Design of Distillation Column
Design of Distillation Column
❖ INTRODUCTION
• In simple terms, vaporization followed by condensation is known as distillation. It is a
method of separating components of solution which are relatively volatile. Distillation
is the most widely used separation method in chemical industries. Simple distillation or
batch distillation was known in first century. Multistage counter current distillation was
invented in 1830 by Aeneas Coffey of Dublin1.
• He used tray lower for separating 95.6% ethanol (by mass) from its dilute solution in
water. But as of today 100% reliable method for designing of distillation column, which
can be applied to all systems without any limitation, is not available. All methods have
limitations. Hence process design engineers use more than one method for the design of
distillation column. For an entirely a new mixture, it is better to verify the design of its
distillation column first on the pilot plant scale column before applying it at commercial
or large scale.
❖ CRITERIA OF SELECTION
• For a given mixture, if all the components are relatively volatile and are required to be
separated in pure form, then distillation is the first choice. If the relative volatility of
the two adjacent components is very high, then evaporation is preferred. For example,
concentration of orange juice.
• If relative volatility of two adjacent components is very low: close to I (e.g. 10 to 30%,
by mass acetic acid in water) or equal to 1 (e.g. azeotropic mixture, 95.6% by ethanol
in water), special type of distillation like Azeotropic Distillation or Extractive
Distillation is used. For the same case, liquid-liquid extraction, membrane separation
or crystallization may be more economical. Examples: (a) For the separation of pure
acetic acid from 10% (by mass) aqueous acetic acid solution, liquid-liquid extraction
using ethyl acetate as solvent is more economical than azeotropic distillation of the
same solution using butyl acetate or ethyl acetate as an entrainer. (b) For the separation
of pure ethanol from its azeotropic mixture with water. [95.6% ethanol (by mass) in
ethanol- water solution], pervapouration unit consumes less than 20% of the energy,
than that used in azeotropic distillation. Also, for the same separation, pervapouration
unit requires low pressure steam (to maintain 80o C temperature) which can be
obtained by flashing the condensate of high pressure steam, (c) For the separation of
xylene from the mixed xylenes, crystallization is used. If the separation of only one
component is required rather than a separation of all the components of the mixture,
then absorption, stripping or liquid-liquid extraction may be more economical than
distillation.
• Examples: (a) For the separation of penicilin from the complex mixture, liquid-liquid
extraction is used. (b) For the removal of hydrogen and methane from aromatics,
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Chapter Name: Distillation
stripping is used. (c) For the removal of propane from the mixture called asphalt,
stripping is used. Volatility of propane is very high compared to volatilities of other
components of the asphalt. (d) For the removal of hydrogen sulphide from the
natural gas mixture, absorption using ethanolamines as solvent is used. (e) For
removal of ammonia from lean aqueous solution, steam stripping is preferred. (f) If
all components of air are to be separated in pure form (nitrogen, oxygen, argon, etc.)
cryogenic distillation is preferred. But if only nitrogen in pure form is to be separated
from air then pressure swing adsorption (PSA) is preferred.
❖ SELECTION OF EQUIPMENT FOR DISTILLATION
In most of the cases, distillation is carried out either in a tray tower or in a packed tower.
Criteria of selection between tray tower and packed tower are as follows.
(a) For high vacuum distillation, a packed tower is selected. Packed tower generally
provides lower pressure drop as compared to the tray tower. For example in the
distillation of the mixture of monochloroacetic acid and acetic acid, absolute operating
pressure in the reboiler should be less than 50 torr a to avoid thermal cracking of bottom
product (monochloroacetic acid). For this case, packed tower should be selected. Packed
tower provides lower residence time for liquid as compared to tray tower. The rate
ofthermal cracking is directly proportional to residence time. For highly heat sensitive
product, decrease in boiling point means improvement in the quality. The rate of thermal
cracking increases exponentially with the temperature. For very high vacuum
distillation, short path distillation is used. Example: Separation of vitamin E from its
crude mixture (such as soybean oil deodorizer distillate) is carried out in short path
distillation equipment. Operating absolute pressure in short path distillation can be as
low as 0.05 mbar or 50 pbar a.
(b) For very small tower diameter packed tower is preferred. With large tower diameter,
tray tower is preferred. With very small diameter (less than 150 mm), fabrication oftrays
is difficult while with large diameter, liquid distribution is difficult in the packed tower.
(c) For handling higher ratio of liquid flow rate to vapour flow rate, packed towers are
preferred. For very law liquid flow rate, tray tower is selected. But for very low L/V
ratio, tray tower is selected. Packed tower requires minimum wetting rate to work
efficiently.
(d) For corrosive system, packed tower with plastic packings like polypropylene
packings, glass fibre reinforced plastic packings, etc. is more economical than tray tower
made from special metal alloys. Example: For the separation of methyl iodide and acetic
acid, packed tower with glass fibre reinforced plastic packings is more economical than
tray tower which should be entirely made from Hastalloy-B.
(e) If the side products are to be drawn from the distillation column, like the distillation
columns of refinery, tray tower is preferred.
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Chapter Name: Distillation
❖ DISTILLATION COLUMN DESIGN
The design of a distillation column can be divided into the following steps.
(a) If the feed mixture contains more than two components, then select two key
components from all the components of feed mixture.
(b) Decide the operating pressure of distillation column. At the operating pressure, find
the vapour-liquid equilibrium data.
(c) Specify the degree of separation required. In case of a binary distillation, decide the
top (distillate) and the bottom (residue) product compositions. In case of
multicomponent distillation, decide the distribution of key components in distillate and
residue. Also, find the distribution of non key components in the same. Complete the
material balance.
(d) Determine the minimum reflux ratio Rm.
(e) Determine the optimum reflux ratio R and find the number of theoretical or
equilibrium stages required for the desired separation.
(f) Select the type of tower: tray lower or packed tower (as discussed in Sec. 8.3). Select
the type of tray in tray tower or type of packing in packed tower.
(g) Find tower diameter and pressure drop across the tower. Decide the top
disengagement and bottom disengagement spaces.
(h) Determine the tray efficiency and find the actual number of trays in case of tray
tower or find HETP (height equivalent to theoretical plate) and decide the height of
packing in packed tower. In case of packed tower, design the liquid distributor,
redistributor, packing support, etc.
(i) Select the material of construction for all parts. Design the suitable insulation system.
(j) Design the condenser and reboiler.
(k) Decide the control methodology for the distillation column, line sizes and locations
of all nozzles.
(1) Mechanical design of distillation column which also includes design of skirt support
for the distillation column. Calculation and equations for the first five steps are different
for binary and multicomponent distillation. In this chapter first eight steps are discussed
in detail
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Chapter Name: Distillation
distillate vapour. For this, bubble point of distillate (in case of total condenser) should
be sufficiently greater than cooling water temperature.
In case of partial condenser, bubble point of reflux (is equal to dew point of distillate
vapour) should be sufficiently greater than temperature of cooling water. But if, this
operating pressure (based on cooling water temperature) is calculated to be very high,
then chilled water or brine can be considered as cooling medium for the overhead
condenser.
Operating pressure in distillation column is always less than the critical pressure of top
product or temperature of cooling medium of overhead condenser cannot be greater than
critical temperature of top product.
In many cases, distillation is carried out under vacuum to avoid the thermal degradation
of heat sensitive product or to facilitate the use of cheaper heating medium like saturated
steam in reboiler or to alter the vapour-liquid equilibrium data.
Examples for the Selection of Operating Pressure:
(i) Distillation of acetaldehyde-ethanol-water mixture is carried out at about 3 atm g
pressure. Pure acetaldehyde is the top product. Normal boiling point (t B) of
acetaldehyde is 20.2o C. To facilitate the use of cooling water as a cooling
medium in the overhead condenser, boiling temperature or condensation
temperature of acetaldehyde should be sufficiently greater than the design
temperature of cooling water from cooling tower (say 320 C). Also the product
acetaldehyde is stored in bullet type storage tanks which are exposed to
atmosphere. Hence, to reduce the cost of storage or to avoid the use of insulation
around storage tank and to avoid the use of any refrigeration system for the
storage tank, boiling point of acetaldehyde should be sufficiently greater than
atmospheric temperature (50o C-maximum). Considering all these aspects,
condensation temperature (is also equal to boiling temperature of pure
component) of acetaldehyde is fixed at around 60o C. For getting 60o C as a
condensation temperature of acetaldehyde, required operating pressure at the top
of distillation column is around 3.6 atm g (vapour pressure of acetaldehyde at 60o
C).
(ii) For the separation of methyl chloride from the mixture of chloromethanes, normal
boiling point or condensation temperature of pure methyl chloride is -240 C. At
10 atm a pressure, its condensation temperature is 47.30 C. Hence to facilitate the
use of cooling water as a cooling medium in overhead condenser, this distillation
column can be operated at 10 atm a pressure. Similarly in case of distillation of
ammonia, saturation pressure of ammonia at 40o C is 1555.5 kPa a. Hence, the
column is operated at about 15 bar g to facilitate condensation of ammonia at 40o
C in the condenser with cooling water at 320 C.
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Chapter Name: Distillation
❖ Vacuum Distillation:
For heat sensitive material or to facilitate the use of cheaper heating medium in reboiler
or to alter the vapour-liquid equilibrium data, distillation column is operated under
vacuum. Advantages and disadvantages of vacuum distillation are:
Advantages:
(a) It prevents thermal decomposition of heat sensitive material. Example: In separation
of monochloroacetic acid and acetic acid by distillation, monochloroacetic acid is
obtained as bottom product. Boiling point of monochloroacetic acid must be restricted
below 120o C, otherwise thermal degradation can take place. If the boiling point of
monochloroacetic acid is kept at 109o C, then operating pressure at bottom of column
must be equal to 40 torr (absolute).
(b) It allows the use of more economical heating medium such as saturated steam against
hot oil in high capacity plant. Example: For the separation of ethylene glycol-water
mixture by distillation, ethylene glycol is obtained as bottom product. Its normal boiling
point is 1970 C. Use of saturated steam as a heating medium could be economical up to
180o C. Hence, this column is better to be operated under vacuum to facilitate the use
of saturated steam against the use of hot oil.
(c) It requires fewer stages or lower reflux ratio or both in many cases where relative
volatility increases with decrease in the operating pressure.
(d) In some case vacuum breaks the azeotrope and make the separation easier. Example:
If the distillation of ethanol water mixture is earned out below 70 torr absolute pressure,
azeotrope does not form.
(e) It reduces undesirable side reactions, if they are taking place. Example: Distillation
of ethyl benzene-styrene mixture under vacuum reduces polymerization.
(f) Vacuum distillation provides safety in the distillation of toxic or hazardous material.
Example: For the separation of nearly 100% pure nitric acid from the azeotropic mixture
of nitric acid and water, extractive distillation is used. This extractive distillation uses
concentrated sulphuric acid as solvent. Material of construction of this column is
borosililate or high quality glass. This column is operated under slight vacuum for safety
purpose. Here, vacuum also facilitates the use of saturated steam in reboiler.
(g) It increases product recovery when dealing with maximum temperature constraints.
Example: Refinery vacuum tower.
Disadvantages of Vacuum Distillation:
(a) It requires larger column diameter and larger diameter vapour line.
(b) Because of the reduction in condensation temperature, costlier cooling source may
be required for condensation.
(c) Presence of air as a non-condensable reduces the efficiency of main condenser.
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Chapter Name: Distillation
(d) Increases the possibility of contamination of products by air or other components of
atmosphere.
Step 3: Degree of Separation
In case of binary distillation, specify xD and xw considering equilibrium limitations in
mind, (where xD = mole fraction of more volatile component in distillate and x w = mole
fraction of more volatile component in residue). Find the molar flow rate of distillate D
and molar flow rate of residue W, by using following two material balance equations
where Zf represents mole fraction of more volatile component in feed. Since feed can
be saturated liquid, saturated vapour or a mixture of liquid and vapour, symbol z F is
used. If it is only liquid, symbol xF can be used. To establish the material balance in
multicomponent distillation is not easy. In case of multicomponent distillation, specify
the distribution of two key components in distillate (top product) and in residue (bottom
product), considering equilibrium limitations in mind. Exact distribution of non-key
components in top product and bottom predict is not possible at the starting of design.
But, the same can be determined approximately by Hegstebeck and Geddes equation.
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Chapter Name: Distillation
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Chapter Name: Distillation
(i) For any equilibrium stage, molar latent heat of vaporization of liquid on tray is
equal to molar latent heat of condensation of vapour leaving the tray.
(ii) Heat losses and heat of solution (or say mixing) are negligible.
(iii) Total condenser is used but there is no subcooling. Condenser removes all the
latent heat from the overhead vapour but does not cool the resulting liquid further.
Because of the first two assumptions, molar flow rate of liquid and molar flow rate of
vapour in each section (enriching section and stripping section) is assumed to remain
constant throughout the section. Because of the third assumption, composition of
overhead vapour is equal to composition of distillate and also equal to composition of
reflux.
L, G, L–, G– = constant xD = yi = xo
where, L, G = Molar flow rates of liquid and vapour, respectively in rectification or
enriching section, kmol/h.
L–, G– = Molar flow rates of liquid and vapour, respectively in stripping or
exhausting section, kmol/h.
xD = Mole fraction of more volatile component in overhand vapour xo = Mole fraction
of more volatile component in reflux
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Chapter Name: Distillation
• Draw the stripping or exhausting section operating line. It starts from the point x = y
= xW passing through the point of intersection of enriching section operating line and
the q line. Operating line of the exhausting (or stripping section) is represented by the
following equation:
where ym+1 is the vapour composition of light component of the tray above m-th tray
and xm is the liquid composition of light component on m-th tray. = L + F · q and V– =
L– – W
• Starting from xD to xW or from xW to xD, carry out the stepwise construction between
operating lines and equilibrium curve. Total number of steps is equal to number of
theoretical or equilibrium stages required for the desired separation.
It is the most widely used short cut method for determining number of equilibrium
stages for multicomponent distillation. In this method first minimum reflux ratio Rin is
determined by Underwood's method. Then Fenskey's equation is used to find the
minimum number of theoretical stages required for the desired separation. Fenskey's
equation
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Chapter Name: Distillation
Selection of Tray Type: Different types of trays used in tray tower are
(i) sieve tray, (ii) bubble cap tray, (iii) valve tray, (iv) Linde trays and other modified
sieve trays.
Various factors that must be considered for the selection of tray type are
(a) cost (b) capacity (c) operating range, (d) efficiency and (e) pressure drop
(a) Cost: Bubble cap tray is the costliest type of tray. With mild steel as a material of
construction, the ratios of cost Bubble cap: Valve: Sieve trays = 3: 1.5:1 (general
guideline) In other words, cost of bubble cap tray is three times the cost of sieve tray
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Chapter Name: Distillation
and double the cost of valve tray with mild steel as material. With different materials
these ratios are somewhat different.
(b) Capacity: If tower diameter required for given flow rates is more it means capacity
of tray is less. The ranking for capacity is in order of modified sieve tray, sieve tray,
valve tray and bubble cap tray. In other words for the given flow rates, tower diameter
required is maximum with bubble cap trays and minimum with modified sieve tray.
However, the difference in the values of tower diameters is not large.
(c) Operating range: It is an important factor for the selection of tray. Operating range
of tray means range of liquid and vapour flow rates over which tray works satisfactorily.
Bubble cap tray provides the maximum operating range while sieve tray provides the
minimum operating range. Operating process plants are designed and operated with
some maximum capacity and also for some minimum capacity. Hence, distillation
columns are operated in the range of some maximum feed flow rate to minimum feed
flow rate. The ratio of maximum flow rate to minimum flow rate is called turndown
ratio. Some process plants are frequently operated at very high turndown ratio to meet
the product's demand and to avoid the shut down and start-up conditions as during shut
down and start-up periods, operating plant provides very poor efficiency. For higher
turndown ratio, bubble cap trays are preferred. Valve trays also offer more flexibility
or higher turn down ratio than the sieve trays. However, in actual plant operation, valves
get stuck-up or fly-away if operating conditions are frequently changed. In such a case,
valve trays loose efficiency.
(d) Efficiency: This factor is not generally considered for the selection of tray type.
Efficiency of trays are almost same, if they are operated at design flow rates, or with
minimum turn down. However, bubble cap columns give good efficiency over a wider
range of turn down in general.
(e) Pressure drop: Pressure drop over the tray and for entire column is important for
vacuum distillation for which a packed tower is the first choice. But for the low vacuum
(upto 700 torr) operation, tray tower can be selected to get other advantages.
For example, to get the better vapour -liquid contact in large diameter column or to
facilitate the side draws. Among the trays, sieve tray provides the lowest pressure drop,
followed by valve tray, while bubble cap provides the highest pressure drop. Sieve trays
and modified sieve trays are the cheapest and are satisfactory for the majority ofthe
applications. Nowadays, majority of chemical plants are having automatic and precise
control system and hence flow rates are not much fluctuating. However, to meet the
fluctuation in the demand of product, some plants are intentionally operated with
different flow rates or capacities. To handle the higher turn down ratio, valve trays or
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Chapter Name: Distillation
bubble cap trays are considered. Valve trays are cheaper than bubble cap trays but they
are not suitable for very low vapour rate. Bubble cap tray provides higher efficiency
even with low vapour flow rate.
Flooding in sieve tray tower fixes the upper limit of vapour velocity through the tower.
Velocity of vapour at which flooding in sieve tray tower occurs is called flooding
velocity, vF. Tower diameter of sieve tray column is decided based on the value of vF.
Actual velocity or design velocity through distillation column should be in the range of
70 to 90% of flooding velocity. Ideally it should be in between 80 to 85%. Flooding is
an inoperative condition.
After finding the tower diameter, liquid flow pattern over sieve tray is decided.
Common liquid flow patterns of cross flow sieve tray are shown in Fig
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Chapter Name: Distillation
7.4 Weir
The height of weir decides the height of liquid over the tray. In most cases, weirs are
straight and rectangular plates. With bubble cap trays, to compensate the fluctuations
in the flow rate, V-notch type weirs are used. A high weir provides higher plate
efficiency but at the expense of pressure drop. For a distillation column operating above
atmospheric pressure, weir height is kept in between 40 mm to 90 mm; while 40 mm
to 50 mm is more common. For vacuum operation, to control the tray pressure drop,
weir height is reduced and it is kept in between 6 to 12 mm. In old designs, inlet weir
was also used, but in recent designs inlet weir is not recommended as it results in
hydraulic jump. Weir length fixes area of segmental downcomer. Weir length is
normally kept in between 0.6 to 0.85 times column diameter. For the first trial
calculations, weir length can be taken as 0.77D, and equivalent down comer area is
12%. Decrease in weir length increases the net area of tray and decreases the tower
diameter, but it decreases the down comer area, increases the pressure drop in down
comer and also decreases the volume of down comer. It also elevates the liquid level in
down comer. Increase in weir length increases the tower diameter. Hence, balanced
weir length and weir height are required.
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Chapter Name: Distillation
At a very low value of vapour velocity liquid rain down through the perforations. This
phenomena is known as weeping. It is again an inoperative condition. Minimum
vapour velocity required to avoid the weeping is given by Eduljee's equation.
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Chapter Name: Distillation
The height of an equivalent equilibrium stage or theoretical plate (HETP) is the height of packing that
gives the same separation as an equilibrium stage. HETP for the given type and size of random
packing is nearly constant and is nearly independent of the system physical properties. HETP values
available in literature are valid only for good liquid distribution and for the reasonable pressure drop.
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Solved sums:
Questions
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Questions
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