I.

Introduction
A method of separating mixtures based on differences in their volatilities in a boiling liquid mixture. The components in a sample mixture are
vaporised by the application of heat and then cooled by the action of cold water in a condenser. Distillation is completed before more sample
mixture is added.

Batch distillation is an unsteady state operation. It is usually carried out in a batch still to which a column
equivalent to a number of equilibrium stages is attached. Alternatively, packings may be used.
The Figure below showed a typical set-up for batch distillation with rectifying column.

As in the case of simple distillation, a fixed quantity of liquid is originally charged to the batch still. During
distillation, the vapour passes upward through the column. The whole column is an enriching section. The
vapour is condensed into liquid at the top of the column. Part of the liquid is returned to the column as
reflux, and the remainder withdrawn as distillate. Nothing is added or withdrawn from the still until the run is
completed. As distillation progress, the MVC in the batch still decreases.

In principle, the alternative setup as shown in the Figure is also feasible. Here the vessel is located at the
top of the column that is operated as a stripping column. Such a set-up is often known as the inverted
batch distillation or the batch stripper. During operation, the LVC are primarily separated from the system.
The liquid is the still depletes in LVC and enriches in MVC.

This mode of operation is seldom applied in industrial processes, but it is necessary for the separation of
mixtures that form minimum-boiling azeotropes. This will covered in the section on azeotropic distillation.

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In a batch process, the main steps are operated discontinuously. In contrast with a continuous process, a
batch process does not deliver its product continuously but in discrete manner. This means that mass,
temperature, concentration, and other properties vary with time. In practice, most batch processes are
made up of a series of batch and semi-continuous steps. A semi-continuous step runs continuously with
periodic start-ups and shutdowns.

Batch processes:

are economical for small volumes

are flexible in accommodating changes

in product formulation

are flexible in changing production rate

allow the use of standardized multi-

purpose equipment for the production of a
variety of products from the same plantare
best if equipment needs regular cleaning
because of fouling or needs regular
sterilization

allow better product integrity: each

batch of product can be clearly identified in
terms of the feeds involved and conditions
of processing. This is particularly important
in industries such as pharmaceuticals and foodstuffs.

Batch distillation is often preferable to continuous distillation where relatively small quantities of
material are to be handled at regularly scheduled periods. It is often more economical for small
volumes productions.

Probably the most outstanding attribute if batch distillation is its flexibility. Little change is
required when switching from one mixture to another. It is flexible in accommodating changes
in product formulation, changes in production rate, changes in feed composition, etc. Batch
distillation allows the use of standardized multi-purpose equipment for the production of a
variety of products from the same plant. They are preferred when the equipment needs regular
cleaning because of fouling or regular sterilization.

Batch distillation may be preferable for processing temperature-sensitive materials, because

distillation pressure can be lowered as the MVC are removed, thus maintaining lower still pot
temperature within the constraint of the condenser temperature. The minimum pressure in
continuous distillation is constrained by the temperature required to condense the lowest-
boiling component, resulting in higher operating temperature.
Another important factor favouring the use of batch distillation is that it permits better product
integrity to be achieved: each batch of product can be clearly identified in terms of the feeds
involved and conditions of processing. This is particularly important in industries such as
pharmaceuticals and foodstuffs.

A disadvantage of batch distillation is the long time the mixture is exposed to high
temperatures. This increases the risk of thermal degradation or decomposition of the
substances. Furthermore, energy requirement is generally higher in batch distillation than in
continuous distillation.

Operation and Control of Batch Distillation System

Load Control

The distillation column load is represented by the vapour flow (or boil-up). The boil-up can be
manipulated by heat input to the batch still. If the heating medium is steam, a simple method is
to maintain constant steam pressure or flow rate to the batch still. This method produces a
constant vapour load if the boiling point difference between the components is small and no
significant temperature rise result from the rise in concentration in the residue. Temperature
difference control results in a constant heat transfer rate provided no significant fouling occurs
during the batch distillation cycle.

Reflux Control

This is used when operating with constant boil-up, the reflux rate can be manipulated to control
product quality. The two ways of operating the batch distillattion are:

(a) maintaining constant reflux ratio

(b) maintaining constant product quality (increasing reflux ratio)

In the first method, the reflux ratio is held constant during the run. The distillate becomes less
rich in MVC as the distillation progresses; and the residue in the still also becomes
progressively depleted in MVC The process starts with the distillation concentration beginning
at a value above the specifications and ending at a value below specifications. When the
average concentration of distillate collected reaches the specifications, the process is stopped.
Operation at constant reflux ratio is relatively simple. However, if a high purity product is
desired, with this method production is possible only to a very limited extent.

An alternative way of operating a batch distillation is to gradually increase the reflux ratio in
order to maintain constant a given distillate purity. The distillation is stopped when the reflux
ratio exceeds a certain pre-determined limit. In practice, operation at constant distillate
concentration is more laborious since the reflux ratio changes and must be continuously re-
adjusted.

In general, the energy requirement is lower with constant distillate concentration than with
constant reflux ratio. The difference is especially high for high purity distillations.

Between these 2 cases, there is an optimal mode of operation that trades off the additional
time, energy and labour needed. A precise calculation of optimal operation is possible with
sufficient data. Even when this is not available, an increase of reflux ratio during a batch
distillation is common. This is sometimes described as "squeezing the batch". Often this is
done in practice using a series of constant reflux ratio periods with increasing values of the
reflux ratio, perhaps also including periods of total reflux.

II. Review of Related Literature

Operating Line Equation for Batch Distillation

An important point about batch distillation (as in simple distillation) is that the concentration will
change continuously with time as distillation progresses. Batch distillation is also an unsteady-
state process.

We have seen from the analysis of simple distillation that the mole fraction of the more volatile
component in the distillate xD will gradually decrease with time as more and more distillate
is being produced. Similarly, the concentration of the more volatile component in the liquid
remained in the still xB will decreaseas more liquid is boiled-off.

Just like the continuous distillation system, we would like to obtain an operating line equation for
batch distillation.
(Remember : there is no feed section or stripping section for batch distillation)

To derive the operating line equation, perform a material balance for the more volatile
component:

Vn+1 yn+1 = Ln xn + D xD
 Assume constant molal overflow;
Vn+1 = Vn = ........ = V
Ln = Ln-1 = ........ = L

The rectifying operating line thus

becomes: V yn+1 = L xn + D xD

Now, from Vn+1 = Ln + D, we have V = L + D

Replacing for V and re-arranging, we have:

Introducing the reflux ratio R = L/ D,

and dropping the subscripts, we have
the operating line for batch distillation:

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The operating line is a straight line with the slope (R / R+1) and the intercept (xD / R+1).

The operating line can be plotted in the same way on the equilibrium curve to obtain
the number of theoretical stages. Because there is no feed section and stripping
section for batch distillation, no q-line or SOL needs to be plotted.
The number of theoretical stages required for the separation a mixture into a
distillate of concentration xD and residual (bottoms) of concentration xB is the number
of triangles that can be drawn between the operating line and the equilibrium line.
See the Figure below.
 The last triangle represents the batch still. There is no reboiler in batch distillation.

The theory is well developed for the prediction of distillation column operations. This section provides
an overview of some of the equations and theory associated with batch distillation. For additional
theory development, see Resources. In batch mode, with no feed, vapor from the reboiler rises up the
trays in the column and is finally liquefied in the condenser. This condensed liquid is either drawn off or
reintroduced into the top of the column. Each tray of the column is assumed to be in vapor-liquid
equilibrium. Geankoplis (1993) (see Resources) provides excellent diagrams illustrating the flows within
a distillation column and the equilibrium on each tray. Several approaches can be taken: • Graphical
Methods (McCabe-Thiele method and Ponchon-Savart method) • Shortcut Methods (e.g. Fenske-
Underwood-Gilliland method) • Rigorous plate-to-plate calculations (using computer software) The
graphical and shortcut methods are specifically for steady state operations. While they do not apply
directly to the unsteady operation of batch distillation (except for the special case of total reflux), they
can be useful in initially characterizing a column. For total reflux calculations, the Fenske equation (part
of the FUG Shortcut Method) can be used to determine the number of plates required for a given
separation. The rigorous plate-to-plate calculations can easily be performed with available computer
aided engineering flowsheet simulation programs or special purpose distillation programs.