Norwegian University of Science and Technology Course: Process Integration

Department of Energy and Process Engineering Number: TEP 4215

Trondheim, 30.12.07, T. Gundersen Part: Separation Systems

PROPOSED SOLUTION - ASSIGNMENT 1

Task 1: Economic Trade-offs in Distillation Columns

Introduction:

For a binary (two-component) separation, the material balance around the column is fixed
when two variables related to the product streams are specified. This is because we have 2
equations (molar balance for each of the two components) with a total of 4 unknown
variables. These could be represented by molar flows of each of the two components in the
product streams, or (as indicated in the figure of the text of this assignment) by two total
molar flowrates (D and B) and the mole fraction of the most volatile component in the same
product streams (XD and XB). With 2 equations and 2 specifications, the system (material
balance around the column) with 4 unknown variables is completely determined.

For separation of a multi-component mixture, a corresponding analysis can be done for a

light and a heavy key component. It is these two components (normally neighbor
components) that define the separation (the split) in the column. The other components can
not be specified, but they will enrich to a larger or smaller extent in the top or bottoms
product depending of the amount of reflux and the number of trays in the column.

Costs:

Investment cost for a distillation column is primarily related to the column itself (depends on
geometric dimensions such as height and diameter, as well as the thickness of the material of
construction which depends on the operating pressure of the column) and secondary to the
heat exchangers providing condensation and evaporation respectively in the condenser and
the reboiler. The cost of these heat exchangers depends on heat duty (QR and QC) and
temperature driving forces (T).

The operating cost is related to the energy consumption in the reboiler (heating) and the
condenser (cooling). These costs are directly related to the amount of reflux (which affects
QR and QC in a proportional way), and they are strongly related to the type of medium used
in the reboiler and the condenser. If the condenser temperature is too low to allow the use of
cooling water, then expensive refrigeration cycles must be used. If heat to the reboiler can
be provided through heat integration with the rest of the process, it is of course much
cheaper (almost for free) than using steam.

Trade-offs:

Before discussing the economic trade-offs it is important to be aware of the fact that the
three mentioned important design/operating parameters R (reflux ratio), N (number of stages
or trays) and P (pressure) are part of a technical relation in the sense that there are a large
number of combinations of R, N and P that will provide the desired separation effect. For a
given column pressure (P), a reduced reflux ratio (R) can be compensated for by increasing

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the number of trays (N) and vice versa. An increased column pressure (P) will in most cases
make the separation process for complicated and this must be compensated for by increased
reflux (R) and/or increased number of trays (N). For a given P there are a number of
corresponding values for R and N that will provide the necessary separation.

Economic Effects:

I) For a given (and reasonably specified= column pressure (P):

a) Increased reflux ratio (R) will lead to:

Increased reboiler and condenser duties (QR and QC) that will result in
increased operating cost (energy) and increased investment cost due to
increased heat transfer areas in the heat exchangers.
Increased gas and liquid flowrates (V and L) which in turn (especially the gas
flowrate) will result in increased column diameter (Di) to handle the increased
traffic in the column. This results in increased investment cost.
Reduced number of stages/trays (N) to achieve the same separation effect.
This results in reduced column height (H) and thus reduced investment cost.

b) Increased number of stages/trays (N) will result in:

Larger column height (H) and thus increased investment cost.

Reduced reflux ratio (R) to achieve the same separation effect. This means
reduced reboiler and condenser duties (QR and QC) which in turn result in
reduced operating cost (energy) and reduced investment cost due to a reduced
need for heat transfer surface in the heat exchangers.
Reduced reflux ratio (R) will also result in smaller gas and liquid flowrates (V
and L) in the column, which in turn (especially the gas flowrate) will result in
reduced column diameter (Di) to handle a reduced traffic in the column. This
then results in reduced investment cost.

II) Increased column pressure (P) results in:

a) The separation becomes more complicated, and this must be compensated for by
increased reflux ratio (R) and/or increased number of stages (N). If R and N were
near optimal before increasing the pressure, the economical optimum will be an
increase in both R and N. For experts in the McCabe-Thiele diagram it could be
mentioned that increased pressure makes the equilibrium curve move closer to the
diagonal. This may force an increase in the reflux ratio to make sure the operating
lines of the column cross inside the equilibrium curve (and thus feasible).

b) The temperature levels of the column (including the reboiler and condenser
temperatures) will increase. This results in changes in temperature driving forces in
the reboiler (smaller T) and in the condenser (larger T). For a considerable
increased in column pressure, new utility types may be required in the reboiler
(more expensive, such as steam at a higher condensation pressure) and in the
condenser (less expensive, such as using cooling water to replace refrigeration).

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 c) The gas flow in the column will have increased density due to higher pressure, and
this will lead to reduced column diameter. At the same time, increased pressure
will result in increased reflux ratio and thus increased column diameter as
mentioned under point I.a above, this we have counter-acting effects.

Heat Recovery:

Profitable heat recovery for a distillation column means to provide heat from the condenser
to some heating requirement in the process and/or to receive heat from the process to be
used in the column reboiler. Key variables to study such heat recovery are the heat duties
(QR and QC) and the quality of the heat given by the temperature levels (TR and TC).

For a given column pressure (P) the heat duties are proportional to the reflux ratio (R) as
discussed above. Increased R means that more heat can be provided by the condenser, but at
the same time, more heat is required in the reboiler. Whether this is advantages or not
depends on possible heat integration opportunities between the reboiler and/or the condenser
with the rest of the process. If the column can not be integrated, then increased R will
increase investment cost and must be accounted for by reduced investment cost.

Changes in column pressure will affect both the heat duties (through the reflux ratio) and the
temperature levels. This will then significantly affect the potentials for heat recovery.
Increased column pressure will increase the temperatures. This will increase the potential
for utilizing the condenser duty for heating purposes in the rest of the process, but at the
same time reduce the potential for finding a suitable heat source to run the reboiler.

Task 2 Sequence and Heat Integration of Distillation Columns

A multi-component mixture with 6 components that should be separated into 6 pure

products by using simple distillation columns (i.e. columns with one feed stream, two
product streams, one reboiler and one condenser). The number of possible sequences is
given by the formula (which is not expected to be remembered):

R = [ 2 (N 1) ] ! / { [ N ] ! [ N 1 ] ! }
Inserting for the number of components (N = 6) this gives R = 42 possible sequences. The
components are ranked according to their volatility (A is most volatile with the lowest
normal boiling point, while F is least volatile and has the highest normal boiling point.

a) We are using the following heuristic rules (rules of thumb) to select sequence:

H1: Favor separation of the most volatile component

H2: Favor near equimolar separation
H3: Favor separation of a rich component
H4: Favor simple separations

The idea behind the heuristic rules is to avoid having to evaluate (simulate and cost
estimate) all the 42 sequences, where each sequence has 5 columns. In this assignment, the
rules should be applied to identify the two most promising sequences. The strategy here is
to go through the various separators in the sequences and to find what the 4 heuristic rules

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recommend or disfavor. The last (disfavor) is not the least important, since quite often;
there will be conflict between the rules.

Notice that except for the 1st separator (where the total mixture with 6 components is the
feed), it is arbitrary what is referred to as the 2nd, the 3rd, etc. separator. Only separators with
3 or more components are discussed in the following, since two-component mixtures can
only be separated in one way and therefore does not give raise to alternative sequences.

1st Separator:

A/BCDEF: Supported by H1, but disfavored strongly by H4 since this is the most
difficult of all separations (A,B = 1.14). The separation of iso/normal
components are often quite complicated (energy demanding). This split is
also strongly discouraged by rule H2 (5/95 is extremely unbalanced).

AB/CDEF: Supported by H2 (perfect 50/50 split) and H4 (this is the simplest separation
for the entire mixture (B,C = 2.09).

ABC/DEF: This split is not a winner for any of the rules, but a very good runner up
for rule H2 (55/45 is not far from 50/50) and rule H4 (C,D = 2.01 is not far
from B,C = 2.09).

ABCDE/F : Supported by H3, however, not carrying a lot of weight (Xf,F = 0.25).

Discussion: Since rules H1 and H4 are in strong conflict regarding the split A/BCDEF,
we choose to disregard this alternative. Of the three remaining alternatives,
AB/CDEF and ABC/DEF appear to be more promising than ABCDE/F
which gives a rather unbalanced column and involves a separation which is
more difficult that the two other alternatives. Since AB/CDEF is the first
choice for both rules H2 and H4, this split is selected to be Base Case.

Base Case: AB/CDEF Alternative: ABC/DEF

2nd Separator: (if AB/CDEF is selected as 1st Separator)

C/DEF: Supported by H1, but disfavored strongly by H2 (only 5% of component C,

while the bottoms stream amounts to 45% of the original mixture). This
split is also vaguely supported by H4.

CDE/F: Supported by H2 (perfect 50/50 split) and H3 (F amounts to 50% of the

column feed).

Discussion: Rule H4 is rather neutral here, since the relative volatilities of the three
alternative splits are 2.01 (C/DEF), 1.95 (CD/EF) and 1.92 (CDE/F). Since
rules H1 and H2 are in strong conflict regarding split C/DEF, that
alternative is disregarded, so for this separator there is only one
recommended split.

Base Case: CDE/F

2nd Separator: (if ABC/DEF is selected as 1st Separator)

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 This alternative gives two 3-components mixtures. Starting with the first of
these 3-component mixtures (ABC), we have:

A/BC Supported by H1 and H2 (20/35 is much better than 50/5), and partly by H3,
but disfavored strongly by H4 (as mentioned under the 1st Separator).

AB/C: Supported strongly by H4 (B,C = 2.09 is much better than A,B = 1.14).

Discussion: Even though AB/C is a considerably simpler separation (rule H4) than
A/BC, it is likely that A/BC should be selected since three of the heuristic
rules (H1, H2 and H3) support this alternative.

Base Case: A/BC

3rd Separator: (if ABC/DEF is selected as 1st Separator)

Here, the second 3-component mixture (DEF) is handled.

D/EF Supported by H1 and rather vaguely by H4 (D,E = 1.95 is only marginally

better than E,F = 1.92).

DE/F: Supported by H2 (20/25 is significantly better than 10/35) and by H3.

Discussion: Since these separations are almost of the same level of difficulty, it may
seem as if DE/F is the best alternative, but D/EF should also be included and
evaluated.

Base Case: DE/F Alternative: D/EF

3rd Separator: (if AB/CDEF is selected as 1st Separator and CDE/F is the 2nd Separator)

C/DE: Supported by H1, but disfavored by H2 (5/20 gives an unbalanced column)

and H3 (component C has the smallest amount, only 5 mole %).

CD/E: Supported by H2 (gives a 15/10 split) and H3 (only vaguely).

Discussion: Rule H4 is rather neutral here, since the relative volatilities of the two
alternative split locations are very close (2.01 and 1.95). Since there is
conflict between the rules for split C/DE there is only one recommended
alternative for this separator.

Base Case: CD/E

In Summary:

The number of sequences has been reduced from 42 to 3 (see the figure on the next page),
where the sequence starting with AB/CDEF as the first split must be regarded as the most
promising one. Even though ABC/DEF was not too far behind as 1st separator, it turned
out that the following separators had more conflict between the rules. The split AB/CDEF
as 1st separator has a number of advantages also for the following separators. The two
components representing the most difficult separation (A/B) are isolated from the rest of the
mixture early in the sequence (in the 1st separator). In addition, these two components

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 represent a large amount (50%) of the mixture. Finally, this is the simplest split in the entire
mixture (B,C = 2.09). The figure below shows the three alternative sequences. In the rest
of this assignment, only the two first (upper) of the three sequences are considered.

AB / CDEF CDE / F CD / E A/B C/D

ABC / DEF A / BC DE / F B/C D/E

D / EF B/C E/F

b) First, we calculate the temperatures of the reboilers and the condensers from information in
the assignment text, assuming that each component contributes linearly to the mixture
boiling points:

TB,mix =
i Xi TB,i

Alternative I:

The columns in this sequence are AB/CDEF , CDE/F , CD/E , A/B and C/D. We will
denote the reboiler temperatures as TR (R for reboiler) and the condenser temperatures as TC
(C for condenser).

AB/CDEF:
TR = (0.05341.9 + 0.10371.6 + 0.10398.8 + 0.25424.0) / (0.05+0.10+0.10+0.25) = 400 K
TC = (0.20301.0 + 0.30309.2) / (0.20 + 0.30) = 306 K

CDE/F: TR = TB,F = 424 K

TC = (0.05341.9 + 0.10371.6 + 0.10398.8) / (0.05 + 0.10 + 0.10) = 377 K

CD/E: TR = TB,E = 399 K TC = (0.05341.9 + 0.10371.6) / (0.05 + 0.10) = 362 K

A/B: TR = TB,B = 309 K TC = TB,A = 301 K

C/D: TR = TB,D = 372 K TC = TB,C = 342 K

Alternative II:

The columns in this sequence are ABC/DEF , A/BC , DE/F , B/C , D/E. We calculate the
temperatures in the reboilers and condensers in the same manner as for alternative I:

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ABC/DEF:
TR = (0.10371.6 + 0.10398.8 + 0.25424.0) / (0.10 + 0.10 + 0.25) = 407 K
TC = (0.20301.0 + 0.30309.2 + 0.05341.9) / (0.20 + 0.30 + 0.05) = 309 K

A/BC: TC = TB,A = 301 K

TR = (0.30309.2 + 0.05341.9) / (0.30 + 0.05) = 314 K

DE/F: TR = TB,F = 424 K

TC = (0.10371.6 + 0.10398.8) / (0.10 + 0.10) = 385 K

B/C: TR = TB,C = 342 K TC = TB,B = 309 K

D/E: TR = TB,E = 399 K TC = TB,D = 372 K

Heat Duties:

It is considerably more difficult to quantify the heat duties of the reboilers and condensers.
These will increase proportionally with the feed flowrate, and will in addition increase
strongly (and non-linearly) when the relative volatilities are reduced and approach 1.0. For
this particular problem, it is only the A/B split that stands out with a relative volatility of
1.14, while the relative volatility for the other splits are around 2.0 (from 2.09 to 1.92).

If this problem had been part of an examination, it would not be expected by the students to
make quantitative considerations regarding heat duties in reboilers and condensers, however,
one ought to be able to mention qualitatively that the duties for the column separating A and
B would be considerably larger than for the other columns in the two alternative sequences.

The columns in the two alternative sequences have the following characteristics that affect
the duties in the reboiler and condenser. Assume that the total feed flowrate (the entire feed
mixture) is 1000 kmole/hour.

Distillation Feed Rate Relative

Column (kmole/h) Volatility

AB/CDEF 1000 2.09

ABC/DEF 1000 2.01
CDE/F 500 1.92
A/BC 550 1.14
CD/E 250 1.95
DE/F 250 1.92
A/B 500 1.14
C/D 150 2.01
B/C 350 2.09
D/E 200 1.95

A qualitative consideration indicates that columns A/BC and A/B will have large energy
requirements in the reboiler and condenser. For the other columns, the expected duties can
be related to the feed flowrate with minor adjustments for the relative volatilities (which do
not differ more than from 2.09 to 1.92). The figures on the next page show qualitatively the
approximate temperature levels and heat duties for the two most promising sequences.

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 Alternative I
T (K)
425

CDE / F
TR = 399 K
400 TR = 424 K

TC = 377 K C
D
375 / TR = 372 K
E
AB / CDEF C
TC = 362 K /
TR = 400 K D
350
TC = 306 K
TC = 342 K

325

A/B TR = 309 K TC = 301 K

300 Q

Alternative II
T (K)
TR = 424 K
425

D
E TR = 399 K
400 /
F
D
/
TC = 385 K E
375
ABC / DEF TC = 372 K

TR = 407 K
350 TR = 342 K
TC = 309 K
B
325 /
C

A / BC TR = 314 K TC = 301 K
TC = 309 K
300 Q

Conclusion:

From the figures above it looks obvious that alternative I has the largest potential for heat
recovery between the columns, since the heat of condensation from three columns (CDE/F,
CD/E and C/D) can be used to cover parts of the reboiler duty in column A/B. With a minor
adjustment of the pressure in AB/CDEF, this column can also be integrated with A/B.

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