The vapor is collected and condensed
to a distillate some of which is as reflux. The composition of the remaining
liquid and the distillate are functions of time.
Description of the column:
The batch distillation column consists of a still at the base, which is charged
with ethanol - water mixture at the start of the experiment, a glass column
packed with small glass cylinders, a condenser positioned above the column, a
reflux valve, a product cooler and a collection
cylinder

Heaters
The
round
bottomed flask
sits
in
an
electric heater,
which
is
controlled
from the heater
control panel.

The heaters
are turned on
and off using
the switches
next to the dials on the heater control panel.

There is no temperature measuring instruments connected to the heater control

so the dial will read zero.
Thermocouple Display

Thermocouples are used to measure the temperature at various points in the

column. The thermocouples that are connected to the display have blue and
white wires. They are numbered from 1-9. Numbers 1-6 measure temperatures
in the column, with 6 being the temperature of the top product vapor. Numbers
7-9 measure the cooling water temperature at the inlet to the product cooler, the
inlet to the condenser and the outlet of the condenser respectively. The dial is
used to select which thermocouple outlet is displayed.
Reflux Valve Control

The reflux ratio is controlled using a solenoid valve which has two positions;
Open - all the condensed liquid is returned to the column
Closed - all the condensed liquid goes to the overhead product
The reflux ratio is determined by the ratio of the time the valve is open to the
time the valve is closed. If the valve is open for twice as long as it is closed then
the reflux ratio is 2. The dial on the reflux valve control box is used to set ratio
of the time the valve is open to the time the valve is closed and therefore the numbers
on the dial represent the actual reflux ratio. When the dial is at zero the valve will be open all
the time. The switch on the control box turns the reflux valve on and off.
Sample Valves

There are 10 sample valves. Number 1 is a syringe which allows a sample to be

taken from the round bottomed flask. Numbers 2 - 9 give samples of the liquid
flow within the packing. Number 10 samples the overhead liquid product.
Types of cross flow trays
Three basic types of cross flow trays used are
Sieve Plate (Perforated Plate)
Bubble Cap Plates
Valve plates (floating cap plates)

Operation at constant product composition:

In many instances processes are carried out in batches, and it is more convenient
to distil each batch separately. In these cases the whole of a batch is run into the
boiler of the still and, on heating, the vapor is passed into a fractionation
column, as shown in Figure 11.33. As with continuous distillation, the
composition of the top product depends on the still composition, the number of
plates in the column and on the reflux ratio used. When the still is operating,
since the top product will be relatively rich in the more volatile component, the
liquid remaining in the still will become steadily weaker in this component. As a
result, the purity of the top product will steadily fall. Thus, the still may be
charged with S1 mols of a mixture containing a mole fraction xs1 of the more
volatile component. Initially, with a reflux ratio R1, the top product has a
composition xd1. If after a certain interval of time the composition of the top
product starts to fall, then, if the reflux ratio is increased to a new value R2, it
will be possible to obtain the same composition at the top as before, although
the composition in the still is weakened to xs2. This method of operating a batch
still requires a continuous increase in the reflux ratio to maintain a constant
quality of the top product. An alternative method of operation is to work with a
constant reflux ratio and allow the composition of the top product to fall.

One of the added merits of batch distillation is that more than one product may
be obtained. Thus, a binary mixture of alcohol and water may be distilled to
obtain initially a high quality alcohol. As the composition in the still weakens
with respect to alcohol, a second product may be removed from the top with a
reduced concentration of alcohol. In this way it is possible to obtain not only
two different quality products, but also to reduce the alcohol in the still to a
minimum value. This method of operation is particularly useful for handling
small quantities of multi-component organic mixtures, since it is possible to
obtain the different components at reasonable degrees of purity, in turn. To
obtain the maximum recovery of a valuable component, the charge remaining in
the still after the first distillation may be added to the next batch.
Operation at constant product composition
The case of a column with four ideal plates used to separate a mixture of ethyl
alcohol and water may be considered. Initially there are S1 moles of liquor of
mole fraction xs1 with respect to the more volatile component, alcohol, in the
still. The top product is to contain a mole fraction xd, and this necessitates a
reflux ratio R1. If the distillation is to be continued until there are S2 moles in the
still, of mole fraction xs2, then, for the same number of plates the reflux ratio
will have been increased to R2. If the amount of product obtained is Db moles,
then a material balance gives:
S1xs1 S2xs2 = Db xd
S1 S2 = Db
S1xs1 (S1 Db)xs2= Db xd
S1xs1 S1xs2 = Dbxd Dbxs2
Db= S1[xs1 xs2/xd xs2]= (a/b)S1

Where a and b are as shown in Figure. If is the intercept on the Y -axis for any
operating line, equation 11.48, then:
xd/(R + 1) = , or R = ( xd/) 1

These equations enable the final reflux ratio to be determined for any desired
end concentration in the still, and they also give the total quantity of distillate
obtained. What is important, in comparing the operation at constant reflux ratio
with that at constant product composition, is the difference in the total amount
of steam used in the distillation, for a given quantity of product, Db. If the
reflux ratio R is assumed to be adjusted continuously to keep the top product at
constant quality, then at any moment the reflux ratio is given by R = dLb/dDb.
During
the course of the distillation, the total reflux liquor flowing down the column is
given by:

Lb

R2

dL b= RdDb
0

R1

To provide the reflux dLb the removal of a quantity of heat equal to dLb in the
condenser is required, where is the latent heat per mole. Thus, the heat to be
supplied in the boiler to provide this reflux during the total distillation QR is
given by:

Lb

R2

Q= dLb= RdDb
0

R1

This equation may be integrated graphically if the relation between R and Dbis
known. For any desired value of R, xs may be obtained by drawing the
operating line, and marking off the steps corresponding to the given number of
stages. The amount of product Db is then obtained from equation and, if the
corresponding values of R and Db are plotted, graphical integration will give the
value of R dDb. The minimum reflux ratio Rm may be found for any given still
concentration xs from equation 11.56.
Operation at constant reflux ratio
If the same column is operated at a constant reflux ratio R, the concentration of
the more volatile component in the top product will continuously fall. Over a
small interval of time dt, the top-product composition with respect to the more
volatile component will change from xdto xd+ dxd, where dxdis negative for the
more volatile component. If in this time the amount of product obtained is dDb,
then a material balance on the more volatile component gives:
More volatile component removed in product = dDb [xd+ dxd/2 ]
which, neglecting second-order terms, gives: = xddDb
and: xddDb= d(Sxs )
But dDb= dS,
and hence: xddS= S dxs xsdS
and: S dxs= dS(xd xs)
Thus:

S2

xs2

dxs
=
dS
S1 S
xs1 xdxs

The right-hand side of this equation may be integrated by plotting 1/(xd xs)
against xs. This enables the ratio of the initial to final quantity in the still to be
found for any desired change in xs, and hence the amount of distillate Db. The
heat to be supplied to provide the reflux is QR = RDb and hence the reboil heat
required per mole of product may be compared with that from the first method.
Limiting Conditions Reflux Ratios

The external reflux ratio, L/D, is often a parameter that is specified for column
operation since it is perhaps the easiest to change under column operation and
changing L/D often has a substantial effect on the overall column behavior and
separation.
There are two limiting conditions with respect to the reflux ratio, L/D, that one
obtains:
Total reflux ratio, D = 0, L/V = 1, and L/D
Minimum reflux ratio, (L/D)min.

One will often see an external reflux specification as a multiple of the minimum
reflux ratio, for example, L/D = 2(L/D)min, etc.
A column which has total reflux and boil-up has no feed the distillate,
bottoms, and feed flow rates are zero.
This is a limiting condition which provides one with the minimum number of
equilibrium stages that can be obtained for a given column.
While one would not typically operate under such conditions, total reflux and
boilup are used for starting up a column, for operating the column off-line when
other unit operations are off-line, and for testing column efficiency.
R L/D
L/V 1.0
LV
L/ V 1.0

At total reflux:

Both operating lines, TOL and BOL, become the y = x auxiliary line.
Operating a column under total reflux yields the minimum number of
equilibrium stages for a particular column.

Total Reflux Minimum Number of Equilibrium Stages

Minimum Reflux

Minimum reflux, Rmin or (L/D)min, is defined as the external reflux ratio at which
the specified separation could just be obtained with an infinite number of stages.
We obtain an infinite number of stages if our operating lines touch the
equilibrium curve.
The point on the equilibrium curve that this occurs is called a pinch point.
Two Types of Pinch Points
For many systems, the pinch point will occur where the feed line crosses the
equilibrium curve.

A second type of pinch point can occur in non-ideal system where the
operating line touches the equilibrium curve before the intersection of the feed
line and the equilibrium curve.
Minimum Reflux Infinite Number of Equilibrium Stages

Rule of Thumb
The best operating condition lies between minimum and total reflux.
As a rule of thumb, the optimum reflux ratio lies between 1.05 and 1.25
(L/D)min.
Too low of an L/D results in a large number of equilibrium stages, while too
high of an L/D increases the re-boiler duty as well as the required diameter of
the column.

FACTORS
AFFECTING
OPERATION

DISTILLATION

COLUMN

The performance of a distillation column is determined by many

factors, for example:

feed conditions
state of feed
composition of feed
trace elements that can severely affect the VLE of liquid
mixtures
internal liquid and fluid flow conditions
state of trays (packings)
weather conditions
Some of these will be discussed below to give an idea of the
complexity of the distillation process.
Feed Conditions

The state of the feed mixture and feed composition affects the operating lines
and hence the number of stages required for separation. It also affects the
location of feed tray. During operation, if the deviations from design
specifications are excessive, then the column may no longer be able handle
the separation task. To overcome the problems associated with the feed,
some column are designed to have multiple feed points when the feed is
expected to containing varying amounts of components.
Reflux Conditions

As the reflux ratio is increased, the gradient of operating line for the
rectification section moves towards a maximum value of 1. Physically, what
this means is that more and more liquid that is rich in the more volatile
components are being recycled back into the column. Separation then
becomes better and thus less trays are needed to achieve the same degree of
separation. Minimum trays are required under total reflux conditions, i.e.
there is no withdrawal of distillate.
On the other hand, as reflux is decreased, the operating line for the
rectification section moves towards the equilibrium line. The pinch
between operating and equilibrium lines becomes more pronounced and
more and more trays are required. This is easy to verify using the McCabeThiele method.
The limiting condition occurs at minimum
reflux ration, when an infinite number of
trays will be required to effect
separation. Most columns are designed to
operate between 1.2 to 1.5 times the
minimum reflux ratio because this is
approximately the region of minimum
operating costs (more reflux means higher
re-boiler duty).
Vapor Flow Conditions
Adverse vapor flow conditions can cause

foaming
entrainment
weeping/dumping
flooding

Foaming
Foaming refers to the expansion of liquid due to passage of vapor or gas. Although it
provides high interfacial liquid-vapor contact, excessive foaming often leads to liquid
buildup on trays. In some cases, foaming may be so bad that the foam mixes with liquid
on the tray above. Whether foaming will occur depends primarily on physical properties
of the liquid mixtures, but is sometimes due to tray designs and condition. Whatever the

cause, separation efficiency is always reduced.

Entrainment
Entrainment refers to the liquid carried by vapor up to the tray above and is again caused
by high vapor flow rates. It is detrimental because tray efficiency is reduced: lower
volatile material is carried to a plate holding liquid of higher volatility. It could also
contaminate high purity distillate. Excessive entrainment can lead to flooding.
Weeping/Dumping
This phenomenon is caused by low vapor flow. The pressure exerted by the vapor is
insufficient to hold up the liquid on the tray. Therefore, liquid starts to leak through
perforations. Excessive weeping will lead to dumping. That is the liquid on all trays will
crash (dump) through to the base of the column (via a domino effect) and the column will
have to be re-started. Weeping is indicated by a sharp pressure drop in the column and
reduced separation efficiency.

Flooding
Flooding is brought about by excessive vapor flow, causing liquid to be
entrained in the vapor up the column. The increased pressure from excessive
vapor also backs up the liquid in the down-comer, causing an increase in
liquid holdup on the plate above. Depending on the degree of flooding, the
maximum capacity of the column may be severely reduced. Flooding is
detected by sharp increases in column differential pressure and significant
decrease in separation efficiency.
Column Diameter
Most of the above factors that affect column operation are due to vapor flow
conditions: either excessive or too low. Vapor flow velocity is dependent on
column diameter. Weeping determines the minimum vapor flow required
while flooding determines the maximum vapor flow allowed, hence column
capacity. Thus, if the column diameter is not sized properly, the column will
not perform well. Not only will operational problems occur, the desired
separation duties may not be achieved.
State of Trays and Packing
Remember that the actual number of trays required for a particular

separation duty is determined by the efficiency of the plate, and the packing
if packing are used. Thus, any factors that cause a decrease in tray efficiency
will also change the performance of the column. Tray efficiencies are
affected by fouling, wear and tear and corrosion, and the rates at which these
occur depends on the properties of the liquids being processed. Thus
appropriate materials should be specified for tray construction.
Weather Conditions
Most distillation columns are open to the atmosphere. Although many of the
columns are insulated, changing weather conditions can still affect column
operation. Thus the re-boiler must be appropriately sized to ensure that
enough vapor can be generated during cold and windy spells and that it can
be turned down sufficiently during hot seasons. The same applies to
condensers.
These are some of the more important factors that can cause poor distillation
column performance. Other factors include changing operating conditions and
throughputs, brought about by changes in upstream conditions and changes in
the demand for the products. All these factors, including the associated control
system, should be considered at the design stages because once a column is
built and installed, nothing much can be done to rectify the situation without
incurring significant costs. The control of distillation columns is a field in its
own right, but that's another story.
Advantages

Flexible
Accurate implementation of recipe specific to a given mixture
Several components separated using one column
Requires least amount of capital

Procedure:
Before starting make sure that all valves on the distillation column are closed.
Open valve V10 on the reflux pipe. Fill the boiler with 10 L of the solution.
Turn on the power from the control panel. Select the temperature to T9 on the
panel. open the valve V5 to enter the cold water to the condenser on the flow
rate of 3L/min. adjust the heater power to 0.75 kW. The heating of the feed will

start and temperature will rise on each plate. Open the valve V6 and V7 to
measure the pressure drop. The 1st and 5th plates are not insulated to observe
distillation. Eventually vapor will rise and will enter the condenser which will
be observed entering the receiver. The distillate will overflow the receiver and
will return to the column by reflux valve because column is operating at total
reflux. Then liquid will reach each plate and vapor will pass through the liquid.
Eventually equilibrium will be achieved when all plate temperature become
constant. Then take the samples and note the boil up rates. Then measure the
pressure across the column using manometer and valve V6 and V7 note down
the The pressure and boil up rate value. Repeat the process and note down the
values and build a graph showing the relationship of boil up rate and pressure
drop.
Observations:

Results:
As the boil up rate increases the vapor flow rate from still to the column also increases so
pressure drop also increases.