Source: A Working Guide to Process Equipment

CHAPTER

41

Super-Fractionation
Separation Stage

he concept of the super-fractionation separation stage in

distillation is a key concept in process operations and chemical
engineering. Yet I have never seen this idea discussed in any
text concerning distillation.
The effect is observed in two areas of a distillation operation:
Partial condensation
Once-through thermosyphon and kettle reboilers

The concept of a super-fractionation tray is important when

separating products, if either the top or bottom product consists of a
multicomponent mixture. For example, if we are fractionating only a
mixture of propane and isobutane, the super-fractionation concept
would not be significant. However, if the product consisted of a
mixture of ethane, propane, and isobutane (i.e., C2s, C3s, and C4s) and
the overhead condenser was a partial condenser (see Fig. 41.1), then
the partial condenser would serve as a super-fractionation stage. The
partial condenser would contribute far more to fractionation than any
of the other stages in the upper portion of the distillation tower.
If the bottom product consisted of a mixture of isopentane, normal
hexane, and normal heptane (i.e., C5s, C6s, and C7s) and the reboiler
was a kettle-type reboiler (see Fig. 41.2), then the kettle reboiler would
serve as a super-fractionation stage. The kettle reboiler would
contribute far more to fractionation then any of the other stages in the
lower portion of the distillation tower.

41.1

My First Encounter with Super-Fractionation

In 1969, I was working for Amoco Oil as a process design engineer. One
of my earliest designs for Amoco was a gasoline debutanizer, the bottom
portion of which is shown in Fig. 41.3. Note that this tower is equipped
with a once-through thermosyphon reboiler. Such a reboiler works as
the bottom theoretical stage of the debutanizer assuming that:

517
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A Working Guide to Process Equipment

Net vapor
product

Total reflux

FIGURE 41.1

A partial condenser serves as a super-fractionation stage.

1. All of the liquid from the bottom tray flows to the reboiler.
2. Valve A is closed.
But valve A was not closed. I had opened the valve myself during
the initial tower start-up. Opening valve A is a necessary part of the
tower start-up procedure. This allows liquid to gravitate out of the
bottom of the tower and into the reboiler, the objective being to
establish thermosyphon circulation until a vapor flow is established
through tray deck one. However, when I tried to close valve A, the
reboiler duty died off, indicating a loss of flow into the shell side of

B
CLOSED

FIGURE 41.2

Net
bottoms
product

A kettle reboiler serves as a super-fractionation stage.

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Super-Fractionation Separation Stage

Chapter 41:
FIGURE 41.3
Once-through
thermosyphon
reboiler is also a
super-fractionation
stage.

S u p e r- F r a c t i o n a t i o n S e p a r a t i o n S t a g e

200F
(8)

519

Feed

200F

(1)

Seal pan

400F

300F
Draw
pan

Heat

CLOSED
Gasoline
400F

the reboiler. So, I was forced to leave the start-up line (i.e., valve A
shown in Fig. 41.3) open to sustain the reboiler duty.
The reboiler now seemed to work fine. The problem was that the
debutanizer tower was not doing a good job of debutanizing. The
butane content of the gasoline bottoms product was 4 percent. My
design for the tower was based on 1 percent butane in gasoline.
Something was terribly wrong.
I rechecked my computer model for the tower. With an assumed
80 percent tray efficiency, which is normal for this service at the
observed reflux ratio, a 1 percent butane in the gasoline would be
expected. To force my computer model to match the observed 4 percent
butane in the gasoline, I had to assume a low 40 percent tray efficiency
for the bottom eight trays. I concluded something was wrong with
these trays.

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My boss organized a meeting with the plant manager. I reported
that the bottom eight trays must have been damaged on start-up as
indicated by their low tray efficiency of 40 percent, as compared to
their design tray efficiency of 80 percent.
The plant manager was doubtful. Perhaps, he asked, this could be
an installation error? Perhaps, he wondered, the trays had not been
installed properly?
No, thats not possible, I replied, as I had personally inspected
the installed trays and approved the tower as ready for closure. No,
the trays were designed and installed properly. They must have
been damaged on start-up. I advised that we should now order new
replacement trays. We should shut down the debutanizer as soon as
the replacement trays arrived.
When the new trays were delivered, the debutanizer was taken
offline, steamed out, and opened. When I entered the tower, I discovered
that each and every tray in the column was totally and completely
intact and clean. Everything was just as I had last seen it six months
ago. Actually, the only thing that had changed was me. I had become
smarter in the last six months. For example, I now noticed that the
sides of the draw pan (see Fig. 41.3) were missing. True, they had been
missing last year too, but I had not noticed their absence then.
This explained why I had been forced to open valve A (the start-up
line) to get flow to the reboiler. That is, the liquid from the bottom tray
seal pan was largely overflowing the draw pan and bypassing the
reboiler. Hence, the only way I could get enough liquid into the reboiler
was to gravitate it out of the bottom of the tower through valve A.
But could this explain the poor fractionation efficiency in the
bottom of the debutanizer? How could opening valve A reduce the
apparent tray efficiency of the bottom eight trays from 80 percent to
40 percent?
The temperatures shown in Fig. 41.3 are design temperatures:
Tray eight temperature = 200F
Bottom tray temperature = 300F
Reboiler outlet temperature = 400F
Tower bottom temperature = 400F
The tower bottom and reboiler outlet temperatures are both 400F.
This is because all the liquid from tray 1 is supposed to be drawn off
to the reboiler. The only liquid in the bottom of the tower is the liquid
portion of the reboiler effluent.
But if valve A is opened, and the feed to the reboiler is coming
from the bottom of the tower, then the reboiler outlet temperature
must be hotter than the tower bottoms temperature. This temperature
difference would be quite small if we had essentially a pure component
(like butane) as the tower bottoms product. But with a wide boiling

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Chapter 41:

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521

range mixture (like gasoline) as the tower bottoms product, the

reboiler outlet temperature would become much hotter than the
tower bottom temperature.
As the amount of liquid overflowing the draw-pan increases, and
the amount of liquid flowing to the reboiler decreases, the tower bottoms
temperature will start to approach the tray temperature. For example,
with valve A wide-open, I had observed the following temperatures:
Observed

Design

Tray 1

300F

300F

Tower bottom

320F

400F

Reboiler outlet

400F

400F

These temperatures indicated that most of the bottoms gasoline

product was coming from the bottom tray of the tower, rather than
from the reboiler effluent. Or, the once-through thermosyphon reboiler
was no longer functioning as the bottom theoretical fractionation stage
of my debutanizer.
But so what? So what if I had lost one fractionation stage? I still
had eight other trays between the reboiler and the tower feed. So
what if I had lost one stage out of nine?
Unfortunately, not all stages are equal. The once-through
thermosyphon reboiler functions as a super-fractionation stage. It
provides not one-ninth but one-half of the fractionation in the bottom
portion of the debutanizer. After all, half of the temperature increase
(see Fig. 41.3) between the 200F tray-8 temperature and the 400F
tower bottoms product temperature occurs across the reboiler, provided
that all the liquid from tray 1 flows to the reboiler. The reason the
reboiler temperature rise is 100F is because heat is added to the reboiler.
Adding heat to a fractionation stage located below the feed point makes
that stage into a super-fractionation stage. If the bottoms product
bypasses this super-fractionation reboiler stage, then a large percentage
of the towers potential fractionation capacity is lost.

41.1.1 The Chickens Come Home to Roost

Looking at my computer model of the debutanizer confirmed my
worst fears. The butane content of the debutanizer gasoline was
4 percent from the second theoretical stage and 1 percent from the
first theoretical stage. Of course, the second theoretical stage of our
computer model is tray 1, and the first theoretical stage is the reboiler.
If the sides of the draw-off pan have been left off, then the colder, lighter
liquid from tray 1 will bypass the reboiler. This reboiler is doing half
of the fractionation work, hence, the overall efficiency of the lower
half of the debutanizer falls by one-half. The apparent overall tray
efficiency drops from 80 to 40 percent.

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A Working Guide to Process Equipment

My boss generously gave me the opportunity to explain all this to
the plant manager. I explained that we had extended the height of the
sides of the draw-pan by 18 in. The debutanizer was now back on-line.
Gasoline was on specification with 1 percent butane.
And the new trays? asked the plant manager. Were they
installed?
Not exactly. The new trays have been carefully placed as spares
in the refinery warehouse storage, I replied. They will provide a
useful hedge against any future cost inflation in replacement tray
charges. They are carried in our accounts as a passive asset.
For years thereafter, the plant manager consistently referred to
my anti-inflationary foresight as gross stupidity. His narrow-minded,
hostile, and totally unfair comments being based on my supposed
negligence in not observing that the sides of the draw pan were
missing before the initial start-up in 1969.

41.2

Kettle Reboiler
I could tell almost the same story about the kettle reboiler shown in
Fig. 41.2. In this case, we were trying to strip ethane out of a mixture
of propane, butane, and gasoline at the Good Hope Refinery in Norco,
Louisiana. Valve B had been left open because of fouling and highpressure drop on the shell side of the kettle reboiler. The kettle reboiler
also, like the once-through thermosyphon reboiler discussed above,
functions as the bottom theoretical stage of the de-ethanizer. Its a
super-fractionation stage because heat is added to the stage. Opening
valve B permitted the bottoms product to bypass this superfractionation stage. We didnt even open the tower. I just had the shell
side of the kettle cleaned. We could then run with valve B closed and
fractionation efficiency was restored to normal.

41.3

Partial Condenser
Figure 41.4 shows the overhead system of the Coastal Refinery crude
distillation tower in Aruba. The island of Aruba is a beautiful country in
the Caribbean Sea off the coast of Venezuela. I often take my wife, Liz,
on a romantic vacation to this tropical paradise. During one such exotic
trip I was assigned by Coastal to find a plan to improve fractionation
between naphtha and jet fuel. The problem was that the naphtha
contained 20 percent jet fuel. A computer simulation of the crude tower
indicated that the apparent tray efficiency of the upper five trays was
only 30 percent. However, fractionation between naphtha and jet fuel
occurs in two regions of the tower shown in Fig. 41.4:
Trays 16 through 20
The hot drum, where the reflux liquid is separated from the
naphtha vapor product

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523

CW
300F

215F
(20)

Hot drum

Cold drum

CLOSED
(16)
(15)

Jet fuel
380F

C
Naphtha
product

FIGURE 41.4

A partial condenser helps to separate naphtha and jet fuel.

To discriminate between the fractionation efficiency of the

trays and the hot drum, I obtained a sample of reflux from the
discharge of the hot drum reflux pump. It contained 25 percent jet
fuel and 75 percent naphtha. I compared the analysis of this sample
to my computer simulation. The degree of fractionation observed
between jet fuel and the reflux indicated a tray efficiency for trays
16 through 20 of 65 percent. This is a normal tray efficiency for this
service.
The partial condenser and the hot drum shown in Fig. 41.4 serve
as the top theoretical separation stage of this tower. The computer
simulation showed that the amount of jet fuel in the reflux should be
25 percent, and the amount of jet fuel in the naphtha product should
be 8 percent.
The samples showed that the amount of jet fuel in the reflux was
25 percent, and the amount of jet fuel in the naphtha product was
20 percent. The reason for the high jet fuel content of the naphtha
was, I found, that valve C shown in Fig. 41.4 was open halfway. The
operators had left valve C open to prevent a high liquid level in the
hot drum. In effect, this ruined the separation efficiency of the top
theoretical stage of the tower.
But why would ruining the separation efficiency of one theoretical
separation stage degrade the apparent tray efficiency of trays 16 through
20 from 65 to 30 percent? Well, because the top theoretical separation
stage represented by the partial condenser is a super-fractionation stage.
Heat is removed from that stage. The heat Im talking about is the duty
of the air cooler upstream of the hot drum.

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Any time heat is removed from a fractionation stage above a
towers feed point, that stage becomes a super-fractionation stage. To
prove my point, note the temperatures shown in Fig. 41.4:
The T between the jet fuel product draw-off (380F) and the
tower top temperature (300F) is 80F.
The T between the tower top temperature (300F) and the
hot drum temperature (215F) is 85F.
For wide boiling range mixtures, such as naphtha and kerosene,
the temperature difference across portions of a distillation tower
approximately correspond to the degree of fractionation achieved.
The Ts indicate that the amount of fractionation work done across
the top five trays is about the same amount of fractionation work
done in the top theoretical separation stage, which is represented by
the partial condenser. The partial condenser consists of the air cooler
and the hot drum.

41.3.1 Another Defect

I blocked valve C shown in Fig. 41.4, waited a few minutes, and
obtained a sample of product naphtha from the hot drum. Lab
analysis showed that the amount of jet fuel in the naphtha product
had dropped from 20 to 10 percent. Another victory to report to the
plant manager of the Coastal Refinery in Aruba.
Next day, I scheduled a meeting with the plant manager to
report on my success. But the plant manager had a different view.
His narrow-minded, hostile, and unfair comments were quite
offensive.
Lieberman, I had a check sample run on our naphtha product.
We now have 21 percent jet fuel in the naphtha, not 10 percent. Youve
made fractionation worse, not better.
I rushed out to the unit, suspecting that the operators had
reopened valve C (see Fig. 41.4). But it was still shut. What now?
Maybe it was best just to accept defeat. But then I looked up at the hot
drum, which was located just above valve C. It seemed as if the level
shown in the gauge glass was 6 to 10 in higher than it had been
yesterday. I then noticed that there was something odd about the
design of the hot drum.
Referring to Fig. 41.5, note that the vapor outlet nozzle is not on the
top of the drum, but on the side. And the liquid level in this drum
exactly coincided with the bottom of the vapor outlet nozzle. I suddenly
recalled a comment that the panel board operator made yesterday
when valve C was closed.
Seor Lieberman, have you noticed that the hot drum level has
increased from 61 to 69 percent?

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525

Partial condenser
outlet
Naphtha
vapor
outlet

Hot drum liquid

Reflux

FIGURE 41.5

Liquid carryover due to a high liquid level.

I didnt pay much attention to the comment because the liquid

level stabilized at 69 percent. But 69 percent coincided with the
bottom of the vapor outlet nozzle. The reflux that had been flowing
through valve C into the cold drum was now overflowing into the
cold drum through the vapor outlet nozzle.
Overflowing reflux from the hot drum into the cold drum
destroyed the efficiency of the super-fractionation stage represented
by the partial condenser. To restore this lost fractionation, I had the
panel board operator lower the reflux drum level to 60 percent by
increasing the tower top reflux rate. This time I waited a few hours
before pulling my naphtha product sample. Analysis then showed
there was now only 7 percent jet fuel in the naphtha product. Finally,
real victory!
Unfortunately, Liz unfairly characterizes this visit to the
Coastal Refinery in Aruba as just another business trip. She refuses
to acknowledge that she had been taken to an exotic island paradise
for a honeymoon vacation. She has persisted in this narrowminded view, disregarding the hundred or so trips we have made
to the Aruba Refinery, all of which have been, in part, romantic
adventures.

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41.4

A Working Guide to Process Equipment

Side Reboilers and Intercoolers

Side or outrigger reboilers are sometimes used to supplement the
capacity of the bottoms reboiler. Intercoolers or side slip-stream coolers
are sometimes used to supplement the capacity of the overhead
condenser.
Side reboilers and intercoolers also function as super-fractionation
separation stages. They are just a subcase of once-through thermosyphon
reboilers and partial overhead condensers.

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