ENGINEERING AND PROCESS DEVELOPMENT

Reflux and Plate Determinations

for Batch Distillation
S. R. M. ELLIS
Chemical Engineering Department, The University o f Birmingham, Birmingham 15, England

I ?rT ASSESSING the number of plates in a binary distillation it

is usual to calculate the minimum reflux ratio and minimum
number of plates by using the Underwood (19) and Fenske (11)
The object of this paper is to re-examine Gilliland’s method and
to see if it can be extended to batch distillation. If this is pos-
sible, the method would also be of value in locating the feed plate
equations, and to calculate the operating reflux ratio and number in continuous distillation.
of plates by using the graphical McCabe-Thiele (16) construction.
When the relative volatility is less than 1.25 and the number of Procedure Includes Correlating Curves Based
theoretical plates in the column is high, the graphical hIcCabe- on Underwood, Fenske, and Smoker Equations
Thiele construction is difficult to apply. I n such cases the num- The procedure was to consider the systems, benzene-toluene,
ber of plates can be accurately determined using the Smoker (17) benzene-n-heptane, phenol-o-cresol, and ideal mixtures where
and Dodge and Huffman ( 7 ) equations. The use of such equa- the relative volatilities of the binary components or key com-
tions is time consuming and requires a high degree of arithmetical ponents in multicomponent distillation are 1.1, 1.05, 1.025, 1.01,
accuracy. and for a number of separations in each system to calculate mini-
As a rapid and reasonably accurate method for the preliminary mum and operating reflux and plate requirements.
determination of the number of theoretical plates in a column, For benzene-toluene the equilibrium data of Griswold, Andres,
Brown and Martin ( a ) and Gilliland ( l a )have proposed empirical
and Klein (IS)were selected, whereas for the system benzene-n-
correlating equations involving the number of plates, the minimum
heptane equilibrium data of Ellis (10) were used.
number of plates, the reflux ratio, and the minimum reflux ratio.
Underwood’s (19) equation was used to calculate all minimum
These equations apply to continuous distillation. Brown and reflux ratios. Except for benzene-n-heptane, the Fenske (11)
Martin and Gilliland allow for different feed conditions. The equation was used to determine minimum plate requirementa
correlating curves, although drawn through a band of points, give
The minimum number of plates for benzene-wheptane was evalu-
reasonably accurate results for continuous distillation. However, ated graphically.
when applied to batch distillation these correlations give inac-
curate results.
Cichelli ( 4 ) and Zuideiweg (21 ) have proposed correlations for
batch distillation between minimum requirements, the plate num- Table I. Calculation of Reflux and Plate Requirements
ber, and reflux ratio, where the difficulty of separation is defined S-Sm R- Rm
by the “pole height.,’ I n batch distillation it is desirable, how-
5* xw (lav. S Sm s+ 1 R Rm R + 1

ever, to be able to calculate rapidly the reflux ratio a t any stage in Benzene-Toluene
the distillation. The need for such calculations is emphasized in 10.2 4.24 0.53 2.27 2.25 0.01
8.3 4.24 0.44 2.45 2.25 0.06
the application of Bogart’s ( I ) equation to the separation of high 5.9 4.24 0.24 3.58 2.25 0.29
5.4 4.24 0.18 4.58 2.25 0.42
purity components from close boiling mixtures. 4.9 4.24 0.12 5.58 2.25 0.57
8.4 6.28 0.22 13.6 10.2 0.23
7.55 6.28 0.15 18.0 10.2 0.41
6.85 6.28 0.07 35.5 10.2 0.69
10.33 6 . 2 8 0.36 10.8 10.2 0.05
9.1 8.1 0.07 48.0 25.5 0.46
Dlstillatc 0.9 8 . 9 0 9 9.5 8.1 0.13 36.6 25.5 0.29
10.5 8.1 0.21 27.0 25.5 0.05
Bottoms 0.02 0.05 0.3
Benzene- n-Heptane
10.7 9.4 6.5
10.3 9.4 0.08 44.0 16.6 0.61
12.3 9.4 0.22 21.5 16.6 0.22
lX8 9.4 0.30 18.6 16.6 0.10
10.9 9.4 0.13 30.0 16 6 0.43
12.3 10.7 0.12 64.3 43 0 0 32
11.6 10.7 0.07 97.0 43. I) 0.56
12.9 10.7 0.16 50.0 43.0 0.14
14.0 6.5 0.5 3.5 3.1 0.09’
8 2 6.5 0.18 8.0 3.1 0 54
9,6 6.5 0.29 5.0 3.1 0.32
11.2 6.5 0.38 4.2 3.1 0.21
7.8 6.5 0.15 10.0 3 1 0.63
Phenol-o-Cresol
0.96 0.30 1.238 23.2 18.8 0.18 47.0 13.1 0.50
0.96 0.30 1.238 25.4 18.8 0.25 23.0 13.1 0.41
0.96 0.30 1.238 34.9 18.8 0.44 15.0 13.1 0.11
0.96 0.10 1.238 36.4 25.1 0.30 47.0 40. 1 0.14
0.96 0.10 1.238 27.8 25.1 0.09 96.0 40.1 0.58
0.96 0.10 1.238 30.6 25.1 0.16 67.0 40.1 0.40
0.96 0.04 1.238 33.6 29.8 0.11 200.0 100.6 0.49
0.96 0.04 1.238 35.8 29.8 0.16 150.0 100.6 0.33
Figure 1. Extrapolation of Curves Calculated for 0.96 0.04 1.238 39.4 29.8 0.24 120.0 100.6 0.16
Benzene-n-Heptane

February 1954 INDUSTRIAL AND ENGINEERING CHEMISTRY 279

ENGINEERING AND PROCESS DEVELOPMENT

suspecting that the relative volatility would influence their

Table II. Calculation of Reflux and Plate Requirements correlations, found no e\Tidence for this effect,. Figure 2 shows
R - Rm s - Sm s - As?,
that when the intercept value, __- , is plotted against R,,, a
XU ZIP R Rm R + 1 S S7n Sfl S-tl
a = 1.1
series of curves are obtained, each of which is related to the
34 5 0 16 61.7 34.5 0 44
relat'ive volatility of the system. For relative volatilities less
0.90 0.25 $1.2
0.90 0.25 00.0 34 5 0 36 48.7 34.5 0 28 than 1.25, the slope of the linear plots of Figure 3 can be corrc-
0.90 0.25 80.0 34 5 0 56 42.6 34.5 0 18
0.90 0,2;2 37.5 34 5 0 078 71.5 34.5 0 51 lated by plotting against the relative vo1atilit)-.
0.90 0.50 19.0 15 8 0.16 48.2 23.0 0 51 Calculation of Reflux Ratio and Number of Plates. From
0.90 0.50 23.0 13 8 0 30 38.4 23.0 0 39
0.90 0.50 30.0 15 8 0 46 32.7 23.0 0 28 Tables I and 11, the resulting curves of the type illustrated in
0.90 0.10 100.0 88 8 0 11 73.0 46.1 0 36
0.90 0.10 120.0 88 8 0 26 62.8 46.1 0 26 Figure 1 have been grouped together into a family of curvcs, as
0.90 0.10 200.0 88 8 0 49 53.5 46.1 0 14 shown in Figure 4.
a = 1.05 I n the application of Figure 4, t'he first' step is to decide nhich
0.83 0.40 83.3 37.3 0.55 57.3 43.8 0 23 correlating curve is to be used for the calculation. From R,,, or
0.85
0.85
0.40
0.40
48.3
40 6
37.3
37.3
0.23
0.078
75.3
107.4
43.8
43.8
0
0
42
58 S , the extrapolated intercept,
s--
- s,
at zero value of
-
R -- R ,
0.96 0.06 500.0 378.9 0 24 169.8 120.6 0 23 SS.1' R i l
0.95 0.05 428,O 378.9 0.11 174.2 120 6 0 30
0.95 0.05 800.0 378.9 0.53 136.1 120.6 0 11 can be evaluated froin &her Figure 2 or 3. This intercept on
0.80 0.50 28 0 23.6 O,l5 63.9 28.4 0 35 Figure 4 gives the appropriate correlating curve and, if R,, and
0.80 0.50 36 8 23.6 0.35 47.0 28.4 0 39
0.80 0.50 50.0 23.6 0.52 38.5 28.4 0 27 S , are known, either R or S can be calculated. The application
0.80 0.10 175 0 155.3 0.11 127.2 73.4 0 42
0.80 0.10 200,o 155.3 0.22 110.8 73.4 0 34 of the above method can be illustrated by the three following es-
Q.80 0 10 230.0 155.3 0.32 100.4 73.4 0 27 amples.
0.80 0.10 315.0 155 3 0.50 88.6 73 4 0 17
a = 1.022
SEPARATIOS O F CHLOROBESZEKE AXD H R O l f O B . Young
(20) gives the relative volatility of chloro- and bromobenzrne as
, O . 80 0.50 56.0 47.6 0.13 128 0 56.3 0 5s
,O. 80 0.50 60.0 47.6 0 20 110.2 56.3 0 48 1.889. Consider a batch distillation in a 10-theoretical-plate
0.80 0.50 95.0 47.6 0.49 75.4 56.3 0 25 column, where it is desired to calculate the necessary reflux ratio
0.80 0.30 125.0 94.9 0.24 151.7 90.6 0 39
,O. 80 0.30 150.0 94.9 0.36 122.8 90.6 0 26 to give an overhead product containing 98.0% chlorobenzene arid
0.80 0.30 182.0 94.9 0.48 112.0 90.6 0 19
a bottoms product containing 11.'7yo of chlorobenxenc.
d = 1.01 The Underwood equation gives a R,, v:ilue of 9.4 and the Ii'enske
0.80 0 50 130 6 119 6 0.20 278 6 140 0 0 47 equation gives a S , value of 9.3. If the I?,, value of (3.1 is
0.80 0.50 180 0 119.6 0.33 219 3 140 0 0 36
0.80 0.50 230.0 119.6 0.47 189 5 110 0 0 26 taken, from Figure 2 by- interpolating betmen the curvefi, the
0.80 0.60 95.5 82.8 0.13 226 3 99 0 0 56
0.80 0 60 120 3 82.8 0.31 173 9 99 0 0 40 raluc of the intercept for 01 = 1.88!1 is 0.4'7. Prom the
0.80 0.60 170 0 82.8 0.51 132 3 99 0 0 23 ST1
correlating curve in Figure 4 correspontliiig t,o intercept value
0.4; and for
R - Ren s -t-s,,,18. 0.14. For
R + 1 = 0.52, the value of ___-
For benzene-toluene and benicne n-heptane, operating reflux S,,= 9.3 this gives a reflux ratio of 20.5, Edge\~orth-Johnslonc
and plate requirements n ere determined froin graphical 3Ic- ( 8 ) ,using a XcCai,e-Thiclc coristruct,ion, calculated a reflux ratio
Cabe-Thiele constructions. In all other cases calculations n ere of 20.0. A comparison is made in Table I11 of the reflux ratios
made using the Smoker equation calculated by li:tlgcir-orth-Johnstone (8).using a i\IcC~"ahc-Thiele
Calculations a l e eunimari/cci in Tnblcs I and 11.

1.0
Correlations Provide Rapid and Accurate
Calculation of Reflux and Plate Requirements
I
The results for the benzene-n-heptane system (Table I ) have
been expressed graphically in Figure 1. For benzcue-n-heptane
separate curves are obtained for varyiii.s tlrgrtw of separation.
Similar graphs (riot shown) for the other tahles result in curves
having a sixiilar trend.
R - Xnz
For values of ___- less than 0.05 the cu
s - s,, value of+unity
I I2 - R,,, approaches zero. 13y es- I I I I I
an
S+1
as
R + l
s - s, are obtained
0 20 40
- R, - 60 80

trapolation of the curves, intercept values of -

Si-1 Figure 2 . Correlation with Minimum Reflux Ratio
which can be correlated by plotting against t h e
ratio of the volatile conmonent in the overheads
and bottoms, or against the minimum reflux
ratio, R,,,, or the minimum number of plates,
S,n. The use of these extrapolated curves
does limit the correlation to those values of
R greatei than 1.05 E,. Such correlations are
shon-n in I'iyuies 2 and 3. When the relatire
volatility is greater than 1.25 the correlation of
the s
s -' Sm
inteicept n-ith R,, is probably the
7-1
most convenient. If the relative volatility is
less than 1.25, the linear correlation mith S, is - sm'
the most valuable.
Gilliland ( I d ) and Zuiderneg ( Z l ) , although Figure 3. Correlation with Minimum Number of Theoretical Plates

280 INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 46,No. 2

 ENGINEERING AND PROCESS DEVELOPMENT

07.5 1 I I I These examples show that this graphical method for calculating
the reflux ratio or the number of plates approaches the accuracy
of the Smoker and Dodge and Huffman equations. Although the
correlating curves are based on the Underwood, Fenske, and
Smoker equations, the method might not have been expected to
give such accurate results in view of the ease with which it may
be applied. The method can be equally well applied to the sep-
aration of key components in an ideal multicomponent mixture
\\\ i I
I I if the correct minimum reflux ratio is used.
Continuous Distillation and Feed Plate Location. To deter-
mine the total number of plates in the distillation column for
a given reflux ratio, it is necessary to use the correlating curves
of Gilliland ( l a ) or Brown and Martin ( 8 ) .
If the total number of plates is known, numerous methods have
I ” ’ 1 # 1 1 1 1
-1
been proposed for locating the feed plate-Le., hlcCabe-Thiele
construction, plate-to-plate analysis, the Smoker equation, and
0 025 0.5 075
the empirical correlation of Kirkbride (14).
It was considered feasible that Figure 4 should be applicable to
s - sm the location of the number of trays above the feed plate. The
Figure 4. Correlation of ____ Intercept with Reflux feed composition entering the column a t ita boiling point is con-
S+ 1 sidered to be the equivalent of a composition in a reboiler in a
and Plate Requirements
batch distillation. This is probably best illustrated by the follow-
ing examples.
SEPARATION OF BENZSNE AND TOLUEXE. Consider a continu-
method, those calculated by Gilliland’s correlation, and by the ous still fractionating a mixture of 40.0y0 benzene and 60.0y0
method proposed in this paper. toluene a t a reflux ratio of 3 to 1, so that each product is 99.0%
Gilliland’s correlation does not apply to batch distillation. pure. The Smoker and RlcCabe-Thiele methods give 7.9 plates
This is not a criticism of the method, since it was developed for above the feed plate. The total number of theoretical plates is
continuous distillation. 15.7.
The relative volatility a t the feed point is 2.45 and the average
value between the feed and overhead compositions is 2.40, R , =
1.65, and S , = 5.6.
Table 111. Comparison of Methods of Calculating Reflux From Figure 2 the
s - s,
intercept is taken as 0.52 and from
Si-1
Ratio R - R,
Figure 4, with -___ as0.34, -
s
-+8, = 0.25. S , the number of
R +

Distillate Bottoms a MoCabe-Thielea Ellis Gilliland

plates above the feed, is 7.8, which is in close agreement with the
0 98 0.26 1 889 7 0 7.0 8.1 above result.
0 98 0 175 1 889 12 0 12 0 19 0
0 98 0 117 1 889 20 0 20 5 31.0 SEPARATION OF 0-, m- and p-MONONITROTOLUENE. In the
a Edgeworth-Johnstone ( 8 ) . srparation of this ternary mixture, Coulson and Warner (6) have
shown by plate-to-plate analysis that a reflux ratio of 5 to 1 re-
quires 21 theoretical plates for the specified overhead and bot-
toms compositions. The number of plates above the feed is 11.0.
For the key components, 0- and p-nitrotoluene, the relative vola-
I O OXYGEV
S C P ~ R ~ T OF N ISOTOPES. For the separation of oxy- tility is 1.7, R, = 2.23, and S , between the feed plate and over-
gen isotopes, Dodge and Huffman ( 7 ) give a relative volatility of
01 = 1.006. For a distillate composition of 2.54%, a bottoms head compositions is 7.9. From Figure 2 the ; ‘ ;%
-___ intercept is
product of 0.20%, and a reflus ratio of 3920, Dodge and Huffmaq 0.58, which locates the appropriate curve on Figure 4. From
(1)and Smoker ( I ? ) calculated the number of theoretical trays as R - R, S - S,
Figure 4 for = 0.46, ~- + = 0.22, such that S = 10.5.
521. If R, is taken as 1960 and S, is taken as 430, then from
~

R + l
Figure 3, by interpolation and extrapolation, the intercept value Multicomponent Systems. I n continuous multicomponent
distillation the presence of other components influences the
- Sm is 0.58. Csing the appropriate curve of Figure 4,for
of ___
R
S + l
_ _R_
-
R +1
m -
- 0.5> ___ ’s + 1
- sm has a value of 0.19. The number of
separation of the key components and the evaluation of their
minimum reflux ratio. Figures 3 and 4 can be rapidly applied
to the location of the feed plate with a reasonable degree of
plates obtained by this procedure is 529, which is in close agree- accuracy if the following procedure is adopted:
ment with the above calculated result.
SEPI R ~ T I O N OF ~L-HEPTAKE AND ~IETHYLCYCLOHEXANE. In 1. R, is determined using the equation of Underwood (18)
the separation of n-heptane and methylcpclohexane (with a rel- between the overhead composition and the composition of the
ative volatility of 1.07) to give an overhead and bottoms product liquid fraction of the feed. The Colburn (6) equation can be
of 06.0 and 3.33%, respectively, and using a reflux ratio of 1000, similarly used for evaluating R,.
2. For a liquid feed, S, is determined between the ratio of key
Dodge and Huffinan ( 7 ) calculated that 105 theoretical plates components in the overhead composition and the ratio in the feed
were required. Since R,, = 415 and S, = 97.0, for S, = 97.0 and by using the Fenske (11) equation. I n the case of flash vaporiea-
a: = 1.07 from Figure 3 the intercept value of -
S -+S, is 0.35. tion of the feed, S, is determined between the ratio of key com-
ponents in the overhead composition and the ratio in the liquid
R - Rm fraction of the feed.
This locates the cun’e on Figure 4, and from
R f l
-
= 0.59 the 3. For a liquid feed, S = n 1 and S,, n, +
1 are equal
to the theoretical and minimum number of theoretical trays above
+ +
value of is 0.09. This gives the number of plates as the feed plate. I n the application of Figures 3 and 4 to feed plate
S + l location the assumption is made that the ratio of key components
105.6, which again is in good agreement with the calculation of in the feed entering the feed tray is the same as that in the liquid
Dodge and Huffman. leaving the tray above the feed plate.

February 1954 I N D U S T R I A L A N D E N G I N E E R I N G CHEMISTRY 281

ENGINEERING AND PROCESS DEVELOPMENT

propriate curve is iocltteci in

Table IV. Calculations for Continuous Multicomponent Systems terms of the minimum reflux
Stages abol e 01'mininirim number of plates
__ Feed Plate and the relative volatility oi
~~~~~~l~ ~ ~N ~ t. ~Above
l Feed Plate plate Ihwres the system. Tho correlatioii
No. of Stages R RTn S,& andlysi- 3 and 4 Iteieience can aim he applied to the
1 8.8 9.0 2.0 5.G 6.0 6.2 Brown and Soudera ( 3 ) ,column 2 . locatiori -if the feed plarc ill
T ~ W 7, p. 1 . ~ ~ 8
2 17.0 3.0 1.35 6.5 6.0 6.1 Brown and Rouders ( 3 ) , coliinin 5 , continuouu dist'illatioit .
Table 7 , p. 1568
3 16.0 1.6 0.93 3.3 6.0 6.2 ICdinister (G), exaniple 27 !flash The method is of particular
vaporization of feed)
4 11.0 2.0 0.9 2.3 3.0 3.1 Robinson and Gilliland ( 1 5 ) ,p. 261 value in the separation ot
5 26.0 10.0 B.1 9.5 13.0 13.6 Robinson and Billiland ( 2 6 ' ) , p. 237 clofie h o i l i n g c ornpo 1 i ~ ' iti8 I
6 29.8 32.3 .>.S 22.0 24.2n 23.2 Brown and Martin (11.n. 696.
CaSP Id since it C D I ~be rapidly ripplied
a By absorption factor method.
with an uecuracy of the orciuv
of the Hnioker equation

4. \Vith flash vaporization of the feed the number of theo- Nomenclature

retical trays and nlinimum number of theoretical trays above
the feed plate are taken to be n and ntrL. The ratio of key com- :ELI, ZIT = distillate and still composition
ponents in the liquid fraction of the feed is assumed t o be the 01 = rt:liitive volatili1,y
composition of the liqcid leaving the feed plate. 12 = number of t,heoret,icwl phtel; in column
5. If the optimum ratio of key components o n the feed plate n,,, = minimum number of theoretical plates in colurriri
is calculated, then, as in step 4,n and nmare the number of theo- s = n + 1
retical and minimum number of theoretical trays above the feed SV,
R
= n,,,+ I
reflux ratio = O / l >
plate, The results given in T:rl,lP T V indicate the accur,ic.y of =
the method. R,,, = minimum reflux ratio
The calculatioii for e.wmple 3 in Table I V is given a s follows: Literature Cited
Minimum number of trays abovc the feed plate:
(1) I3ogar.r, M . J . P., Tmns. ,in,. rt7sl. (,'hem, Engrs., 33, 139 (193;]~
( 2 ) Brown. C. G., a n d X n r t i n , TI. Z.,
Ibi'd., 35, 579 (1939).
( 3 ) 13r.ou-n, C. G., a n d Houders, 31.. "Science of Petroleum," 1.01~
9Zm +2 = 5.3
2, p. 1544, London, Oxford U n i ~ e m i t yPress, 1938.

111this instance, with flash vaporization ot the feed snd p:titiaI

condensation, the minimum number of t l a n above the ircd plittr
is 3.3. In the application of Figures 3 and 1,S,, = 3.3 London. 1949,
From Figwe 3 for S, 3.3 and CY = 2.35, (7) Dodge, B. F.,nnd Iluft'nixn, ,J. It., Is[).I~NI:.CHRM.,29, 14:%
(1937).
(8) Edgeirorth-Johiistonc, R., Ibid., 3 6 , 1068 (1944).
(9) Edmistor, W.C., P e i d e t ~ nEng?.,
~ 19, 74 (June 1948).
(10) &Xis, Y. I?. AI., T~uras.I n a l . (,'hem. Rngr.c, ( L o n d o n ) , 30, ,jri
For R = 1.5 and R , = 0.95, then, from Figure 4.
1. R., IND. I h c . C(H€:?,I., 24, 482 (19;32)~
E. Ti.,Ibid.. 32, 1220 (1940).
J., Andres, D., and Klein, V , A, Trans, .1m. I N S [ .
Chena. Erzgrs., 37, 228 (1943).
(11) Kirkhiide, C . G., Petiok:um, Refi7?w,23,
(15) MrCahe, W.I,..and Thiele, E . W., I,
(1925).
Thus the number of plates above the feed tray is 6.2. (16) Robinson, C. S., a n d Gilliland, E. I<.. "Elements of E'mctiond
It would appear that the main advantage for this method of Distillation," 4th o d . . Yew Yoi k, IIcGraw-Hill Book Co.,
1950.
feed plate lowtion is the rapidity with which it can be applied in (17) Smolcer, E. H., Tram. A m . I l l & C'herri. Enurs., 34, 165 (10:3X).
the preliminary iissessment of ti problem. (18) Underwood, -4. 6. T'., C ng. Pmgr.. 44, 603 (1948).
(19) Underwood, A. ,J. V., . I n s f . Chsm. Bngrs. (London). 10,
131 (1932).
Summary (20) Y o u n g , S., T r a m . Chrwt. Soc., 81, 7G8 (1902).
(21) Zuiderwog, F. J., Chem. EUQ.S e i . , 1 , 8 (1951)*
Gillilaud's empirical reflux a i d plate correlation has been ex-
tended to batch distillation by using a family of curves. The ap- Rr:caivmu for review Mar011 20, 1853. ACCFPTED
October 43, 1 ! ) 3 3 ~

END OF ENGINEERING A N D PROCESS DEVELOPMENT SECTION

282 INDUSTRIAL AND ENGINEERING CHEMISTRY Vol. 46,No. 2