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Part 1.
DISTILLATION:
Revisiting Some
Rules of Thumb
C. M. Lek
Singapore Armed Forces
G. P. Rangaiah and K. Hidajat
National University of Singapore
istillation is the most common
unit operation for separating
liquid mixtures into valuable
and/or high purity products. It
is also one of the most energyintensive operations. Hence, optimization of distillation-column design and
operation should get high priority.
Numerous distillation heuristics
(rules of thumb) for quick optimization have emerged over the years. For
instance, heuristics on optimal reflux
ratio as a certain multiple of the minimum reflux ratio have been widely
used as quick tools to estimate optimum reflux ratio.
However, changes over time in the
relative cost of equipment and energy
(which affects operating cost) can affect the validity of such rules of
thumb. Meanwhile, it has now become
more feasible to assess their validity,
as todays availability of commercial
simulators and high-speed computers
allows rigorous and thus more-accurate distillation calculations be carried out with relative ease.
This article assesses the validity of
optimal-reflux-ratio and other heuristics in light of recent cost data, by considering seven binary and six multicomponent
systems.
Distillation
columns for each of the 13 have been
designed and optimized by both shortcut (heuristics-based) calculations
and rigorous simulations. In addition
to the reassessment, a key observa-
50
Example
No.*
1
2
3
4
5
6
7
Components
Benzene
Toluene
i-Butane
n-Butane
Propylene
Propane
Acetone
Water
n-Hexane
p-Xylene
Methanol
1,4-Dioxane
Methanol
Water
Product Purity
Specifications (mole%)
Top : 92% Benzene
Btm : 95% Toluene
Top : 91.7% i-Butane
Btm : 90% n-Butane
Top : 96.2% Propylene
Btm : 91.1% Propane
Top : 91% Acetone
Btm : 97.8% Water
Top : 95% n-Hexane
Btm : 97% p-Xylene
Top : 99% Methanol
Btm : 98% Dioxane
Top : 99% Methanol
Btm : 99% Water
*Sources for Examples: 1 and 2 from Peters and Timmerhaus (1991); 3 and 4 from King (1980); 5 to 7 from Doherty and Malone (2000).
Items in italics indicate unavailable specifications, or ones modified to allow column optimization by varying the reflux ratio.
Thermodynamic package used: Peng-Robinson for Eamples 1, 2, 3 and 5; and NRTL for Examples 4, 6 and 7.
Cooling water for cold utility unless stated otherwise.
Pcond = pressure at condenser; Preb = pressure at reboiler
have been changing, particularly during the latter years of that time period.
Furthermore, some of the early studies on optimal reflux ratio were based
on shortcut calculation methods or
graphical correlations, whereas today,
rigorous calculations (with more-accurate results) can be made with ease.
Such calculations can assess the
suitability of the heuristics on optimum reflux ratio with current cost
data and, if necessary, update those
heuristics. Furthermore, it is possible
to determine whether, and how, the
capabilities of commercial simulators
for rigorous distillation simulation
can also be used for optimizing reflux
ratio. Both of these questions are addressed in what follows, by considering industrially relevant applications
that involve both binary and multicomponent mixtures. Along the way,
we also scrutinize the validity of some
other heuristics for distillation-column design.
Equations and data for sizing and
costing of columns, including reboilers
and condensers, are taken from the
open literature. This study is limited
to simple (but not necessarily binary)
columns, each with a single feed
stream and two product streams.
Zdonik,1977 [21]
King,1980 [7]; Walas, 1987 [20]
Thompson,1980 [15]
Perry, others, 1997 [13]
Ropt/Rmin
1.1 to 1.6
1.1 to 1.5
1.05 to 1.1
1.1 to 1.2
1.2 to 1.3
1.25
1.1 to 1.2
1.2
1.2 to 1.3
1.1 to 1.5
1.1 to 1.2
1.2 to 1.4
1.05 to 1.10
1.10 to 1.20
1.2 to 1.5
1.4 to 1.5
1.05 to 1.2
Remarks
Lower values for high relative
volatilities
Low-level refrig. (< -150F)
High-level refrig.
Water- and air-cooled condensers
Generally accepted
With increased energy costs
Common fractionators
Petroleum-distillation columns
Refrig. is involved
Cooling-tower water used in condensers
Low-level refrig. (-300 to -150F)
High-level refrig. (-150 to 50F)
Cooling water
Air cooling
1.2 to 1.25
51
Example
No.*
Components
Nitrogen
CO2
Methane
Ethane
Propane
i-Butane
n-Butane
Propylene Oxide
Propylene Glycol
Water
Propene
Propane
1-Butene
n-Butane
n-Pentane
Acetone
Methanol
Ethanol
Water
1-Butanol
Propylene
Propane
1,3-Butadiene
n-Butane
n-Pentane
Ethane
Propylene
Propane
Propadiene
n-Butane
10
11
12
13
Product Purity
Specifications
(Mole %)
Top : 0.6% n-Butane
Btm : 2% Propane
Top : 2 X 10-5 %
Propylene Glycol
Btm : 0.5% Water
Top : 4.74% 1-Butene
Btm : 2.54% Propane
Top : 2% Ethanol
Btm : 2% Methanol
Top : 1% n-pentane
Btm : 1% n-butane
Top : 2% Propane
Btm : 50% Propene
*Sources of Examples: 8 and 9 from HYSYS Documentation; 10 from Van Winkle and Todd (1971);
11 from Ishii and Otto (2001); 12 and 13 from typical petrochemical industries.
Items in italics indicate unavailable specifications, or ones modified to allow column optimization by varying the reflux ratio.
Thermodynamic package used: Peng-Robinson for Examples 8, 10, 12 and 13; UNIQUAC for Example 9; and NRTL for Example 11.
Cooling water for cold utility unless stated otherwise.
Pcond = pressure at condenser; Preb = pressure at reboiler
TABLE 4. SELECTED RESULTS FROM RIGOROUS SIMULATION AND OPTIMIZATION OF ALL 13 EXAMPLES
Example Number of
Feed
Annualized Operating
Total
Ropt
Rmin@
Ropt/Rmin
Nmin@
Stages*
Stage#
Capital
Cost,
Cost,
Cost, $/yr
$/yr
$/yr
1
21
10
57,741
364,533
422,274
1.362
1.261
1.08
5.3
2
65
34
316,353
10,752,075 11,068,428
10.36
10.00
1.04
13.3
3
102
72
199,542
197,489
397,031
18.63
15.08
1.24
47.7
4
9
8
31,145
59,013
90,158
0.365
0.348
1.05
1.7
5
9
5
29,018
94,197
123,215
0.540
0.381
1.42
2.2
6
23
21
46,517
110,516
157,034
1.135
0.764
1.49
6.1
7
23
19
57,188
296,692
353,880
0.798
0.484
1.65
6.1
8
25
11
54,695
170,794
225,489
0.491
0.441
1.11
8.7
9
21
18
77,954
795,940
873,900
0.080
0.050
1.60
5.3
10
18
8
55,025
902,703
957,729
0.961
0.778
1.24
3.9
11
48
19
194,885
1,343,503
1,538,388
2.019
1.730
1.17
10.0
12
25
13
75,286
428,830
504,117
0.771
0.727
1.06
8.0
13
105
42
452,312
1,617,538
2,069,850
6.081
5.215
1.17
37.0
* Excluding reboiler and condenser.
# Counted from the top with condenser as zero.
@ Minimum reflux ratio and minimum number of stages (excluding reboiler and condenser) obtained from shortcut calculations.
Cost totals may not agree with cost components due to rounding.
53
Cover Story
TABLE 5. RESULTS BY SHORTCUT CALCULATIONS WITH ROPT/RMIN = 1.2,
tal cost. As for Example 10, alFOLLOWED BY RIGOROUS SIMULATION AND FEED-STAGE OPTIMIZATION
though the column is short, a large
feed rate of 1,000 mol/h and a sepaExample Results for Ropt/Rmin = 1.2
Results for Ropt/Rmin = 1.2
after feed stage optimization
ration requiring a refrigerant result
Number of
Feed
% Increase
Feed
% Increase
Ropt/Rmin
in a high operating cost. Examples
stages
stage in total cost Stage
in total cost
11 and 13 process large quantities
1
15
7
3.1
7
3.1
1.19
of feed; accordingly, the bulk of the
2
29
20
11.4
20
11.4
1.18
total cost lies in the operating cost.
The optimal number of stages is
3
97
58
3.5
68
1.1
1.29
expected to be close to twice the
4
8
3
71.5
7
1.8
1.10
minimum number of stages [12].
5
9
4
0.1
5
0
1.42
However, the results in Table 4
6
18
10
19.8
16
1.7
1.70
(Column 2 and last column) show
7
18
8
16.1
14
1.7
1.80
that this heuristic is generally not
8
25
14
3.1
11
0
1.11
valid.
9
25
25
29.0
22
0.2
1.40
To test the validity of the heuris10
12
6
4.2
5
3.6
1.34
tic saying that Ropt/Rmin equals 1.1
11
25
13
15.0
11
12.2
1.45
to 1.6, the column for each example
12
22
10
0.9
11
0.4
1.09
is first designed in accordance with
13
78
42
12.1
28
4.1
1.27
successive shortcut column calculations to estimate the number of
Note: % increase in total cost is from the minimum total cost shown in Table 4.
stages and the feed stage assuming
that Ropt/Rmin equals 1.1 to 1.6 in in- that the feed stage from the shortcut feed stage optimization via minimizing
crements of 0.1; these estimates are calculations
(for
instance,
for the reflux ratio. This equivalence is to
followed by a rigorous simulation and Ropt/Rmin equaling 1.2 in Table 5) is be expected, as the total cost is often
cost estimation. For each case, percent very different from the feed stage in dominated by operating cost when the
increase in total cost from the mini- Table 4, even if the total number of total number of stages is fixed.
mum total cost in Table 4 is calculated. stages is comparable.
After the feed stage optimization,
In fact, Reference [7] points out that the feed-stage location, the Ropt/Rmin
Results from this extensive study
show that the variation in percent in- the guideline for optimal feed stage is value and the percent increase in total
crease in total cost depends on the ex- that the ratio of key-component mole cost for Examples 1, 2, 5, 10 and 12
ample; it is within 11% in five exam- fractions in the liquid on the feed are comparable to those with the feed
ples (1, 5, 8, 10 and 12), but is stage should be close to the corre- stage determined by the shortcut calsponding ratio in the liquid part of the culations. On the other hand, the total
significantly more in other examples.
A reasonable value for Ropt/Rmin feed. The key-ratio plot in Figure 1 for cost decreases dramatically in Examwithin 1.1 to 1.6 is 1.2. Results for this Example 4 indicates that the feed- ples 4, 6, 7, 9 and 13. In the other
particular case (Columns 2 to 4 in stage location should be closer to the three examples (Nos. 3, 8 and 11), too,
Table 5) show that the increase in reboiler. The feed stage in the opti- the total cost decreases, by about 3
total cost is in the range of 0.1% to mized design is consistent with the percentage points.
about 70%, and the average increase heuristic given in Reference [7].
Thus, after the feed stage optimizaA recent reference [8] states that the tion to minimize the reflux ratio, the
is about 14% for all 13 examples.
Thus, although the heuristic on optimal feed location for a specified increase in total cost (from the miniRopt/Rmin equaling 1.1 to 1.6 seems to total number of stages and separation mum total cost shown in Table 4) is
be valid in five out of the 13 examples minimizes the reflux ratio (and there- less than 4.1% for all examples except
tested, these results nevertheless show fore the reboiler and condenser duties). Nos. 2 and 11. The optimal total numthe potential for reducing the total col- In accordance with this guideline, the ber of stages and reflux ratio for these
umn cost by further optimization.
feed stage for the case of Ropt/Rmin two examples (Table 4) are different
equaling 1.2 in Table 5 is optimized by from those for Ropt/Rmin equaling 1.2
Revelations about the feed stage varying the feed stage in the rigorous (in Table 5).
In addition to the above findings, a simulation and finding the reflux ratio
In other words, column design by
closer analysis of the results for vari- to achieve the desired separation. shortcut calculations can be improved
ous Ropt/Rmin values indicated that These optimized results after feed significantly by changing the feed
the feed stage given by shortcut col- stage optimization are shown in the stage to minimize reflux ratio for the
umn calculations can be inappropri- last three columns of Table 5.
same total number of stages found for
ate. The most extreme case is ExamA separate exercise was carried out Ropt/Rmin equaling 1.2. This change
ple 4, for which increase in the total to optimize the feed stage by minimiz- can be carried out easily with the aid
cost ranged from 70 to 260% with ing total cost for the case of Ropt/Rmin of a simulator, because it does not inRopt/Rmin in the range 1.1 to 1.6. One equaling 1.2 for all examples. These re- volve sizing and cost estimation of the
can see from the optimized results sults are identical to those obtained by column, condenser and reboiler.
54
Authors
FIGURE 1.This plot, relevant to Example 4, relates the column stage number with the
key ratio for the liquid at that stage, for both shortcut and optimized design
age 14% higher than the minimum attainable by rigorous simulation and
optimization. However, the design in
this case can often be improved substantially by optimizing the feed stage
(for a specified number of stages and
separation), and the total cost of a column can be reduced to within 4% of
the minimum.
In a few cases, potential exists for
further cost reduction by varying both
the number of stages and feed stage,
and simulating the column rigorously.
These findings are applicable to simple columns with a single feed stream
n
and two product streams only.
Edited by Nicholas P. Chopey
C.M. Lek is currently an Engineering Officer in the Singapore Armed Forces. Mr.
Lek received his bachelors
degree in chemical engineering from the National University of Singapore in 2003 with
second class honors (Upper
Division). The work reflected
in this article began as his senior-year research project,
and continued after completion of that project. Mr. Lek has a particular interest in software development.
G.P. Rangaiah is an Associate Professor in the Dept. of
Chemical and Biomolecular
Engineering, National University of Singapore (Singapore 119260; Phone: [65]
6874-2187; email: RangaiahGP@nus.edu.sg).
He
worked for Engineers India
Ltd. (New Delhi) for two
years, and has been lecturing
at the National University of
Singapore since 1982. His research interests are
in process control, modeling and optimization.
He has supervised nine research fellows/assistants and more than 20 postgraduate theses, has
published about 70 papers in international journals, and has presented nearly 50 papers in conferences. He received his baccalaureate, masters
and doctorate degrees in chemical engineering
from Indias Andhra University, IIT Kanpur and
Monash University, respectively.
Kus Hidajat is an Associate
Professor in the Dept. of
Chemical and Biomolecular
Engineering, National University of Singapore (email:
chehidak@nus.edu.sg).
He
has been lecturing at the National University of Singapore since 1983. His research
interests are in simulatedmoving-bed adsorptive separation processes with or without reaction, plus modeling and optimization,
and catalytic membranes. He has supervised
four research fellows/assistants and 26 postgraduate theses, has published about 65 papers
in international journals, and has presented
about 40 papers in conferences. He received his
baccalaureate and doctorate degrees in chemical
engineering in the U.K., from the University of
Manchester Institute of Science and Technology
(UMIST) and the University of Cambridge, respectively.
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55