Sequencing of separation

columns
The design of distillation systems comprise only simple
columns. These simple columns employ:
• one feed split into two products;
• key components adjacent in volatility, or any components
that exist in small quantities between the keys will
become impurities in the products;
• a reboiler and a condenser.

If there is a three-component mixture to be separated into

three relatively pure products and simple columns are
employed, then the decision is between two sequences,
direct sequence in which the lightest component is taken
overhead in each column.
indirect sequence, takes the heaviest component as
bottom product in each column.
• If the distillation columns have both reboiling and
condensation supplied by utilities, then the direct
sequence often requires less energy than the
indirect sequence. This is because the light
material (Component A) is only vaporized once
in the direct sequence.

• However, the indirect sequence can be more

energy-efficient if the feed to the sequence has
a low flow rate of the light material and a high
flow rate of heavy material. In this case,
vaporizing the light material twice in the indirect
sequence is less important than feeding a high
flow rate of heavy material to both of the
columns in the direct sequence.
PRACTICAL CONSTRAINTS or HEURISTICS
Process constraints often reduce the number of options
that can be considered. Examples of constraints of this
type are:

1. Safety considerations might dictate that a particularly

hazardous component be removed from the sequence
as early as possible to minimize the inventory of that
material.
2. Reactive and heat-sensitive components must be
removed early to avoid problems of product degradation.
3. Corrosion problems often dictate that a particularly
corrosive component be removed early to minimize the
use of expensive materials of construction.
4. If thermal decomposition in the reboilers product, then
this dictates that finished products cannot be taken from
the bottoms of columns.
5. Some compounds tend to polymerize when distilled
unless chemicals are added to inhibit polymerization.
These polymerization inhibitors tend to be non-volatile,
ending up in the column bottoms. If this is the case, it
normally prevents finished products being taken from
column bottoms.

6. There might be components in the feed to a distillation

sequence that are difficult to condense. Total
condensation of these components might require low-
temperature condensation using refrigeration and/or high
operating pressures. Condensation using both
refrigeration and operation at high pressure increases
operating costs significantly. Under these circumstances,
the light components are normally removed from the top
of the first column to minimize the use of refrigeration
and high pressures in the sequence as a whole.
7. Separations where the relative volatility of the key
components is close to unity or that exhibit
azeotropic behavior should be performed in the
absence of nonkey components. In other words, do
the most difficult separation last.
8. A component composing a large fraction of the feed
should be removed first. And favor splits in which
the molar flow between top and bottom products in
individual columns is as near equal as possible.
Example: Each component for the mixture of alkanes in Table is to be
separated into relatively pure products. Table shows normal boiling
points and relative volatilities to indicate the order of volatility and
the relative difficulty of the separations. The relative volatilities have
been calculated on the basis of the feed composition to the
sequence, assuming a pressure of 6 barg using the Peng–Robinson
Equation of State with interaction parameters set to zero. Different
pressures can, in practice, be used for different columns in the
sequence and if a single set of relative volatilities is to be used, the
pressure at which the relative volatilities are calculated needs, as
much as possible, to be chosen to represent the overall system.
Use the heuristics to identify potentially good sequences that are
candidates for further evaluation.
Heuristic 1. Do D/E split last
since this separation has
the smallest relative
volatility.
• Again the heuristics are in conflict. Heuristic 1
again suggests doing the D/E split last, whereas
again Heuristic 3 suggests it should be done first.
Heuristic 2 suggests the B/C split first and
Heuristic 4 the C/D split first.
• Rather than relying on heuristics that are qualitative,
and an be in conflict, a quantitative measure of the
relative performance of different sequences would be
preferred. A physical measure that can be readily
calculated is the vapor flow up the columns. This
provides an indication of both capital and operating
costs.
• There is clearly a relationship between the heat duty
required for the reboiler and condenser to run the
distillation and the vapor rate since the latent heat of
vaporization relates these parameters.
•The heat duty in the reboiler relates directly to the cost of hot
utility for the distillation (e.g. cost of steam).

•The heat duty in the condenser relates directly to the cost of cold
utility for the distillation (e.g. cost of cooling water or refrigeration).

• However, there is also a link between vapor rate and capital cost,
since a high vapor rate leads to a large diameter column. High
vapor rate also requires large reboilers and condensers. Thus,
vapor rate is a good indication of both capital and operating costs
for individual columns.
we know that Underwood Equations can be used to
calculate the minimum reflux ratio. A simple mass
balance around the top of the column for constant molar
overflow, at minimum reflux gives:
Vmin = D(1 + Rmin)
where Vmin = minimum vapor load
Rmin = minimum reflux ratio
D = distillate flowrate
Equation can also be written at finite reflux, Defining RF to
be the ratio R/Rmin (typically R/Rmin = 1.1):
V = D(1 + R/Rmin)

If the feed is partially vaporized, the vapor flow below the

feed will be lower than the top of the column.
For above ambient temperature separations, the cost of
operating the distillation will be dominated by the heat
load in the reboiler and the vapor flow in the bottom of the
column.
• For below ambient temperature separations, the cost of
operating the column will be dominated by the cost of
operating the refrigerated condenser and hence the
vapor flow in the top of the column.
• If constant molar overflow is assumed, the vapor flow in
the bottom of the column V is related to the vapor flow in
the top of the column by
V = V’ – F(1 − q)
where V = vapor flow below the feed
V’ = vapor flow above the feed
F = feed flow rate
q = thermal condition of the feed
=heat required vaporize one mole of feed
molar latent heat of vaporization of feed
= 0 for saturated vapor feed,
or 1 for saturated liquid
 SEPARATING A FIVE-COMPONENT ALCOHOL MIXTURE
• Suppose we have a mixture of five alcohols that we shall label
A, B, C, D, and E with flows in the feed of I, 0.5, I, 7, and 10
molls respectively, for a total of 19.5 moles.
• Suppose further that their relative volatilities are 4.3, 4, 3, 2,
and 1 respectively.
• For example, for a column to split D from E, having C present will increase the
minimum vapor flow by 2.000 molls, having B present by 0.800 molls, and so on.
Having both C and B present will add 2.000 + 0.800 = 2.800 molls to the minimum
vapor flow.

Marginal Vapor Flows Estimated

for Nonkey Species for Alcohol Example
A B C D E
A/B 2.6 6.5 3.2
B/C 5.3 - 9.3 4.0
C/D 2.4 1.3 - 6.7
D/E 1.5 0.8 2.0
• we tabulate the total
marginal vapor flows for all
the columns that can exist
in any of the separation
processes possible based
on simple distillation
columns.
• They are placed in such a
way that we can more easily
see the total flows for each
of the different sequences
we can construct.

• For example, suppose we select the

direct sequence. From this figure, the
marginal flows should be for AlBCDE,
B/CDE, and C/DE for a total of 12.3 +
13.3 + 6.7 = 32.2 moles.
 A B C D E
A/B 2.6 6.5 3.2
B/C 5.3 - 9.3 4.0
C/D 2.4 1.3 - 6.7
D/E 1.5 0.8 2.0
• We wish to find the sequence with the minimum sum of
marginal flows. We can readily do this from this figure by
performing a branch and bound search.

• We start by comparing all the first separations we might

make for the original feed:
AlBCDE,
AB/CDE,
ABC/DE and
ABCD/E.
• The one with the lowest marginal vapor flow is the split
ABCD/E at 4.3 mol so With this split made, we next
compare flows for AlBCD, AB/CD and ABC/D, choosing
the split ABC/D for a total of 4.3 + 3.7 = 8.0 mol so We
have the mixture ABC to separate and compare A/BC
and AB/C; we select AlBC to add another 2.6 moles for a
total of 10.6 moles.
• Thus we back up to our first decision. Only the
decision ABC/DE could be less expensive but it has a
marginal flow already of 10.4 molls.
• The lowest marginal cost comes from using A/BC with
a flow of 2.6 moles; it leads to too high a final marginal
flow. Thus we now know that our solution ABCD/E,
ABC/D, and A/BC must be the best solution based on
the marginal flow estimates we have made to carry out
our search.
• We see that marginal vapor flows range from a
minimum of 10.6 moles to maximum of 32.3 moles.
• We now have a complete solution. We need to
examine only solutions that can be less that 10.6
moles.
• Backing up to the decision among the alternatives
AlBCD, AB/CD and ABC/D, we see that the second
best decision, AlBCD with a flow total marginal flow of
4.3 + 9.1 = 13.4 molls, will lead to a partial solution
that exceeds 10.6 molls.