CW

Operations & Maintenance

Distillation Clean
solvent
A

Reboiler Startup Feed FIGURE 1.

93% A The extractive
7% B distillation tower
discussed in this article
employs two reboilers

Can Pose Challenges 108°C

#3 ∆Pout
140°C
Kettle
hs, REB reboiler

1 5 Steam
Future designs can benefit from the lessons 109°C
3

H
that were learned via a well-planned Thermosiphon
reboiler
∆Pin 2

#1 109°C
investigation of this startup problem #2 140°C 4

Contaminated solvent
2% A 1% B 97% solvent
Etienne Rubbers, Kirsten Green TABLE 1. DESIGN STREAM COMPOSITIONS
and Terry Fowler, Stream #1 Stream #2 Stream #3
Sasol Technology (Pty.) Ltd.
Liquid to Liquid Vapor
Flashed Flashed
kettle ex kettle ex kettle
Henry Z. Kister and Walter J. Stupin, Temperature,°C 109 124 137 140 140
Fluor
A, wt, % 30 3 2 2 62
B, wt, % 14 2 1 1 29

D
uring the initial startup of a
new extractive distillation
tower* at a Sasol plant in Se-
cunda, South Africa, the
chimney tray feeding liquid to the
tower’s once-through kettle reboiler
unexpectedly overflowed. The plant
quickly implemented a successful fix,
but the cause of the overflow remained
obscure. Further joint troubleshooting
by a Sasol/Fluor team cleared up the
mystery, and provided lessons for how
to avoid similar problems in other ex-
tractive distillation units.
The investigation utilized pressure
drop measurements, neutron back-
scatter, surface temperature surveys,
and hydraulic calculations to estab-
lish the force balance that led to the
overflow. Among other things, the
measurements offered strong evi-
dence of boiling maldistribution in the
reboiler. The team came up with a
theory that is consistent with all the
measurements and force balance; it
subdivides the reboiler into a stag-
nant region, an intense boiling region,
and a kettle region.
This regional maldistribution pat-
tern is believed to be unique to mix-
tures such as those encountered in ex-
*The tower was not designed by the authors’ em-
ployers.
C, % wt 56 95
Vaporization, mol% — 69.0
Mass flow, kg/h 134,000
tractive distillation, with the boiling
liquid consisting of a large concentra-
tion of very high boilers and a small
concentration of volatile components.
The mulitifeed and multidraw kettle
arrangement, and possible foam for-
mation, may also play a role.
Process description
The process feed to the tower (Figure
1) contains: 93% Component A, an or-
ganic with an atmospheric boiling
point of 80°C, which is recovered as a
high-purity overhead product from the
top of the tower; and 7% Component B,
an organic that boils at 84°C under at-
mospheric pressure. B has a higher
affinity to the solvent and leaves at the
tower bottom. The solvent boils at
above 250˚C at atmospheric pressure.
In the unusual boilup supply sys-
tem for the tower (Figure 1), liquid at
108˚C from the bottom trays is col-
lected on an upper chimney tray, from
where it gravity-flows to a once-
through thermosiphon side-reboiler.
The liquid from the outlet of the ther-
mosiphon is collected on a lower chim-
CHEMICAL ENGINEERING WWW.CHE.COM FEBRUARY 2004
97 97 9
71.7 72.3 —
72,000 62,000
ney tray at 109˚C, and gravity-flows to
the kettle reboiler. Vapor generated in
the kettle reboiler at 140˚C is re-
turned to the tower above the lower
chimney tray. Unboiled liquid from
the kettle reboiler, also at 140˚C, over-
flows the reboiler weir into the kettle
draw compartment, from where it
gravity-flows into the tower bottom-
product sump.
Table 1 shows the rapid change in
component concentration that takes
place near the bottom of the tower.
The tower bottoms contain 2% by
weight of Component A, 1% of Compo-
nent B, and 97% solvent (Component
C). One stage up, at the bottom chim-
ney tray, the liquid composition
changes to 30 wt.% A, 14 wt.% B, and
only 56 wt.% solvent. This difference
is the reason for the steep tempera-
ture change near the tower bottom.
Such steep composition and tempera-
ture changes are typical of extractive
distillations, using a high-boiling sol-
vent to separate relatively low-boiling
organics.
(Continues on p. 56)
55
 Operations & Maintenance
The startup problem
Upon startup, the lower chimney tray
operated at the design temperature of
109˚C. The kettle reboiler vapor was at
145˚C, somewhat hotter than the de-
sign 140˚C. However, the bottom sump
temperature was 109˚C, much colder
than the design temperature of 140˚C.
This low temperature meant a much
larger concentration of A (around 30
wt.%) in the sump, compared to the de-
sign (around 2 wt.%). Because of the
discrepancy, the recovery of A in the
product stream was much poorer than
the design recovery. What’s more,
flooding was apparent in the solvent
stripper downstream of the extractive
distillation tower, due to the significant
variation in its feed composition.
Operators first tried to improve perfor-
mance by manipulating some of the
tower operating variables. Raising the
steam rate as far as possible only had a
small effect, raising the sump tempera-
ture from 109 to 112˚C. Reducing the feed
flowrate had a much greater effect, rais-
ing the sump temperature as high as
130˚C, but at the penalty of lower pro-
duction rates. The situation was not tol-
erable, and changing operating variables
did not produce a satisfactory solution.
The higher reboiler temperature
suggests that the flowrate through the
kettle reboiler was lower than as de-
signed. The only plausible explana-
tion for the low sump temperature is
that the liquid from the lower chim-
ney tray was bypassing the kettle re-
boiler and reaching the bottom sump.
Such bypassing can be due either to
liquid leaking from the lower chimney
tray, or to liquid overflowing into the
chimneys. The observation that the
sump temperature rose at lower feed
rates argued against tray leakage
being the root cause, thus supporting
liquid overflow into the chimneys.
There was another possible route
for liquid to bypass the lower chimney
tray. Vapor-liquid effluent from the
thermosiphon side reboiler enters the
vapor space above the lower chimney
tray (Figure 1). Though the bottom of
this nozzle is 300 mm above the hat of
the chimneys, it was possible that liq-
uid trajectories from the side reboiler
effluent were finding their way into a
chimney that had its opening oriented
towards the effluent nozzle.
56 CHEMICAL ENGINEERING WWW.CHE.COM FEBRUARY 2004
FIGURE 2. Temperature measurements made during troubleshooting of the kettle
reboiler constituted a key input for the analysis of its performance problem
Based on the overflow theory, the
tower was shut down after one day in
service, and the chimney heights on
the lower chimney tray were extended
from 200 mm to 900 mm. Furthermore,
the chimney into which the side re-
boiler could have been blowing liquid
was blanked. Upon return of the sys-
tem to service, the sump temperature
reached the design 140˚C and stayed
there during all periods of normal oper-
ation. The reboiler temperature de-
clined from 145˚C to the design 140˚C.
The chimney tray modifications were
successful in preventing any further
liquid bypassing from the lower chim-
ney tray into the bottom sump.
Taking the pulse
Although the problem thus went
away, understanding its root cause
posed an interesting challenge. Fur-
thermore, such understanding would
be valuable, both for dealing with sim-
ilar systems and for application dur-
ing any future debottlenecking of the
same Sasol distillation unit. So, the
following checks and measurements
were performed:
Pressures: The team measured pres-
sures at the vapor space above the ket-
tle reboiler and in the vapor above the
lower chimney tray in the tower. The
measured pressure drop at startup was
4–8 kPa, higher than the design 2.5-
kPa maximum, even though the
flowrates were lower. The outlet-line
pressure drop was recalculated, using
three alternative procedures: a Fluor
method, a commercial simulation, and
a simple hand method based on Perry’s
Handbook [2]. All three methods gave
numbers in the 4–6-kPa range, which
were slightly lower than, yet well in
line with, the field measurements
Liquid level: Neutron backscatter
scans were performed to determine
the liquid level on the lower chimney
tray. The level was found at 300 mm.
This finding confirmed that, with the
initial 200-mm chimneys, the liquid
level would have been above the top of
the chimneys and overflow would
have occurred. It also confirmed that
increasing the chimney height to 900
mm would have indeed eliminated the
overflow. Thus, this test fully con-
firmed the startup team’s analysis
and solution.
The neutron backscatter scans also
argue against the liquid trajectories
from the side reboiler causing the by-
passing. With the trajectories fully
eliminated during the startup fix, the
chimney tray liquid level still exceeded
the original chimney height of 200 mm.
Entrainment: Entrainment of liquid
in the vapor leaving kettle reboilers
has been known to occur when the
vapor space above the tube bundle is
small [1]. To explore this possibility,
the team assessed the design of the
existing kettle in light of good-design
criteria listed in the literature [1]. The
ratio of kettle diameter to overflow
baffle height in the existing kettle is
1.4, which is near the recommended
minimum (1.3 to 1.6). The ratio of tube
bundle to kettle diameter is 0.63,
which slightly exceeds the recom-
mended maximum 0.6.
Foaming: The team conducted some
limited tests to check for foaming. The
tray-pressure drop across the column
did not provide any evidence of foam-
ing on the trays. So, if foaming took
place, it would be confined to the kettle,
where the solvent concentration was
high and where vigorous boiling takes
place. A sample of reboiler liquid was
shaken, and was observed to produce
about 25 mm of froth above the liquid,
which took 1–2 min. to disappear.
Because of the high fluid tempera-
tures, it was not possible to simulate
the operating conditions. So foaming
could have played a role, even though
no stable foam was observed. Older-
shaw tests [1] during the piloting of the
column indicated some wall-supported
foaming, but the foam was unstable.
Temperatures: Laser-guided infrared
pyrometers measured the surface tem-
peratures around the kettle reboiler
shell. Several sets of these measure-
ments were made. While the tempera-
ture varied from one set of readings to
another due to changes in steam pres-
sure, the trends observed did not vary
and were completely repeatable. Figure
2 shows the results of the most compre-
hensive temperature survey.
The kettle reboiler has four liquid
inlets and four vapor outlets, a con-
figuration that is often used to provide
good fluid distribution in horizontal
shell-side reboilers. The average sur-
face temperatures at the two vapor
outlet nozzles furthest away from
the overflow baffle were low (122
and 128°C). The surface temperature
at the next vapor-outlet nozzle was
141˚C, and at the vapor nozzle closest
to the overflow baffle, the temperature
was 144˚C.
The surface temperatures at the
reboiler liquid pool displayed the op-
posite trend. Temperatures were high
(176 and 186°C) near the flange, and
were progressively lower along the
final half of the reboiler length. The
surface temperatures at the liquid
pool were 160–168°C in the third
quadrant away from the overflow baf-
fle, 157–160°C in the second quadrant
away from it, and 154°C at the quad-
rant just before the overflow baffle.
Heat transfer: The heat transfer
coefficient was calculated to be 839
kW/(m2)(˚C), which is lower than the
design 1,026 kW/(m2)(˚C).
Assessing reboiler operation
The measurements and determina-
tions made as outlined above enabled
the team to assess the operation
within the reboiler.
Pressure balance: The pressure bal-
ance between the elevation at Point
1 at the vapor space above the lower
chimney tray and that at Point 2 at
the reboiler floor (see Figure 1) is as
follows (with all pressures expressed
in millimeters of liquid head):
H = ⌬Pin + hs,REB + ⌬Pout (1)
where H is the liquid driving
head (top of chimney tray liquid level
to reboiler floor), ⌬Pin is the pressure
drop in the inlet piping, hs,REB is the
static head in the reboiler and ⌬Pout is
the pressure drop in outlet piping.
The neutron scan measurements
gave H as 15.5 kPa at normal operat-
ing conditions. The ⌬Pin was calculated
at about 1 kPa. The ⌬Pout at normal
operating conditions was calculated at
5–7 kPa; this range was slightly higher
than the startup ⌬Pout, which was 4–6
kPa and agreed with the plant data at
its original startup. With the assump-
tion of no aeration in the reboiler liq-
uid, and allowing for the head over the
weir as recommended [3], hs,REB was
calculated at about 8 kPa. The right
side of Equation (1) thus gives 14-16
kPa, which is slightly on the low side
(but well within calculation accuracy)
of the 15.5 kPa head on the left side of
Equation (1).
Basic to this force balance is the as-
sumption that the static head inside
the reboiler, hs,REB, is equal to the head
of actual liquid from the top of the
overflow baffle (plus the small head
over the weir) to the reboiler floor. This
assumption makes hs,REB the head of
non-aerated liquid, which may be ques-
tionable for a pool of boiling liquid.
This assumption is made in some
key literature references on the sub-
ject [3, 4], and is often the conserva-
tive assumption made for design.
More-comprehensive models [5, 6]
replace the non-aeration assumption
by a model that takes into account the
generated vapor volume, as well as the
tube-bundle two-phase pressure drop.
Application of these models to kettle
reboilers is further complicated by the
recirculation of liquid inside the kettle
and the existence of fairly clear liq-
uid zones between the bundle and the
sides of a kettle reboiler [5].
In the Sasol reboiler, there is an ad-
ditional justification for the non-aera-
tion assumption. As is discussed below,
there is evidence that the nozzle clos-
est to the tubesheet enters a stagnant
liquid region. In that case, this inlet
will see the full hydrostatic head be-
tween the overflow (Point 3) and the
CHEMICAL ENGINEERING WWW.CHE.COM FEBRUARY 2004
reboiler floor (Point 2) in Figure 1.
Based on the Equation (1) force bal-
ance, the chimney tray overflowed be-
cause the pressure drop in the reboiler
outlet line was high and because the
full static head of the non-aerated re-
boiler liquid acted to raise the driving
head on the chimney tray. Entrain-
ment from the kettle could have also
contributed. This entrainment would
further increase the pressure drop in
the reboiler vapor outlet line, and ac-
count for the outlet line pressure-drop
measurement being slightly higher
than calculated. Calculations show
that about 10-30% entrainment in
the vapor would account for the slight
pressure drop difference. However,
this difference can also be explained
by simple inaccuracies in measure-
ment and calculation.
Although the pressure balance ex-
plains the chimney tray overflow, it
is unable to explain the observations
from our temperature measurements.
These are discussed below.
Vapor disengagement between
tubesheet and first vapor outlet noz-
zle: The tubes are 6,100 mm long (this
measurement does not appear in Figure
2). Of this length, about 1,500 mm (or
25%) lies between the tubesheet and the
beginning of the first vapor outlet noz-
zle. So if the heat exchanger were to va-
porize the liquid uniformly, practically
all the vapor exiting at the first vapor
outlet nozzle should initiate in the ex-
changer section between the tubesheet
and the beginning of that nozzle.
The kettle overflow baffle is 1,150
mm high. A Francis weir formula cal-
culation [2] shows that a 72,000-kg/h
liquid overflow over the outlet weir will
incur an additional liquid head of 50
mm. So, the liquid level is at least 1,200
mm above the kettle floor (without al-
lowance for hydraulic gradients or for
aeration of the liquid, which will tend to
make the liquid height even taller).
The first 236 mm of tubes are in the
1,000-mm-dia portion of the kettle,
with no vapor disengagement space.
Over the next 1,090 mm of the tubes,
the kettle diameter expands from
1,000 to 1,628 mm, at a 30-deg angle.
Geometry dictates that the first 350
mm of that expansion will be fully
submerged by the 1,200 mm of liquid.
So the total tube length at which there
57
 Operations & Maintenance
is no vapor disengagement whatso-
ever is about 590 mm. In this length,
40-50% of the vapor reaching the first
vapor nozzle should be generated.
Further, in light of the expected vapor
generation, vapor velocities should be
locally high. And, there will not be
much disengagement of liquid in the
next 500 mm or so of tube length, as
this section has a restricted vapor-
passage area due to the smaller diam-
eter. (However, as we have concluded
below, the actual vapor generation in
this section is very low.)
Stagnant liquid region (Figure 3):
For the liquid in the tubesheet region,
the surface temperatures measured
were high. This is also the region that
has little disengagement space above.
Liquid temperatures in the range of
168 to 186°C imply concentration of
Components A and B of less than 0.5%
by weight; in other words, very low.
Under the assumption that these
temperatures apply to the mixture
close to the tubesheet throughout the
tube bundle, the material in this re-
gion thus consists almost entirely of
the non-volatile solvent, Component
C. It then follows that in this region,
very little boiling and heat transfer
take place. This absence will occur if
there is only a small flux of material
flowing around the tubes in this area.
The small flow generates only a
small quantity of vapor, and the liquid
around the tubes will get hotter and
hotter as its low-boiling components
flash off. All that will be left is the
heavy liquid, which tends to sit there.
This behavior turns most of the first
quadrant into a stagnant zone or dead
pocket of hot, heavy liquid, mostly
Component C.
It is worth noting that temperatures
of 168 to 186°C were surface measure-
ments at the shell, some distance away
from the hot tubes. The stagnant layer
between the tubes and shell is a good
insulator, and it is possible that near
the tubes the temperatures will be
higher, probably approaching that of
the condensing steam.
Since not much liquid vaporizes in
the stagnant zone, the froth density in
this region is high, much closer to that
of the liquid than to that of a vapor/liq-
uid mix, and much higher than that of
the froth or aerated liquid in the other
58 CHEMICAL ENGINEERING WWW.CHE.COM FEBRUARY 2004
FIGURE 3. Boiling behavior varied significantly across regions of the kettle reboiler
quadrants of the kettle. This means
that there is less flow resistance, due
to the lower static head of the froth in
the central and baffle regions. Conse-
quently more incoming liquid will
channel toward the central region.
Our calculations indicate only a few
hundred millimeters of head differ-
ence are enough to account for the es-
sential absence of flow in one feed noz-
zle while the adjacent nozzle feeds the
bulk of the liquid to the reboiler. As
less feed flows towards the tubesheet
end, the liquid in the tubesheet region
will stagnate more and vaporize less.
The end result is a self-accelerating
mechanism that promotes the dead
zone in the tubesheet region and a
high-liquid-flux central region.
The high-L/V, intense boiling, cen-
tral region (Figure 3): This region
has a higher-than-design liquid fee-
drate (and a high liquid/vapor, or L/V,
ratio), to compensate for the reduced
flow to the stagnant region. The high
rate results in lower liquid tempera-
tures, but with intense boiling and
higher than design vapor generation.
A pressure balance across the re-
boiler (Figure 1) equates the pressure
difference between the common liquid
inlet line (Point 4) and the common re-
boiler vapor space (Point 3), no matter
which region one travels through. The
pressure difference is given by Equa-
tion (2), again with all pressures ex-
pressed as millimeters of liquid head:
P4 - P3 = hs +
Pn +
PREB (2)
where hs is the static head in a given
reboiler region,
Pn is the pressure
drop in the liquid line leading to the
region, and
PREB is the reboiler pres-
sure drop in that region.
In the stagnant region discussed
above, hs approaches the full head of the
non-aerated liquid, and the
P terms are
quite small due to the low flow. Con-
versely, in the intense boiling region, the
boiling aerates the liquid, which lowers
the liquid head. This induces high
flowrates of liquid into the region until
the pressure-drop terms balance the dif-
ference between the aerated-liquid head
in this region and the non-aerated-liquid
head in the stagnant region.
The high liquid flowrate induced
into the vigorous-boiling central re-
gion means that the fraction of the liq-
uid vaporized in this region is lower,
so less of the low-boiling components
are removed from the liquid. This
lights-rich liquid could possibly per-
sist all the way to the two vapor noz-
zles closest to the tube sheet.
The lower temperatures observed
near the vapor nozzles closer to the tube
sheet are the result of the high liquid
flux in the tube field and the resulting
lower temperatures through the re-
gions providing the vapor to these noz-
zles. The vapor nozzle closest to the
tubesheet is the coldest, because that is
where the intense boiling starts and is
more vigorous, and there is a smaller
fraction vaporized. Also, some of the liq-
uid is likely to be projected into the
vapor outlet nozzles in the form of en-
trainment. The action in this region has
some similarities to the action in hori-
zontal thermosiphon reboilers, in that
the quantity of vapor generated results
in a low-density froth, which promotes
liquid flow to this region, in contrast to
the behavior with the more dense liquid
in the more stagnant zones.
One might wonder what caused
the measured wall temperatures of
the liquid in this region to remain
hot. The key is that our survey mea-
sures the wall temperatures, not the
bulk temperatures. The intense boil-
ing takes place at the bulk of the
bundle, and may not reach the wall.
Equation (2) shows that along the
wall in this region, there is horizon-
tal flow of hot liquid from the higher-
static-head stagnant region towards
the overflow baffle. This flow is some-
what tempered by the boiling. On the
other hand, the vapor temperatures
were measured right above the bulk
of the bundle, where the boiling is
most intense.
The kettle boiling region (Figure
3): There is a net flow of liquid from
the central region to the overflow
baffle, because this is the only manner
in which the solvent can permanently
exit the kettle reboiler system. As one
moves closer to the overflow baffle,
there are two effects: this net flow
increases, and the composition of the
liquid can be expected to contain less
of low-boiling material. As a result,
less vigorous boiling and a higher aer-
ated-liquid density can be expected in
this region. This higher aerated-liquid
density will provide more resistance
to liquid feed from the inlet nozzle in
this region and, in turn, reduce the
inlet feed to the kettle boiling region.
This is the one region of the reboiler
that actually operates as it should,
like a kettle. Not much entrainment
takes place here, and there is much
disengagement space in this region,
both of which promote the true kettle
action. As the reboiler-feed liquid flow
through this region is lower than the
design and the percent vaporization is
close to or higher than design, the tem-
perature of vapor flowing to the last
nozzles is close to or above design.
If liquid entrainment from the in-
tense boiling region is significant, it
will generate a higher pressure loss
in the reboiler outlet lines above the
intense-boiling region. Since the pres-
sure difference between Points 5 and
3 in Figure 1 is constant no matter
which path is taken, this higher pres-
sure loss in the nozzles above the in-
tense boiling zone will induce a higher
vapor flow into the outlet nozzles
closer to the outlet baffle.
Mysteries explained
This overall assessment of the reboiler
operation led us to the development of
a model. Described in greater detail
in Reference [8], the model quantifies
the theory presented above, and it ex-
plains all of the observations.
The model confirms a maldistribu-
tion situation: a single zone can han-
dle substantially more than the de-
sign liquid flowrate and produce much
more than the design amount of vapor,
based on a much improved tempera-
ture driving force. Further, the model
confirms that this high vapor produc-
tion comes about because of relatively
small gradients in head within the
tube field, brought about by regions
of low froth density due to high vapor
production. The relatively inactive
zones explain the lower-than-design
overall heat transfer.
The regional maldistribution pattern
reported here may be universal among
kettle reboilers. But in most cases, it
will not result in significant perfor-
mance issues. Instead, this maldistri-
bution is more significant in reboilers
for mixtures such as those used in ex-
tractive distillation, where the boiling
liquid consists of a large concentration
of very high boilers and a small concen-
tration of volatile components.
The mulitifeed, multidraw arrange-
ment plays a major role. A single feed,
single draw kettle would have experi-
enced a different maldistribution pat-
tern, possibly even more severe.
A stagnant region or dead zone is
formed in the tubesheet quadrant by a
self-accelerating mechanism. With little
disengagement space, not much boiling
takes place. The low-boiling compo-
nents tend to preferentially vaporize
out of the liquid, so the liquid becomes
rich in the non-volatile component. The
nonvolatile liquid, with little aeration,
develops a high hydrostatic head, which
resists movement of fresh liquid into
this region and promotes stagnation.
This region could constitute a signifi-
cant performance issue, with lower than
expected heat transfer rates, or lead to
fouling in heat sensitive materials
The high hydrostatic head in the
stagnant zone, and the enhanced
amount of fresh feed diverted into the
central region, initiate a region of high
L/V ratio, with vigorous boiling in the
bulk of the bundle. The boiling is prob-
ably accompanied by entrainment into
the overhead vapor line, low fractional
vaporization, and a relatively high
concentration of lights.
Finally, the region near the overflow
baffle receives close to the design feed
flow and has ample disengagement
CHEMICAL ENGINEERING WWW.CHE.COM FEBRUARY 2004
space, and is the only region behaving
like a kettle.
This pattern explains all the ob-
servations made: the high pressure
drop, the measured temperatures, the
lower heat transfer coefficient (caused
by the stagnant region), and even the
likely entrainment.
The regional maldistribution pat-
tern reported here gives complete
support to the assumption that the
reboiler liquid head in Equation (1),
hs,REB, is the static head of non-aer-
ated liquid in the reboiler. This head
is set by the static head of the liquid
in the stagnant region. This explana-
tion closes the loop on the reason for
the chimney tray overflow. The high
reboiler static head, plus the high re-
boiler outlet line pressure drop led to
the high liquid heads in the chimney
tray. Entrainment from the intense
boiling central zone could also have
been a contributor.
The low temperatures at the vapor
outlet nozzles right above the intense-
boiling region were caused by the high
L/V ratios in this region, possibly as-
sisted by entrainment. Above the kettle
region, the L/V ratios were much lower,
and so was entrainment, leading to the
higher than expected temperatures.
The high temperatures measured
near the walls of the exchanger were
caused by horizontal flow of hot liquid
from the stagnant zone along the wall
towards the boiling zones.
The wall-supported foaming ob-
served on the Oldershaw tests, and
the slight foaming observed in the
foaming tests, could also be a contrib-
uting factor that could aggravate the
intense boiling effect.
The malfunction reported here,
namely, excess pressure drop in a
kettle reboiler circuit when compared
to the available head, was identified
[7] as the most common malfunction
experienced in reboilers. The employ-
ment of good design practices, coupled
with compiling a valid reboiler pres-
sure balance, can readily circumvent
such malfunctions.
In contrast, the maldistribution
pattern reported here has not previ-
ously been reported. It is unique to
mixtures such as those encountered in
extractive distillation, where the boil-
ing liquid consists of a large concen-
59

Operations & Maintenance
tration of high boilers and a small con-
centration of volatile components.
This maldistribution affects both ket-
tle heat transfer and pressure drop,
and it, too, needs to be accounted for
in the kettle design.
Lessons for design
Kettle reboiler designs should:
1. Strictly adhere to the reboiler pres-
sure-balance equation. Four-fifths
of kettle reboiler malfunctions are
caused by excess pressure drops in
reboiler circuits [7].
2. Be based upon the clear liquid head
in the reboiler, not on aerated-liquid
head.
3. Take account of froth density gradi-
ents within the reboiler, and the re-
sulting maldistribution.
4. Trade off pressure loss through inlet
nozzles (which provide liquid distri-
bution to the reboiler) against the
head and column height required.
5. Consider a horizontal thermosiphon
60 CHEMICAL ENGINEERING WWW.CHE.COM FEBRUARY 2004
reboiler as an alternative for mix-
tures containing a large concentra-
tion of components boiling at high
temperatures together with compo-
nents that are volatile. ■ interest in process engineering. He holds a B.Sc.
Edited by Nicholas P. Chopey
References
1. Kister, H. Z., “Distillation Operation,” Mc-
Graw-Hill, New York, 1990.
2. Perry, J. H., “Chemical Engineers' Hand-
book,” 7th Ed., McGraw-Hill, New York, 1998.
3. Lieberman, N. P., “Process Design for Reli-
able Operation,” 2nd Ed., Gulf Publishing,
Houston, 1988.
4. Palen, J. W. and Small, W. M., Kettle and Internal
Reboilers, Hydrocarb. Proc., 43 No. 11, p. 199, 1964.
5. Fair, J. R. and Klip, A., Thermal Design of
Horizontal Reboilers,” Chem. Eng. Prog., p.
86, March 1983.
6. Ishihara, K., others, Critical Review of Correla-
tions for Predicting Two-Phase Flow Pressure
Drop Across Tube Banks, Heat Transfer Engi-
neering, 1, No. 3, p. 23, January–March 1980.
7. Kister, H. Z., What Caused Tower Malfunc-
tions in the Last 50 Years?, Trans. IChemE,
Vol. 81, Part A, p. 5, January 2003.
8. Rubbers, E., Green, K., Fowler, T., Kister, H. Z.,
and Stupin, W. J. Once-Thru Reboiler Startup
Can be Exciting, in “Distillation 2003: on the
Path to High Capacity, Efficient Splits,” Proceed-
ings of Topical Conference, AIChE Spring Meet-
ing, New Orleans, La., March 31–April 3, 2003.
Authors
Etienne Rubbers is a corpo-
rate finance consultant for
Sasol (Rosebank, Johannes-
burg, South Africa; Phone:
+27 11 441 3472; e-mail: eti-
enne.rubbers@sasol.com), in-
volved in merger and acquisi-
tion activities. Previously, he
was a process engineer in the
concept development group,
developing a number of the
firm’s projects from concept to
basic engineering, construction and commission-
ing. Despite his career change, he still has keen
(chemical engineering) from Wits University
(Johannesburg) and a master’s degree in indus-
trial management from Belgium’s University of
Leuven, and is a CFA charterholder.
Kirsten Green is a senior
process engineer for Sasol
Technology (Phone: +27 11
344 0082; e-mail: kirsten.
green@sasol.com). She started
her career at Sasol’s coal
preparation plant, gaining ex-
perience in materials han-
dling. She then joined the con-
cept development group,
where she has been involved
in feasibility studies for the
company’s chemical projects. She spent the past
year on rotational training with MWKL in Lon-
don, doing basic engineering in petroleum refin-
ing. She holds a B.Ing. from the University of
Stellenbosch and an M.Sc. from University of
Cape Town, both in chemical engineering.
Terry-Ann Fowler is a senior
process engineer for Sasol
(Phone: +27 11 344 0092; e-
mail: terry.fowler@sasol.com).
She forms part of a team in-
volved in conceptual develop-
ment and design of a number
of the firm’s chemical and re-
finery projects. She has
gained experience on projects
from pilot plant studies,
through feasibility and con-
ceptual development, basic engineering, and on
to construction and commissioning. Her B.Sc.
and M.Sc., both being in chemical engineering,
are from the University of Cape Town, and her
Ph.D., also in chemical engineering, is from Wits
University.
Henry Z. Kister, a Fluor
Corp. senior fellow and direc-
tor of fractionation technology
(Phone: 1-949-349-4679; e-
mail: henry.kister@fluor.com),
has over 25 years experience
in design, troubleshooting, re-
vamping, field consulting, con-
trol and startup of fractiona-
tion processes and equipment.
Previously, he was Brown &
Root’s staff consultant on frac-
tionation, and worked for ICI Australia and Frac-
tionation Research Inc. (FRI). The author of text-
books “Distillation Design” and “Distillation
Operation,” as well as 70 published technical arti-
cles, he has taught the IChemE-sponsored “Prac-
tical Distillation Technology” course 250 times. A
recipient of Chemical Engineering’s 2002 Award
for Personal Achievement in Chemical Engineer-
ing, Kister holds B.E. and M.E. degrees from the
University of NSW in Australia. He is a Fellow of
IChemE and a member of AIChE, and serves on
the FRI Technical Advisory and Design Practices
Committees.
Walter J. Stupin is an exec-
utive director for Fluor
(Phone: 1-949-349-5209; email:
walter.stupin @fluor.com). He
manages and executes process
engineering for petroleum re-
fining and chemical plants.
His over 40 years of process
engineering experience
ranges from vice president of
technology at C F Braun Inc.
to research at Fractionation
Research Inc. (FRI). The distillation field has
been an area of key interest, in which he has
published over 20 technical papers. Dr. Stupin
holds B.S., M.S. and Ph.D. degrees, all in chemi-
cal engineering, from the University of Southern
California.