Types of Distillation
Types of Distillation
Types of Distillation
There are many types of distillation columns, each designed to perform specific types of
separations, and each design differs in terms of complexity.
Batch and Continuous Columns
One way of classifying distillation column type is to look at how they are operated. Thus we
have:
batch and
continuous columns.
Batch Columns
In batch operation, the feed to the column is introduced batch-wise. That is, the column is
charged with a 'batch' and then the distillation process is carried out. When the desired task
is achieved, a next batch of feed is introduced.
Continuous Columns
In contrast, continuous columns process a continuous feed stream. No interruptions occur
unless there is a problem with the column or surrounding process units. They are capable of
handling high throughputs and are the most common of the two types. We shall concentrate
only on this class of columns.
Types of Continuous Columns
Continuous columns can be further classified according to:
where the extra feed exits when it is used to help with the separation,
extractive distillation - where the extra feed appears in the bottom product stream
azeotropic distillation - where the extra feed appears at the top product stream
tray column - where trays of various designs are used to hold up the liquid to provide
better contact between vapour and liquid, hence better separation
packed column - where instead of trays, 'packings' are used to enhance contact
between vapour and liquid
BASIC DISTILLATION EQUIPMENT AND OPERATION
Main Components of Distillation Columns
Distillation columns are made up of several components, each of which is used either to
tranfer heat energy or enhance materail transfer. A typical distillation contains several
major components:
a vertical shell where the separation of liquid components is carried out
a condenser to cool and condense the vapour leaving the top of the column
a reflux drum to hold the condensed vapour from the top of the column so that
liquid (reflux) can be recycled back to the column
The vertical shell houses the column internals and together with the condenser and reboiler,
constitute a distillation column. A schematic of a typical distillation unit with a single feed
and two product streams is shown below:
Thus, there are internal flows of vapour and liquid within the column as well as external
flows of feeds and product streams, into and out of the column.
COLUMN INTERNALS
Trays and Plates
The terms "trays" and "plates" are used interchangeably. There are many types of tray
designs, but the most common ones are :
Bubble cap trays
A bubble cap tray has riser or chimney
fitted over each hole, and a cap that
covers the riser. The cap is mounted so
that there is a space between riser and
cap to allow the passage of vapour.
Vapour rises through the chimney and is directed
downward by the cap, finally discharging through slots
in the cap, and finally bubbling through the liquid on the tray.
Valve trays
In valve trays, perforations are covered by liftable
caps. Vapour flows lifts the caps, thus self creating a
flow area for the passage of vapour. The lifting cap
directs the vapour to flow horizontally into the liquid,
thus providing better mixing than is possible in sieve
trays.
Valve trays (photos courtesy of Paul Phillips)
Sieve trays
Sieve trays are simply metal plates with holes in them.
Vapour passes straight upward through the liquid on
the plate. The arrangement, number and size of the
holes are design parameters.
Because of their efficiency, wide operating range, ease of maintenance and cost factors,
sieve and valve trays have replaced the once highly thought of bubble cap trays in many
applications.
Liquid and Vapour Flows in a Tray Column
The next few figures show the direction of vapour and liquid flow across a tray, and across a
column.
Each tray has 2 conduits, one on each side, called ‘downcomers’.
Liquid falls through the downcomers by gravity from one tray to the
one below it. The flow across each plate is shown in the above
diagram on the right.
A weir on the tray ensures that there is always some liquid (holdup)
on the tray and is designed such that the the holdup is at a suitable
height, e.g. such that the bubble caps are covered by liquid.
vapour distribution
on the tray. This is because better vapour-liquid contact means better separation at each
tray, translating to better column performance. Less trays will be required to achieve the
same degree of separation. Attendant benefits include less energy usage and lower
construction costs.
Liquid distributors - Gravity (left), Spray (right)
(photos courtesy of Paul Phillips)
Packings
There is a clear trend to improve separations by supplementing the use of trays by additions
of packings. Packings are passive devices that are designed to increase the interfacial area
for vapour-liquid contact. The following pictures show 3 different types of packings.
These strangely shaped pieces are supposed to impart good vapour-liquid contact when a
particular type is placed together in numbers, without causing excessive pressure-drop
across a packed section. This is important because a high pressure drop would mean that
more energy is required to drive the vapour up the distillation column.
Packed columns are called continuous-contact columns while trayed columns are
called staged-contact columns because of the manner in which vapour and liquid are
contacted.
COLUMN REBOILERS
There are a number of designs of reboilers. It is beyond the scope of this set of introductory
notes to delve into their design principles. However, they can be regarded as heat-
exchangers that are required to transfer enough energy to bring the liquid at the bottom of
the column to boiling boint. The following are examples of typical reboiler types.
Tubesheet
Fitting a Shell & Tube Heat Exchanger
(photo courtesy of Paul Phillips)
(photo courtesy of Paul Phillips)
a liquid is said to ‘boil’ when its vapour pressure equals the surrounding pressure
liquids with high vapour pressures (volatile liquids) will boil at lower temperatures
the vapour pressure and hence the boiling point of a liquid mixture depends on the
relative amounts of the components in the mixture
distillation occurs because of the differences in the volatility of the components in the
liquid mixture
The Boiling Point Diagram
The boiling point diagram shows how the equilibrium compositions of the components in a
liquid mixture vary with temperature at a fixed pressure. Consider an example of a liquid
mixture containing 2 components (A and B) - a binary mixture. This has the following
boiling point diagram.
This difference between liquid and vapour compositions is the basis for distillation
operations.
Relative Volatility
Relative volatility is a measure of the differences in volatility between 2 components, and
hence their boiling points. It indicates how easy or difficult a particular separation will be.
The relative volatility of component ‘i’ with respect to component ‘j’ is
defined as
Distillation columns are designed based on the boiling point properties of the components
in the mixtures being separated. Thus the sizes, particularly the height, of distillation
columns are determined by the vapour liquid equilibrium (VLE) data for the mixtures.
Vapour-Liquid-Equilibrium (VLE) Curves
Constant pressure VLE data is obtained from boiling
point diagrams. VLE data of binary mixtures is often
presented as a plot, as shown in the figure on the
right. The VLE plot expresses the bubble-point and
the dew-point of a binary mixture at constant
pressure. The curved line is called the equilibrium
line and describes the compositions of the liquid and
vapour in equilibrium at some fixed pressure.
Note the shapes of the respective equilibrium lines in relation to the diagonal lines that
bisect the VLE plots.
Both plots are however, obtained from homogenous azeotropic systems. An azeotrope that
contains one liquid phase in contact with vapour is called a homogenous azeotrope. A
homogenous azeotrope cannot be separated by conventional distillation. However, vacumn
distillation may be used as the lower pressures can shift the azeotropic point.Alternatively,
an additional substance may added to shift the azeotropic point to a more ‘favourable’
position.
When this additional component appears in appreciable amounts at the top of the
column, the operation is called azeotropic distillation.
When the additional component appears mostly at the bottom of the column, the
operation is called extractive distillation
The VLE curve on the left is also generated by an
azeotropic system, in this case a heterogenous
azeotrope. Heterogenous azeotropes can be identified
by the ‘flat’ portion on the equilibrium diagram.
Next, we will look at how VLE plots/data are used to design distillation columns.
heat effects (heats of solution, heat losses to and from column, etc.) are negligible
The design procedure is simple. Given the VLE diagram of the binary mixture, operating
lines are drawn first.
Operating lines define the mass balance relationships between the liquid and vapour
phases in the column.
There is one operating line for the bottom (stripping) section of the column, and on
for the top (rectification or enriching) section of the column.
Use of the constant molar overflow assumption also ensures the the operating lines
are straight lines.
Operating Line for the Rectification Section
The operating line for the rectification section is constructed as follows. First the
desired top product composition is located on the VLE diagram, and a vertical line
produced until it intersects the diagonal line that splits the VLE plot in half. A line with
slope R/(R+1) is then drawn from this instersection point as shown in the diagram
below.
R is the ratio of reflux flow (L) to distillate flow (D) and is called the reflux ratioand is
a measure of how much of the material going up the top of the column is returned
back to the column as reflux.
Operating Line for the Stripping Section
The operating line for the stripping section is constructed in a similar manner.
However, the starting point is the desired bottom product composition. A vertical line
is drawn from this point to the diagonal line, and a line of slope Ls/Vs is drawn as
illustrated in the diagram below.
Ls is the liquid rate down the stripping section of the column, while Vs is the vapour
rate up the stripping section of the column. Thus the slope of the operating line for
the stripping section is a ratio between the liquid and vapour flows in that part of the
column.
Equilibrium and Operating Lines
The McCabe-Thiele method assumes that the liquid on a tray and the vapour above it
are in equilibrium. How this is related to the VLE plot and the operating lines is
depicted graphically in the diagram on the right.
A magnified section of the operating line for the stripping section is shown in relation
to the corresponding n'th stage in the column. L's are the liquid flows while V's are
the vapour flows. x and y denote liquid and vapour compositions and the subscripts
denote the origin of the flows or compositions. That is 'n-1' will mean from the
stage below stage 'n' while 'n+1' will mean from the stage above stage 'n'. The
liquid in stage 'n' and the vapour above it are in equilibrium, therefore, x n and yn lie
on the equilibrium line. Since the vapour is carried to the tray above without changing
composition, this is depicted as a horizontal line on the VLE plot. Its intersection with
the operating line will give the composition of the liquid on tray 'n+1' as the
operating line defines the material balance on the trays. The composition of the
vapour above the 'n+1' tray is obtained from the intersection of the vertical line from
this point to the equilibrium line.
Number of Stages and Trays
Doing the graphical construction repeatedly will give rise to a number of 'corner'
sections, and each section will be equivalent to a stage of the distillation. This is the
basis of sizing distillation columns using the McCabe-Thiele graphical design
methodology as shown in the following example.
Given the operating lines for both
stripping and rectification sections, the
graphical construction described above
was applied. This particular example
shows that 7 theoreticalstages are
required to achieve the desired
separation. The required number of trays
(as opposed to stages) is one less than
the number of stages since the graphical
construction includes the contribution of
the reboiler in carrying out the
separation.
Typical values for tray efficiency ranges from 0.5 to 0.7 and depends on a number of
factors, such as the type of trays being used, and internal liquid and vapour flow
conditions. Sometimes, additional trays are added (up to 10%) to accomodate the
possibility that the column may be under-designed.
The Feed Line (q-line)
The diagram above also shows that the binary feed should be introduced at the 4'th
stage. However, if the feed composition is such that it does not coincide with the
intersection of the operating lines, this means that the feed is not a saturated liquid.
The condition of the feed can be deduced by the slope of the feed line or q-line. The
q-line is that drawn between the intersection of the operating lines, and where the
feed composition lies on the diagonal line.
q = 0 (saturated vapour)
q = 1 (saturated liquid)
0 < q < 1 (mix of liquid and vapour)
q > 1 (subcooled liquid)
q < 0 (superheated vapour)
Consider as a base case, a 10 stage column. The feed is a binary mixture that has a
composition of 0.5 mole fraction in terms of the more volatile component, and
introduced at stage 5. The steady-state terminal compositions of about 0.65 at the
top (stage 1) and 0.1 at the bottom (stage 10) are shown below:
Composition Profile: 10 stages, feed at stage 5
Suppose we decrease the number of stages to 8, and keep the feed at the middle
stage, i.e. stage 4. The resulting composition profile is:
We can see that the top composition has decreased while the bottom composition has
increased. That is, the separation is poorer.
Now, if we increase the number of stages to 12, and again introduce the feed at
mid-column, i.e. stage 6, the composition profile we get is:
Composition Profile: 12 stages, feed at stage 6
Again, the composition has changed. This time the distillate is much richer in the
more volatile component, while the bottoms has less, indicating better separation.
As the feed stage is moved lower down the column, the top composition becomes less
rich in the more volatile component while the bottoms contains more of the more
volatile component. However, the changes in top composition is not as marked as the
bottoms composition.
The preceding examples illustrate what can happen if the position of the feed tray is
shifted for this particular system. They should not be used to generalise to other
distillation systems, as the effects are not straightforward.
state of feed
composition of feed
trace elements that can severely affect the VLE of liquid mixtures
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 refluxconditions, i.e.
there is no withdrawal of distillate.
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 reboiler duty).
Vapour Flow Conditions
Adverse vapour flow conditions can cause
foaming
entrainment
weeping/dumping
flooding
Foaming
Foaming refers to the expansion of liquid due to passage of vapour or gas.
Although it provides high interfacial liquid-vapour 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 vapour up to the tray above and is
again caused by high vapour 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 vapour flow. The pressure exerted by the
vapour 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 vapour flow, causing liquid to be
entrained in the vapour up the column. The increased pressure from excessive
vapour also backs up the liquid in the downcomer, 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.
Reboiler Temperature
As a reboiler slowly plugs on the tube side, the bottoms temperature goes down
and this leads to low vapor flow. Online monitoring of the heat transfer
coefficient in control system can identify this problem early on along with the
monitoring of bottoms temperature. A self cleaning heat exchanger when used
in place of a reboiler can mitigate this problem.
Reduction in Vacuum
A slight drop in vacuum causes the boiling point(s) to go up, leading to low
vapour flow, loss of production and and off spec products.
Wet Feed
If a column is typically fed a dry hydrocarbon feed but the feed becomes
contaminated with water then at some point, when the water/ hydrocarbon
mixture enters the tower the water can vaporize so rapidly that it causes an
over pressure event. This can and will damage trays. This effects column
efficiency and product quality.
Column Diameter
Most of the above factors that affect column operation is due to vapour flow conditions:
either excessive or too low. Vapour flow velocity is dependent on column diameter.
Weeping determines the minimum vapour flow required while flooding determines the
maximum vapour 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 Packings
Remember that the actual number of trays required for a particular separation duty is
determined by the efficiency of the plate, and the packings if packings 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
reboiler must be appropriately sized to ensure that enough vapour 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. COSTELLO can provide engineering design for new
columns and support/ troubleshooting for existing columns. Our engineers have extensive
experience in column instrumentation and controls.
Types of Distillation
Simple distillation
Fractional distillation
Steam distillation
Vacuum distillation
Air-sensitive vacuum distillation
Short path distillation
Zone distillation
Simple Distillation:
The vapor is immediately channeled into a condenser. Consequently, the distillate is not pure but rather its composition is identical to the
composition of the vapors at the given temperature and pressure.
Simple Distillation
Fractional Distillation:
It is used in order to separate the components by repeated vaporization-condensation cycles within a packed fractionating column. This
separation, by successive distillations, is also referred to as rectification.
Steam Distillation:
Steam Distillation is a method of distilling compounds which are heat-sensitive. The temperature of the steam is easier to control than the
surface of a heating element. This allows a high rate of heat transfer without heating at a very high temperature.
Vacuum Distillation:
Some compounds have very high boiling points. Sometimes its easier to lower the pressure than to reach its high boiling point. This
technique is referred to as vacuum distillation and it is commonly found in the laboratory in the form of the rotary evaporator.
Air-Sensitive Vacuum Distillation:
Some compounds have high boiling points as well as being air sensitive. For these compounds, a simple vacuum distillation system can
be used. Wherein the vacuum is replaced with an inert gas after the distillation is complete.
Short Path Distillation:
It is a distillation technique that involves the distillate traveling a short distance, often only a few centimeters. This technique is normally
done at reduced pressure allowing a lower operating temperature range.
Zone Distillation:
It is a distillation process in a long container with a special arrangement. With the partial melting of refined matter in moving liquid zone
and condensation of vapor in the solid phase at condensate pulling in cold area.
For more detailed information about Distillation and other concerned topics, download BYJU’S – The Learning App.
Simple Distillation
If water is placed in a sealed container and allowed to evaporate, it will eventually reach an equilibrium such
that the water vapor is condensing just as fast as the water is evaporating. The pressure of the vapor at this
equilibrium is called the vapor pressure. Vapor pressure is different for different substances and varies with
temperature. In a mixture of two liquids with different boiling points, the vapor will have more of the liquid that is
more volatile, i.e., evaporates more readily. In simple distillation, the liquid mixture is heated and the vapor
rises through a tube and is collected and recondensed. The recondensed liquid will have a higher concentration
of the more volatile component than the original mix. If the two liquids in the original mix have widely different
boiling points, a one-step evaporation and recondensation process is all that is necessary. This process is
Fractional Distillation
Fractional distillation is similar to simple distillation, except the same process is repeated in successive cycles.
Each cycle produces a mixture richer in the more volatile compound than the mixture before it. Fractional
distillation is necessary when the boiling points of the liquids in the original mix are close enough to each other
Vacuum Distillation
Some liquids boil at such high temperatures that simple or fractional distillation using the process described
above would be impractical or dangerous. Vacuum distillation, however, offers another alternative. The boiling
point of a liquid falls when the pressure is reduced. The boiling point of water, for example, is lower at high
altitude than at sea level. By reducing the pressure in the container, the boiling point of the liquids in the
mixture can be reduced and the mixture distilled at a lower temperature. This technique is called vacuum
distillation.
Azeotropic Distillation
Owing to the intermolecular attractions between molecules in the mixture, mixtures may have a higher or lower
boiling point than either of their components. A mixture of this kind is called an azeotrope. When the liquids in
the azeotrope evaporate, the vapor has the same composition as the mixture, so azeotropes cannot be distilled
using the techniques described above. They can still be distilled, however, but only through one of several
other methods.
In extractive distillation, a solvent that will mix freely with one component but not the other is added to the
mixture. The new mixture can then be separated by distillation. In reactive distillation, by contrast, a chemical
that will react with one agent but not the other is added, creating a new mixture that can be separated by
distillation. Finally, adding ionic salts may alter the volatilities of the compounds in the mix in such a way that
they can be distilled. These three techniques are collectively called azeotropic distillation.