PETROLEUM REFINING EQUIPMENT

BASIC FRACTIONATION PARAMETERS IN R E D I S T I L L A T I O N

OF N A P H T H A IN M O D E L UNIT

N. N. B u s h u e v a , L. N. M o t u s , UDC 542.48 : 66.048

a n d A. I. S k o b l o

For a solution of problems involved in the design, operation, control, and optimization of the operation of frac-
tionating towers, data must be available on the interrelations among the basic parameters of fractionation: the sharp-
ness of separation, the reflux ratio (and vapor ratio), and the number of trays. These data can be obtained either by
calculation or by experiment. Considering that the existing methods for calculating fractionating towers (particu-
larly for the separation of multicomponent mixtures) are based on a number of simplifying assumptions, the most re-
liable method for obtaining such relationships consists of obtaining experimental data. The possibilities for experi-
mentation with commercial fractionating towers are limited, so that it is of interest to build continuous laboratory
fractionating columns that model the operation of the corresponding commercial equipment.

This article is devoted to the experimental investigation of the basic parameters of fractionation in applica-
tion to the process of naphtha redistillation to obtain feedstock for cataIytic reforming. The characteristic feature
of the naphtha redistillation process in these cases is the increased requirements for sharpness of separation, as a c c o m -
plished by the use of fractionating towers with a comparatively large number of trays, high reflux ratios, and corre-
spondingly large consumptions of energy.

The experimental studies of the basic fractionation parameters were conducted in a continuous model-unit con-
sisting of an electric heating furnace, a packed-glass fractionating column with a rectifying section and a stripping
section, a surface condenser for the overhead product vapors, an electrically heated reboiler for vaporization of the
bottom product, a piston-type feed pump, and instrumentation. Adiabatic column operation was maintained by regu-
lation (with laboratory autotransformers) of the electric heaters in the air jackets of the column.
The fractionating column was 1 m in height and 20 mm in diameter. The packing consisted of Nichrome
helices with an inside diameter of 1 mm. The number of equivalent theoretical plates in the column was adjusted
by changing the height of the bed of packing. The equivalent number of theoretical plates for the packing was de-
termined experimentally by the usual procedure, using artificial mixtures of two to five individual hydrocarbons.

In order to maintain a constant hydrodynamic regime of column operation, the amount of reflux returned to
the column from the condenser was metered and held constant. The reflux ratio was varied by changing the load on
the column.
In all experiments, the temperature of the feed entering the column was maintained constant at 115~ which
corresponded to liquid-phase feed, heated to approximately the initial flash vaporization temperature. For vaporiza-
tion of the bottoms, the supply of heat to the lower part of the column (analogous to the operation of a number of
commercial columns) was regulated by stabilization of the liquid level in the still pot.
The distillation curves of the feed, distillate, and residue were determined in accordance with GOST 2177-66
[similar to ASTM distillation] and by close fractionation to obtain TBP curves.
In parallel experiments that were set up to differ specifically in distillate takeoff (mass ~o), reflux ratio, and
number of plates, it was shown that the unit gives good stability of the regimes and good repeatability of the condi-
tions of the experiment.

I. M. Gubkin Moscow Institute of the Petrochemical and Gas Industry (MINKh i GP ira. Gubkina). Translated
from Khimiya i Tekhnologiya Topliv i Masel, No. 5, pp. 38-41, May, 1974.

@1975 Consultants Bureau, a division of Plenum Publishing Corporation, 227 West 17th Street, New York, N. Y. 10011. No part
of this publication may be reproduced, stored in a retrieval system, or transmitted, in any form or by any means, electronic, me-
chanical, photocopying, microfilming, recording or otherwise, without written permission of the publisher. A copy of this article
is available from the publisher for $15.00.

384
TABLE 1. Comparison of Indices for Fractionating Capability of Commercial and Laboratory Columns for Naphtha
Redistillation
Difference -
Operating Distillation curve between
indices of (GOST 2177-66), product dis-
~ illation tern )s.
column tCOST 2177.
Column Products from column 66), ~C
O~
o
ul =~,
So ' ~s
m,

Laboratory 44,0 ,69 2,10 Distillate (IBP-105"C cut) 43 78 I01 112

Residue (105-180~ cut) 123 142 166 [190 11 30
Commercial K-3 44,3 ,64 2,03 Distillate (IBP-105~ cut) 48 72 93 ]103
114 135 161 180 11 29
Residue (105-180~ cut)
Laboratory 31,4 ,20 1,92 Distillate (IBP-62~ cut) 31 45 57 [ 63,5
78 87 96 126 1160 14,5 30
Residue (62-105~ cut)
Commercial K-4 31,2 ,24 2,60 Distillate (IBP-62 ~ cut) 26 32 40 54 I 62
78 86 98 129 1150 16 32
Residue (62-105 C cut)
Laboratory 43,7 ,85 2,21 Distiilate (IBP-105-140~ cut) 96 121 132 51142
146 152 l 157 173, [190 4 19,5,
Residue (140-180~ cut)
Commercial K-5 44,6 ,87 1,85 Distillate (IBP-105-140~ cut) 104 107] 114 123 1136 4 21
Residue (140-180~ cut) 140 1441 152 167 [182

TABLE 2. Influence of Reflux Ratio (vapor ratio) on Sharp-

ness of Separation of Naphtha Fractions (21 theoretical
plates in column)
Distillation temperature. ~
distillate * i residue *

90% 95% 98% IBP [ 5% lo%

14,6 1,780 94,2 96,0 98,0/126,7131,0132,1

I
12,0 1,480 95,0198,0100,0125,5130,8131,9
10 9,5 1 1,200 101,0, 104,0108,0]126,5[131,0132,1
7,3 ] 0,884 104,5] 108,0 112,0,116,0,122,0125,5
6,0
/~ 8~119,0'122,0 127,01119,51126,5129,0

I
6,70 3,34 111,5 1 114,5 118,0 133,01138,0 139,5
4,30 2,24 110,5] I14,5 ll8,0 128,0/136,0]137,0
2,76 1,67 119,0 / 125,01129,01120,01131,01133,0
30 2,30 1,49 125,0 / 130,01135,01115,01125,01127,0
1,84 1,23 135,0 / 140,0 [ 146,0] 109,0[119, O[120,0
1,56 1,08 138,8 / 143,8/149,3/107,01116,01119,0

2,95 5,88 125,0129,51133,5144,01147,5t148,2

1,90 4,36 t24,5 131,0 138,5140,0t143,01144,5
60 1,18 3,27 139,0145,0136,01141,01142,0
1,00 3,00 136131'5,5 143,2149,0131,0t136,01137,0

*Product distillation by GOST 2177-66 method.

In order to determine how well the fractionating capability of the laboratory unit matched up with that of com-
merical towers, tests were run on a naphtha with a distillation curve of IBP 50~ 10% at 74~ 50% at 115~ 90% at
154~ and EP 176~ In these tests, the primary regime indices of the laboratory column, i.e., distillate takeoff
(mass %) and reflux ratio, were set to be identical with those of three commercial towers in the redistillation block,
a combination ~LOU-AVT- 6-VP unit [electric desalting/atmospheric-vacuum pipestill/redistillationunit]. Detailed
characteristics of these commercial towers were given in [1]. Comparative data are presented in Table 1. In these experi-
ments, the separating capability of the laboratory column corresponded to 30 theoretical plates; in the commercial
towers, the number of shower-type valve trays was 30 for K-3 and 60 each for K-4 and K-5. Analysis of the data of

385
 8~
80
25
ZO
15
3 g

"I0
",5
"gO
-g5
Fig. 1. Sharpness of separation of naphtha frac-
tions as a function of reflux ratio. Distillate
takeoff (mass %): 1) 10; 2) 30; 3) 60.

,.'6

~ I~ ~

, ) , , I
~ -lO _ ~ I0 Z# 80 4,0
tIBPW- t88~, 00
-1,5

-85

Fig. 2. Interrelation between different indices of

separation sharpness for naphtha fractions. Exper-
i m e n t a l data from column operation: 9 l a b o r a -
tory; @) c o m m e r c i a l .

Table 1 shows that, for all three cases, the c o m m e r c i a l and laboratory columns were essentially identical in fraction-
ating capability, and this gives us a basis for assuming that it is indeed feasible to use a laboratory unit to model the
operation of c o m m e r c i a l fractionating towers in redistillation units. It should be noted that, for the K-4 and K-5 c o l -
umns, 60 valve trays were equivalent to 30 theoretical plates in the laboratory column. For the K-3 column, t h e r e a l
and theoretical numbers of plates were identical (30). The more efficient operation of the trays in the K-3 column
in comparison with K-4 and K-5, as noted in [1], is explained by the higher loading of the K-3, which is 130-150%
of the m a x i m u m design load, in comparison with 48-72% for K-4 and 94-113% for K-5.

The influence of reflux ratio on the sharpness of separation of naphtha fractions in the model unit is shown in
Fig. 1 and Table 2. Data on the distillation curves of the distillate and residue in Table 2 are presented in terms of
the most characteristic temperature points, i.e., the 90, 95, and 98~ points for the distillate, and the IBP, 5~ and
10% points for the residue, these points changing markedly when the regime parameters are changed and hence p r o -
viding a good evaluation of the sharpness of separation. These data allow us to follow the changes in distillate and
residue distillation curves and in the sharpness of separation, when the reflux ratio and vapor ratio are changed. For
example, with a distillate takeoff of 10 mass %, a reduction of reflux ratio from 14.6 to 6 is accompanied by an i n -

386
 TABLE 3. Influence of Number of Trays in Column on Sharp-
ness of Separation of Naphtha Fractions
Distillation temperature, *C
distillate 1" risidue
t o ~?
tn ~ ~

9o% 95% 98%I IBP 5% x0% INto

~.~.
I ~

10 21 6,001119,0 122,0 127 0 119 5 126,5 129,0 10,0

30 5,881112,01115,0 117,5 12015 128,0 130,0 18,0

40 21 2,52 1119,0 123,5 129,0 133,0 137,8 138,8 19,8

30 i2,55 [118,0 122,6 127,0 138,01141,8 142,8 25,8

21 1,90 124,5 131,0 138,5 140,0 143,0 144,5 20,0

30 2,00 127,0 131,5 136,5 147,01150,0 150,5 23,5
21 1,18 131,5 139,0t145,0 136,01141,0 142,0 10,5
60 30 1,20 131,5 137,9 144,0 140,51144,0 145,0 13,5
21 1,0 136,5 143,2 149,0 131,51136,0 137,0 --0,5
30 1,0 138,5 145,51151,5 136,5[140,3 144,2 2,7

, YO0~
o" /
n:::~-,,,'-~ 0
,.,._'-a 80~ "
OC o / 0 (9 0

o ooo -tA.

~.~ ~" 70t- -I10o =

0 ~,.-..~ ~ ^ |
~,o~,"~"" O U ~ I - ~ S I I~ I / 0 ~'~"
O 10 ZO d5 ~0 #0

Fig. 3. Concentrations of desired fraction in distillate (O)

and residue ((D) in relation to arbitrary index of sharpness
of fraetionation.

crease in the 90% point of the distillate from 94 to I19~ the 95% point from 96 to 122~ and the end point from
98 to 127~ as well as a lowering of the IBP of the residue from 127 to 120"C, the 5~ point from 131 to 126~ and
the 10% point from 139 to 129"C. Correspondingly, the sharpness of separation as judged by the quantity (h0w-t0D)
was changed from 38 to 10~ (see Fig. 1, curve 1).
The initial sections of the curves relating sharpness of separation to reflux ratio (see Fig. 1) have a compara-
tively steep rise, indicating that a small increase in reflux ratio will lead to a marked increase in sharpness of separa-
tion. Thus, these experimental data, when applied to a specific commercial distillation tower, provide an estimate
of the region of effective regulation of reflux ratio. It should be noted that, in order to ensure a given sharpness of
separation, the required reflux ratio will be higher when the distillate takeoff is smaller.
The sharpness of separation of the naphtha fractions can be estimated by the difference in GOST 2177-66 dis-
tillation points, using either the difference between the 10% point of the residue and the 90% point of the distillate
(see Fig. 1) or the difference between the initial and final boiling points of the column products tIBPW--%sD. The
experimental data shown in Fig. 2 characterize the interrelation between the indices of separation sharpness for the
model unit (37 data points) and the commercial towers (13 data points). The same sort of interrelation has been es-
tablished for the difference between the 5% point of the residue and the 95% point of the distillate (tsw-%sD). Thus,
these data indicate that any of these indices can be used in estimating the separating capability of distillation towers.
In view of the possibility of large errors in determining the initial and end points of petroleum products, and r_he rar-
ity of determining 5070and 95% points in commercial practice, preference should be given to the use of the index
(h0w-t0D), characterizing the gap between the 10% point of the residue and the 90% point of the distillate.

387
 In order to determine the influence of number of plates on the sharpness of separation of naphtha fractions, e x -
periments were performed in the column with 30 theoretical plates; these experiments were performed using the same
regime parameters (distillate takeoff and reflux ratio) as those used in the previous tests on the column with 21 theo-
r e t i c a l plates. Comparative data are presented in Table 3; it can be seen that increasing the number of theoretical
plates from 21 to 30 is accompanied by an increase in the sharpness of separation, the value of (qoW-tg0D) increasing
by amounts of 3 to 8"C.

The r e l a t i v e l y small slope of the final section of the G O S T 2177-66 distillation curve (difference between 98%
and 90% points) for the distillate obtained with 30 theoretical plates is another characteristic indicating better separa-
tion.

The increased sharpness of separation given by increasing the number of plates from 21 to 30 is c o m p a r a b l e to
that obtained by increasing the reflux ratio with a constant number of plates (21).

It can also be seen from Table 3 that the increase in sharpness of separation corresponds to an increase of reflux
ratio by 0.1-1.8, or by 10-727o.

The index adopted to characterize the fractionating c a p a b i l i t y (tl0 W-tg0D) is arbitrary, but it does agree (Fig. 3)
with the basic index of the sharpness of fractionation, the concentrations of desired fraction in the distillate and in the
residue, on the basis of TI3P curves.

LITERATURE CITED
1. A. I. Skoblo, N. N. Ipatenko, L. N. Moths, et al., Khim. Tekhnol. Topl, Masel, No. 4, 38-41 (1973).

388