n

THEODORE J. WILLIAMS
Monsanto Chemical Co., St. Louis, Mo.

Instrumentation and Control of Distillation Columns

Automation of a continuous distillation column is tricky. Work in the past has
either been on experimental columns or involved mathematical theory. Here is in-
formation which combines both-and forms the basis for a workable arrangement
for controlling distillation columns.

C~SIDERARZE has been cbritten on

distillation as a unit operation and diffi-
culties encountered in column control.
Most of the early work was either em-
pirical or devoted to experimental
studies of distillation column control
(4, 5, 7, 70, 72, 14, 75, 20, 27), but
recently several theoretical or mathe-
matical studies have appeared (7,22-24).
However, there has been little correla-
tion between these two types of investi-
gations.
I n this work such a correlation is
attempted by developing, on purely
theoretical bases, an optimum control
scheme for a distillation column.
Basic Factors of Distillation Control
Variables of Distillation Process.
For any distillation column, only six
independent operating variables are
needed to define its operation.
External Independent Variables
1. Feed rate
2. Feed composition
3. Feed temperature or feed quality
4 . Ambient pressure of operation
Internal Independent T7ariablee
5,6. Two of the following four
quantities:
Overhead product composition
(complete)
Bottoms composition (complete)
Boil-up rate-feed rate ratio
Feed split or distillate bottoms
ratio
Semi-independent Variables of Column
Operation
1. Location of feed tray
2. Column reflux temperature
For a binary mixture, the overhead
product and bottoms composition is
given by the mole fraction of only one
component. For a multicomponent
mixture of n components, the mole
fraction of n - 1 components must be
specified. 'This condition is assumed
to prevail in this work, where the over-
head or bottoms composition is con-
sidered.
The semi-independent variables of
feed tray location and of reflux tempera-
ture can affect distillation column con-
trol. However, in distillation theory
these are secondary factors usually con-
sidered noncritical. For simplification,
it is assumed that the optimum feed
tray location has been chosen and that
the reflux is returned at its boiling point.
Thus proper choice of the six main vari-
ables will permit determination of all
the dependent variables for any given
mixture. such as:
Dependent Variables
Liquid composition. Bottoms, plate.
distillate
T7apor compositions at each plate
or location in the column
All unspecified flow rates. Liquid,
vapor, distillate take-cff , bottoms take-off
Temperatures at each location in col-
umn

12 14 INDUSTRIAL AND ENGINEERING CHEMISTRY

 These dependent variables are, of
course, interrelated through the ther-
modynamic laws governing the vapor-
liquid equilibria of the mixture and by
the material balance requirements of
the column itself.
The basic problem in distillation
control can now be resolved into three
parts: determining which two of the
four possible internal independent vari-
ables should apply, which method is
most direct for sensing variations in
independent variables specified as con-
stants, and how the displaced variable
can be restored to its chosen operating
value through adjustment of the con-
trolled system. If the internal vari-
ables are to be truly independent, it is
absolutely necessary that the boil-up
rate be specified as the ratio of the re-
spective stream rate to the feed rate
rather than as simply that variable’s
rate of flow alone.
Classes of Distillation Control. O n
the basis of these statements, several
schemes for distillatioQ column control
may be suggested (Table I and Figure 1).
Because of the instrumentation system
chosen for each control scheme, certain
internal independent variables should
be selected. I n Table I, these systems
are arranged in order of increasing
flexibility to illustrate the development
of the optimum system.
The scheme of Figure 1, A, requiring
a constant feed composition, is the
simplest example possible and seems
entirely unrealistic in most plant situa-
tions. This method has been called
inferential or environmental control
(9), and succeeds only when it can pre-

Figure 1. Comparison of simple inferential or environmental control with proposed, more sophisticated schemes.
Units en-
circled by arrows show successive stages in control scheme rearrangement required for necessary flexibility of operation
A. Original arrangement; 6. This allows far smoother control of heads composition but constant feed still required) C. Ratio of boil up rate to feed rate
permits some flexibility; D. Composition detection of heads sample allows ultimate degree of control

VOL. 50, NO. 9 SEPTEMBER 1958 1215

 a

vent all upsets originating from external

sources from reaching the column. RE LA TI VE VOLA T I L I T Y 3(

Here flow controllers alone are sufficient Figure 2. Pressure must be closely controlled, if temperature is to b e the pri-
to maintain steady operation because mary column variable detected by the sampler
only boil-up rate and distillate take-off
rate need be kept constant.
.4 constant feed rate, as required by
1, B, can be attained either if sufficient
tankage can be installed between the
column and the preceding plant unit
or if it is the first element in a processing
line. The desire for true flexibility of
operation, however, leads to the scheme
of C. Here the resetting of the reboiler-
steam, input-rate control by a cascade

," - PROPORTIONAL CONSTANT

00 10 20 30 40 50 60 70 a t
PROPORTIONAL CONSIANT

Figure 3. Diagrams of allowable ranges of controller settings show relations

of sampling for five-plate column
Relative volatility, cx = 5.0 ( 1 6 )
A. Top plate sampling only
B. Intermediate plate sampling only

12 1 6 INDUSTRIAL A N D ENGINEERING CHEMISTRY

 DISTILLATION COLUMNS

A TE

-p,...
7 OUT

The ultimate control scheme for a distillation column embodies results of theo-
This simplifies the control of cooling
water, but makes the use of temperature
alone as a composition detector im-
possible. In such a situation some
device must be used which measures
composition directly or meavures an-
retical studies to give automatic control other composition-sensitive but non-
temperature-sensitive property, because
controller operating from feed input
rate measurements makes it possible to
maintain the boil-up rate-feed rate
ratio mentioned. I t would then be
easily possible to maintain the distil-
late take-off rate necessary to keep the
feed split at that value determined by
the instantaneous feed composition as
it varies. Thus the feed rate and feed
composition can vary independently, as
long as the physical limitations of the
column, such as flooding rate, are not
exceeded.
Designation of the boil-up rate-feed
rate ratio and the overhead product
composition as the specified internal
variables allows feed quality to vary
along with the feed composition. Slight
variations of distillate take-off rate will
automatically compensate for the flow
variations caused by quality shifts.
Thus, the simple constant temperature
feed preheat control of Figure 1, A ,
can be retained throughout. If this
temperature can be set to give a feed
quality of 1.0 a t the lowest feed composi-
tion expected and if the feed mechanism
can handle a mixed feed, such an ar-
rangement helps to smooth out column
composition fluctuations caused by the
change in feed composition itself (24).
Figure 1, D, carries the scheme of
C one step further and allows the am-
bient operating pressure to vary also.

VOL. 50, NO. 9 SEPTEMBER 1958 12 17


temperature will vary drastically with
pressure.
Figure 2 relates the boiling point-
Le.: tray temperature-variation to the
resulting composition variation for vari-
ous relative volatilities of binary mix-
tures. I t is therefore necessary to main-
tain a very close control of pressure, if
temperature is to be the primary column
variable detected by the sampler for
control purposes. Otherwise, another
property must be used for satisfactory
results.
Thus boil-up rate-feed rate ratio and
overhead product composition are speci-
fied as the optimum internal variables
for control. Is this really so? The
present situation allows the bottoms
take-off rate to be determined by an
auxiliary level controller in the reboiler,
Thus a constant heat transfer area is
maintained in the reboiler and boil-up
rate control can be tied directly to
steam input rate. Any other scheme
would result in level fluctuations with
corresponding heat transfer area varia-
tions in the reboiler. Thus the steam
rate andlor pressure would have to
vary in a complex manner to maintain
the boil-up rate at its established value.
Bottoms composition may be used as
an independent variable, but because
pot volumes are usually ten or more
times greater than plate holdups, bot-
toms composition can vary only a t a
correspondingly slower rate than any
plate compositions. Thus a much
greater sensitivity can be attained with
overhead product composition as the
independent variable, even when the
bottoms is the desired product.
Problems in Top of Column
Sampling
Effect of Dead Space in Samplers.
Automatic control theory demands that
an error detector be located as close
as possible to the point in the system
12 18 INDUSTRIAL AND ENGINEERING CHEMISTRY
These recommendations should be helpful in considering dis-
tillation column control systems.
b For maximum flexibility, cycle must be used, the
primary column control should sampling cycle should be kept
maintain boil-up rate-feed as small as possible-less
rate ratio and overhead com- than one half the mixing time
position constant. constant of the column plates.
b Sampling the top plate b
The rate control mode or
will give the best control, if derivative control is ineffec-
the sampling device is sen- tive for distillation column
sitive enough to detect the control.
required range of composi-
tion variations. When top plate sampling
b When the sampling device can be used, the proportional
has an appreciable dead band mode alone is suffi-
space error, sampling on a cient. For all other plates
lower plate than the top reset rate or integral control
plate may give a more ac- is necessary for the compo-
curate control. Dead space sition controller.
error should be kept as low
Condenser holdup should
as possible.
be kept small, as it i s desta-
b When a composition sam- bilizing. Still pot holdup is
pler working on an intermittent stabilizing.
Table I. Relation of Choice of Independent Internal Variables to Possible Action
of External Variables
External Variable Refer
Feed Feed Feed Ambient to
rate composition quality pressure Choice of Internal Variable Figure 1
Fixed Fixed Fixed Fixed Boil-up rate-feed rate ratio A
Distillate rate-bottoms-rate ratio
Fixed Variable Variable Fixed Boil-up rate-feed rate ratio
Overhead composition B
Variable Variable Variable Fixed Boil-up rate-feed rate ratio
Overhead composition C
Variable Variable Variable Variable Boil-up rate-feed rate ratio
Overhead composition D
Table II. Summary of Recommended Control Scheme
Main Control Functions
Method of Determining and Regulating
Designated Independent Internal S'arlable Required Variation
Overhead product composition Sampled by dependent variable near top of
column and maintained as constant as
possible by resetting reflux rate controller
Boil-up rate-feed rate ratio Variations of feed rate detected by flow
controller and used to reset steam input
rate controller previously set at some
intermediate rate for task at hand
Required Subsidiary Controls
Subsidiary I'ariable Method of Control
Feed preheater on feed line
Feed temperature
Bottoms take-off rate Levei control on reboiler
Pressure (where necessary for temperature Variation of condenser cooling water rate
elements)
Distillate take-off rate Level control on accumulator
 lDlSTlLLATlON COLUMNS

where the control correction is applied, 60

so that overcorrections do not cause
an oscillatory response of the control \
system (78). Studies of distillation \
50
column responses under automatic con-
trol when carried out on analog com- \,
puters (76,24) show that the top plate \
of a distillation column can give over
ten times as close control as an interme-
diate plate. This is because fluid flow
lags on plates located between the
error-detecting and control points allow
I

I
2
40

30
\
\
'... . \
IU
\
the oscillations to occur as soon as
the controller settings are greater than
2
& \
some given small value. Figure 3 20 - \,

shows this, because it diagrams the al- \

lowable range of controlleq settings for \
each case. \
The results shown here were obtained

now greater than the expected excursion

on the controlled variable. Figure 7, A , /
and B classifies the cause, of the resulting
output error, while Figure 7, C, shows
the effect of going still further down the Figure 5. Graphical representation of dead space
column t o pick the sampling point.
The actual choice of the sampling
point is thus a compromise between the 0 05
unavoidable output errors due to con-
trol system oscillations and those due
to the low sensitivity of the detector. 0 04
The only solution is to produce a sen-
sitive detector (temperature or other-
wise) and locate it as close to the top of
--
I
+I

2 003
the column as possible. Y

Effects of Intermittent Samplers. c

c
Another factor which can have a major
002
effect upon the control method chosen
is the greatly increased use of samplers
which determine composition directly
but operate on an intermittent cycle. 0 01

Mass spectrometers and scanning infra-

red and ultraviolet analyzers fall into
this category (79). Many of these in- 00
00 0 01 0 02 0 03 0 OA 0 05
struments, because of their high cost,
are used to determine the output a t DEAD SPACE

several different sampling points through Figure 6. For a dead space of less than 0.01 5 mole fraction, top plate
a time-sharing system. sampling is best

VOL. 50, NO. 9 SEPTEMBER 1958 12 19

 00 c 01 0 02 0 03 0 04 0 05
D E A D SPACE

A. Sampling on top plate only

Figure 8 shows how such a device
might operate. This one is a postulated
spectrometer used to determine several
components in a multicomponent stream.
Figure 9 is another diagram of the time
0c5 -
sequence of events occurring in such a
device; Figure 10 compares the results
as determined by the analyzer to the
actual stream composition sampled.
The response of a computing spec-
trometer such as this or any of the other
intermittent devices mentioned above,
~ v h e nused as part of a control system,
has been extensively studied by analog
simulation methods (23) (Figure 11).
For spectrometers operating on very
fast cycles-Le., period of operation
less than the basic liquid residence
Eime on a plate; time constant, 7, top
plate sampling gives much better con-
trol; the allowable controller setting s 01 0 02 0 03 0 04 0 05
is much tighter. For long-period sam- D E A D SPACE
plers it makes little difference whether
E. Sampling on Intermediate plate only

:. 003

/
,OQ/
/
Q
Lb%\/
/
/
/

/n DD IiI ONA L c o NT R I 8 u T Io N
OF D E A D S P A C E TO OUT
PUT ERROR
\

001-
/’ P R O B A B L E ERROR DUE T O FLUID FLOW LAG
/
/
//
I

co 1 I

00 0 0‘ 0 02 0 03 0 04 0
D E A D SPACE

C. Sampling possible on plate two down from top plate

Figure 7. Actual choice of sampling point is a compromise among

unavoidable output errors
5-plate column. a = 5.0 ( 2 4 )

1 220 INDUSTRIAL AND ENGINEERING CHEMISTRY

 DISTILLATION COLUMNS
the sampler is located on the top plaFe
or lower down. The deterioration of
CORRECTION SIGNAL
sensitivity due to enforced sampling
SAMPLING POINT I N REFLUX
TO COLUMN time lags quickly equals that due to
LINE OR O N ONE OF COLUMN
1 CONTROL VALVES fluid flow lags within the column (23).

SPECTROMETER OBTAINS MASS OR

I Semi-independent Variables of
ABSORPTION SPECTRUM A N D EVALUATES
TO DETERMINE COMPOSITION OF Column Operation
COMPONENTS OF SAMPLE STREAM
LENGTH OF FINITE TIME PERIOD REQUIRED I Optimum Feed Plate Location. One
SAMPLING LINE of the semi-independent variables of
CAUSES FINITE - column operation is feed plate location.
COMPUTING CONTROLLER
TRUE TIME DELAY
SPECTROMETER If feed composition does not vary greatly,
CONTROLLER OPERATES O N COMPOSITION
one feed plate location is sufficient.
A S DETECTED B Y THE SPECTROMETER AND However, for some possible wide varia-
ASSOCIATED COMPUTER.COMPARES WITH DESIRED tions of feed composition "pinches"
VALUE A N 0 COMPUTES CORRECTIONS TO VALVE and a corresponding reduction in column
SETTINGS separating capacity may occur beyond
Figure 8. This is the way such a device might operate the capacity of the control system to
correct. Thus some sort of automatic
feed plate changes would be desirable.
Figure 12 shows a sample chart of the
/
F I R S T SAMPLE FIRST SAMPLE TO
TAI(EN HERE C O N T R O L I E R HERE optimum feed plate locations for a
TIME REQUIRED TIME REQUIRED 10 PERIOD OF USE small column. Feed plate location is a
k F O R SAMPLE L I N E - ~ E V A L U A T sPECTIIU&-OF
E FIRST SAJPLE function of the feed quality as well as
comparison of the actual feed composi-
tion to the reference or median feed
SECOND SAMPLE SECOND SAMPLE TO composition. Such a chart can be
/ TAKEN HERE , CONTROLLER HERE developed for any given column and

f- TIME REQUIRED
FOR SAMPLE LINE +tEVALUATE
TIME REQUIRED T O
SPECTRUM?
OF USE OF
+PERIOD
SECOND SAMPLE 1 feed mixture. The resulting data can
then be used to set a controller which,
by means of quick-opening valves,
transfers the feed from plate to plate
as necessary when the feed composition
I
THIRD SAMPLE
T A K E N HERE
THIRD SAMPLE
TO C0,NlROLLER varies.
Effect of Reflux Temperature. In
a
all cases except Figure 1, A , care has
been taken to control the amount of
reflux fed back to the column rather
FOURTH SAMPLE

+
~ ~ t ~ E N R ~ Q Y t R E D
FOR SAMPLE LINE

Time, t -
Figure 9. Time relation of events in operation of intermittent sampling model

V A R I A T I O N OF OUTPUT
A C T U A L V A R f A T l O N OF[
A S USED B Y CONTROLLER
OUTPUT
TIME D E L A Y
2 1 %

Figure 10. Comparison of real output of process and that used by controller

VOL. 50, NO. 9 SEPTEMBER 1958 1221

 or other analyzer results has not been
recommended. Analog computer sim-
ulation indicates that good column con-
trol can be achieved without the com-
plexity and expense of a digital com-
puter to determine the operating pa-
rameters ( 6 ) .
Analog computer simulation has also
shown that only proportional and in-
tegral control modes can give adequate
I action in the control of a distillation
TOP PLATE SAMPLINI column. The derivative or rate mode
A INTERMEDIATE PLATE proved completely ineffective for all
SAMPLING cases tried. This fact has also been
noted by several experimental investi-
I gators. I t is therefore recommended
that only two mode controllers (pro-
I portional and integral or reset) be
procured for this purpose.

References
(1) Bauer, R. L., Orr, C. P., Chem. Eng.
PrOgr. 50, 312-18 (1954).
(2) Berger, D. E., Campbell, G. G.,
Ibid., 51, 348-52 (1955,.
(3) Berger, D. E., Short, G. R., IND.
IO0
ENG. CHEM.48. 1027-30 (1956).
IO 10
(4) Boyd, D. M.; Jr., Petrot. Re&r 27,
S A M P L I N G INTERVAL, I, IN SECONDS 115-18 (October 1948); 114-17 (No-
vembpr 1948’1.
-,
Figure 1 1. For spectrometers operating on very fast cycles, top plate (5) Coulter, K. E., Ibid., 31, 137-8
sampling gives best control (December 1951).
(6) Engel, H. L., Control Eng. 4, 144-7
than to control the amount of distil- the reflux control scheme of Figure (September 1957).
(7) Gallagher, G. G., Petrol. Refiner 27,
late withdrawn directly. because any 1, B to 1, D, prevents such oscillations 116-17 (March 1948).
fluctuations in condenser vapor rate from occurring. (8) Hoyt, P. R., Stanton, B. D., Ibid., 32,
would be propagated by an accumu- 113-19 (October 1953).
lator level controller to the reflux stream (9) Kiguchi, S. T., Ridgway, R. L.,
Optimum Column Control Scheme Ibid., 35, 179-84 (December 1956).
in the case of 1, A . This must be avoided (IO) Moore, H. F., Gross, G. W., Petrol.
whenever possible, as such fluctuations The optimum control scheme for the Processing 1948, 441-8 (May 1948).
can be self-propagating and can lead majority of distillation column applica- (11) O’Connor. Ward. A.1.Ch.E. Suring
’ Meeting.”, Philadel&ia. Pa.. 1954: ”
to sustained control oscillations if a tions includes the recommendations
(12) Perrv, C. W., ‘Chem. @’ Met. Eng.
cold reflux is used on the column. developed in the previous discussions. 52, 108-12 (October 1945).
By effectively choking off such fluc- Control of the column by any type (13) Poffenberger, Xoland, private com-
tuations at the accumulator and trans- of automatic computer other than that munication, -.4ugust 1955.
ferring them to the distillate stream, necessary to evaluate the spectrometer (14) Rector, N. K., Petrol. Processing
1949, 525-8 (May 1949).
(15) Reynolds, E. H., Troutman, Wil-
c liam, Lawn, Gordon, Petrol. Rejner
x
i 26, 132-6 (April 1947).
0 (16) Rose, Arthur, Williams, T. J.,
-
v)
Ih-D. ENG.CHEM. 47, 2284-9 (1955).
2 (17) SOC. Instrument Technol., ”Plant
0
and Process Dynamic Characteristics,”
Butterworth Scientific Publications, Lon-
u, don, 1957.
4 (18) Thaler, G. J., Brown, R. G., “Servo-
u. mechanism Analysis,” McGraw-Hill,
0 New York, 1953.
LL (19) Thomas, B. W., IND. ENG. CHEM.
46, 1371-441 (1954).
i (20) Tivy, V. V. St. L., Petrol. Refiner
0 27, 123-8 (Sovember 1948).
-
v)
(21) Uitti, K. D., Ibid., 29, 130-4 (March
2 1950); Petrol. Processing 1950, 41-4
0
U
(January 1950).
(22) Williams, T. J., Ph.D. thesis, Pennsyl-
E vania State University, 1955.
L

i
(23) Williams, T. J., Harnett, R. T.,
4 Chem. Eng. Progr. 53, 220-5 (1957).
2 (24) Williams, T. J., Harnett, R. T.,
4 ROW,Arthur, IND.END.CHEM.48, 1008-
19 (1956).

01 02 03 04 05 O b 07 0; 09 RECEIVED
for review J’anuary 29, 1958
REFERENCE FEED C O M P O S I T I O N ACCEPTED May 19, 1958
‘ 0

Figure 12. Best feed plate location depends on feed quality as well New Jersey Section, ACS, January 27,
as composition 1958.

1222 INDUSTRIAL AND ENGINEERING CHEMISTRY