Determination of Reflux Ratio and Boil-Up Rate for Distillation
Column with Intermittent Take-Off-Type Reflux Control
Yi-Chung Chang,' U. S. Bureau of Mines, Morgantown, W. Va., and Liang-tseng Fan,2
West Virginia University, Morgantown, W. Va.
N BATCH distillation work, accurate
I control of reflux ratio is important.
Reflux ratio isa major factor affecting
sharpness of separation and time of
distillation. Inaccuracy in its control
often leads to w o n g interpretation of
data.
One of the many reflux regulating de-
vices is an intermittent take-off type
[Brandt, P. L., Perkins, R. B., ,Jr.,
Halverson, L. K., Oil GUS J . 45, KO.
31, 86,102 (1946)], as shown in Figure 1.
The condensate from the reflux con-
denser falls into a small glass cup, to
which a distillate take-off tube is con-
nected a t the bottom. The interior of
the cup is ground t o form a valve seat.
A spherical plug, which fits into this
seat, seals the distillate tube when
reflux is to be returned to the column,
the reflux overflowing the cup.
In operation, reflux from the con-
denser falls into the cup, overflows, and
is returned to the column when the
valve is seated, closing the distillate
line; but the entire reflux is taken over-
head when the valve is lifted. The
reflux ratio can thus be controlled by
suitable timer switch actuation, open-
ing and closing the valve.
Depending on the size of the column,
the cup has a holdup of from 0.1 to 0.5
ml. and at each lift of the plug, one of
these quantities of distillate is taken
over, in addition to the proportion of
reflux indicated by the timer setting.
Vnder conditions of low vapor through-
put, this holdup becomes an appreci-
able part of the total distillate, and the
reflux ratio actually realized is consider-
ably different from that determined
by the timer setting as shown in Figure
2. If the boil-up rate were calculated
from the apparent reflux ratio deter-
mined by the setting of the timer and
the distillate collected in a certain time
interval, considerable error might result.
Using the conditions stipulated for
Figure 2 for a boil-up rate of 1000 ml.
per hour, the distillate collected in five
minutes is 10.3 ml. (assuming no leak-
age). This, when multiplied by 1 plus
the apparent reflux ratio, or 11, will
give a calculated boil-up rate of 1360
nil. per hour, n hich is 36% off the actual
value.
Hom-ever, the relationship between the
reflux ratio and the other operating
1 Present address, Research Center,
IT. S. Steel Corp., Jlonroeville, Pa.
Present address, Kansas State College,
Rlanhattan, Kaxi.
variables can be expressed by
BT - 3600_
= ~
C _
Bt +
3600 C
where
R = reflux ratio = reflux/product
B = boil-up rate a t top of column
excluding internal reflux, ml.
per hour
T = reflux time, seconds per cycle
t = discharge time, seconds per
cycle
C = volume of cup, nil.
In deriving this equation, it is as-
sumed that the spherical plug fits the
seat perfectly, so that during reflux
no condensate can leak out.
If leakage exists, Equation 1 may be
modified to include a leakage term.
BT - 3600 ( C T L ) +
R = Bt +3600 (C + TL)
where L = rate of leakage, ml. per
second.
T17ith values for B , C, and L given.
the reflux ratio can be calculated by
Equation 2 for each combination of
timer settings. Khen B, C, and L are
TOSO.E%OID
1 4 and 5, B and C can be obtained.
REFLJX
-CON3EVSE3
PACK€:.
COLLKk
Figure 1. Intermittent take-off reflux-
control device for distillation column
REFLUX . T I M E - 2 0 SEC.
O l S C H 4 R G E T I M E - 2 SEC.
c 5 CUP C A P 4 C I T Y - 0 2 ML
BOIL-UP R 4 T E . M U H R
Figure 2. Effect of boil-up rate on
corrected reflux ratio
not given, they can be determined ex-
perimentally.
To determine the leakage, the column
(1)
may be operated under total reflux and
the volume of the condensate collected
in the receiver over a certain interval
of time measured. Boil-up rate usually
has no appreciable effect on leakage;
the column can be operated a t any
convenient rate.
Boil-up rate may be determined by
a rate device placed between the pot
and the column [Nples et al.,
Znd. Eng. Chem. 43, 1452 (1951)l or
by the following formula, if the product,
P , collected during 1 hour is known.
B =
+
P ( T t ) - 3600(C TL) +(3)
t
In using Equation 3, C must be known
first. When both B and Care unknown,
(*I the product rate may be measured a t
t v o different timer settings using equal
boil-up rates, and these two sets of
values substituted in Equation 3.
+ +
B = Pi(T1 t i ) - 360WC T I L ) (4)
tl
B = +
Pz(Tz +
t z ) - 3600(C TzL)
(5)
tz
Note. tl must be different from t ~ .
By simultaneously solving Equations
In one test on a 1-inch column, the
leakage through the valve determined
under total reflux was 0.71 ml. per
hour or 0.0002 ml. per second. The dis-
tillates collected were 166.5 ml. per hour
a t a timer setting of TI = 20 seconds
and tl = 2 seconds, and 120.4 ml. per
hour a t Tz= 40 seconds, t z = 3 seconds.
On substituting these values in Equa-
tions 4 and 5 and solving simultane-
ously, the value for C was 0.18 nil., and
the boil-up rate was 1500 ml. per hour.
The boil-up rate determined from the
heat removed by the cooling water flow-
ing through the reflux condenser was
1430 ml. per hour. Considering the
loss of some heat due to imperfect
insulation, these results agree well.
Without this correction, the boil-up
rates calculated by employing the ap-
parent reflux ratio determined by the
timer settings are 1832 ml. per hour for
the first setting and 1726 for the second
setting.
K i t h the type of control described,
the reflux ratio determined by the
ratio of the reflux time and discharge
time can deviate considerably from the
actual value. By the procedures de-
scribed, accurate reflux ratios can be
easily determined and controlled.
VOL. 31, NO. 6, JUNE 1959 1121