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Evaluation of flooding in a batch distillation column

Silvia Maria C.Silva1, Elioni M.A. Nicolaiewsky1, Cristina L. C. Costa1, Letcia Maria C. Santos1.
1

Escola de Qumica Universidade Federal do Rio de Janeiro

Abstract. Jet flooding originated from high vapor rates forms a liquid seal at the top of the column, affecting equipment
separation efficiency due to poor product quantity and purity. That liquid seal prevents higher quantities of vapor to reach the
condenser, thus reducing reflux and affecting the whole column operation. The aim of the present work is to evaluate the
relation between the vaporization rate and the height of the liquid seal formed (severe entrainment) at the top of a batch
distillation column, operating at atmospheric pressure. The laboratory scale glass distillation column has been used in the
undergraduate course of Chemical Engineering at Escola de Qumica/UFRJ and is fully controlled, regarding temperature and
heating requirements. It has 10 plates, having nominal diameter of 40 mm, with 1 bubble-cap each, and a tray spacing of 60
mm. Reflux and distillate rates are set up by a digital control system connected to a solenoid valve. The vapor rate is a
function of the heat added to the system, from a heating mantle. The column digital control system shows on its screen the
percentage of the heating power used (maximum 1.2 kW). The systems investigated are aqueous solutions of commercial
interest. The mixtures will be analyzed using a refractometer. The estimation of column efficiency was achieved only for the
methyl alcohol solution; the other alcoholic mixtures form azeotrope, so product purity as a function of flooding could not be
observed. It was also established the maximum vaporization rate in which jet flooding would be avoided, for each system
investigated, operating the column at total reflux.
Key words: flooding, batch distillation, heating power

1. Introduction
The present work is an attempt to measure flooding and to establish procedures on how to prevent it, in a
batch laboratory scale distillation column. The column was produced by QVF, a De Dietrich Inc. subsidiary,
located in Mainz, Germany, and has been used for Chemical Engineering undergraduate lab courses. The
laboratory column is made of glass, which enables a good perception on column hydraulics. One of the main
reasons for pursuing on this work was our little ability, during the lab under graduation classes, to control the
reboiler-heating rate in order to avoid flooding in that column. As the column heating requirements can be
controlled and is supplied by a very robust heating mantle, having maximum power of 1.2 kW, the heating
power was varied in order to establish the relationship between the mixture vaporization rate and the occurrence
of flooding. Another reason is that studies on small scale batch columns are rare in the literature, especially the
ones dealing with entrainment and flooding occurrence.
In order to run the tests on the batch column, it was chosen mixtures containing alcohol due to their
commercial importance. On the laboratory classes, ethyl alcohol is used, however, there was an attempt to
establish batch column performance, when working with different boiling point solutions. To accomplish that
task, several runs were performed in the batch column, using different aqueous solutions, relating height of the
liquid seal to the physical-chemical parameters of the solutions and to the heat added to the system. It has been
verified that flooding has not occurred whenever a high boiling point solution or very low heating powers were
tested.
1.1 Previous work
Flooding is defined by Kister (1990) as excessive accumulation of liquid inside the column, caused by one of
the following mechanisms:

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a)

spray entrainment flooding, which happens at low liquid flow rates, with trays operating in the spray
regime, where most of the liquid on the tray is in the form of liquid drops. As vapor velocity increases,
the bulk of these drops are entrained into the tray above. Thus, the liquid accumulates on the tray above
instead of flowing down to the tray below;

b)

froth entrainment flooding, which is characteristic of higher liquid flow rates, with the dispersion on
the tray in the form of froth. When vapor velocity is raised, froth height increases, approaching the tray
above, if the tray spacing is small. When tray spacing is over 24 in, the froth envelope seldom
approaches the tray above. So, if vapor velocity is raised, some of the froth inverts into spray and
flooding will take place by the spray entrainment mechanism;

The other two mechanisms, cited by Kister (1990), are caused by downcomer malfunctions, which are not
our concern here, for they happen mainly at high liquid flow rates and large diameter columns.
Flooding on a bubble-cap tray may be brought on by either excessive entrainement or liquid backup in the
downcomer (Bolles in Buford Smith, 1963). The true point of flooding is difficult to determine experimentally
and maximum capacity is usually synonymous with an incipient flooding condition. Regardless of cause, the
onset of flooding is detected by (1) a sharp increase in pressure drop and (2) a sharp decline in efficiency.
Other factors affect flooding in industrial columns: pressure, L/V relation and design parameters. When
dealing with a ND 40 glass distillation column, having one bubble-cap per tray, the factors affecting entrainment
flooding are very hard to figure out. Therefore, our concern in this work will be the evaluation of the influence of
vapor velocity, which is highly affected by the reboiler duty, on flooding. As spray entrainment flooding is far
more common, only that type will be discussed here.
1.2 Flooding prediction
Most entrainment flooding prediction methods available in the literature use the concept introduced by
Souders and Brown (1934), who analyzed entrainment flooding in terms of droplet settling velocity. Thus,
flooding occurs when the upward vapor velocity is high enough to suspend a liquid droplet, giving

u S , flood = c SB

L V
V

(1)

where cSB is the Souders and Brown constant at the flood point. Most correlations nowadays still use the
parameter cSB, but not it constant. Instead, they express cSB as a function of several variables such as: tray
spacing, liquid load, and fractional hole area and hole diameter.
Fair and Matthews (1958) developed a generalized correlation of flooding in bubble-cap trays by means of
liquid-vapor flow and vapor capacity parameters. The liquid-vapor flow parameter is defined as

Flv =

w
W

v
l

(2)

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Fairs correlation has been the standard of the industry for entrainment flood prediction and was recommended
by most designers. On Fairs correlation cSB is a function of the flow parameter (Flv), tray spacing, surface
tension and fractional hole area.

(3)

The flooding vapor velocity is calculated from

u N , flood = c SB
20

0.2

L V
V

(4)

Fairs correlation applies to nonfoaming or low-foaming systems. To be applied for bubble-cap trays, the
fractional hole areas used on the correction term are the ratio of the slot area to bubbling area.
When Fairs correlation was developed, little was known about the difference between spray and froth
entrainment flooding. Kister (1990) compared predictions from Fairs correlation to a much wider data bank
available at present and concluded that the correlation predicted most of these data well, but on a conservative
side.
Kister and Haas (1990) have developed a recent correlation for entrainment flooding

d 2
c SB = 0.144 H
L

0.125

0.1

S

hct

0.5

(5)

where
dH is the hydraulic diameter
S is the tray spacing
hct is the clear liquid height at the transition from froth to spray regime

- surface tension
G vapor density
L liquid density
For surface tensions greater than 25 dyne/cm, the authors recommend using that value. Both cSB and uflood are
calculated based on the net area, which in terms of bubble-cap plates is defined as the column area subtracted of
the area occupied by one downcomer.

2 The batch distillation column

The laboratory scale glass distillation column has been used in the undergraduate course of Chemical
Engineering at Escola de Qumica/UFRJ and is fully controlled, regarding temperature and heating requirements
(Figure 1). It has 10 plates, with one bubble-cap each, having nominal diameter of 40 mm and 60 mm tray
spacing. Liquid samples can be withdrawn from every tray, making it possible to undergo point efficiency
experiments. On Figure 2, there is a simplified drawing of the batch distillation unit.

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A digital control device, connected to a solenoid valve, sets up reflux and distillate rates. The reboiler is a 6
liter vessel, sitting on a heating mantle. The vapor rate is a function of the heat added to the system. The
maximum heating power is 1.2 kW and the percentage of the heat added to the vessel can be set up and is shown
on the screen of the digital control system. The column heating control system works with on-off mode and the
maximum temperature of the mantle is 213 oC. When that temperature is reached, the mtle heating control goes
off. After some time, when the still temperature is reduced to 194 oC, the heating system starts again
automatically.

Fig. 1. Picture of the batch distillation

column

Fig. 2. Schematic drawing of the column with

thermo couples

2.1 Test Procedure

The systems investigated were alcoholic solutions of commercial interest, such as ethyl, methyl and isopropyl
alcohol solutions. Those solutions have been prepared, with a concentration of 15% weight. The reagents were
high purity grade and have been purchased from VETEC (the former two) and THEDIA. The water used to
prepare the aqueous solutions was bi-distilled.
The test runs were initiated with a 3 liter-solution in the still. Using the selected heating power, varying from
25 to a 100% of the maximum (1.2 kW), the time for the mixture to reach the boiling temperature has also
varied, as expected. The mixture was distilled, on total reflux mode, until the temperature profile throughout the
column remained constant. With some mixtures, flooding would occur, especially with higher heating power.

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The solution of isopropyl alcohol, however, has not suffered flooding, on any of the heating levels tested.
Whenever flooding had occurred, the height of the liquid seal was then measured with a ruler.
During the test runs, at total reflux, after the temperature profile had reached constant values, the
vaporization rate was estimated by collecting the condensate formed in one minute-period of time. After
measuring the vaporization rate, the heating mantle was turned off and the system would remain at rest so the
temperature would decrease and another test run could start, with a different set up concerning the heating
power.

3. Results
The distillation unit software (Readwin 2000) gives the temperature profiles along the column of all the test
runs. Those plots are presented on Figures 3, 4 and 5 respectively for methyl, ethyl and isopropyl alcohol
solutions. The plates are numbered from bottom to top of the column. As the energy added to the system
increases (25, 50, 75 and 100% of the maximum heating power) the time for the mixture to reach the boiling
point decreases, ranging from 100 to 15 minutes.
In Table 1, it is presented the height of liquid seal formed and the vaporization rate, as a function of the
energy added to the system, by the heating mantle. As already mentioned, on the distillation of isopropyl alcohol
flooding has not occurred. However, its vaporization rate varied, as with the other solutions, that is, increasing
with the heat added to the system, as shown on Figure 6.
Table 1. Experimental data
Methyl alcohol
600 900 1200

Isopropyl alcohol
300 600 900 1200

300

Height of liquid (cm)

11.0

9.0

8.0

10.0

11.0

9.0

Vaporization rate
(ml/min)
Top temperature (0C)

4.1

6.0

9.3

10.7

3.5

7.6

13.0

16.0

2.6

7.1

10.8

11.0

64.8

68.8

70.2

71.2

78.2 78.2

78.2

78.2

80.0 80.0

80.0

80.0

100.0 90.0

84.0

82.5

88.9 88.9

88.9

88.9

68

68

Distillate
(%mol)

300

Ethyl alcohol
600 900 1200

Heating Power (kW)

68

68

In Table 1, it is also shown the peculiar behavior of methanol solution. The top tempearature is that of the
vapor (dew point) before going to the condenser. When low energy is added, the vaporization is slow and mass
transfer in each plate tends to be ideal, as pure methanol is obtained at the top of the column, when the lowest
heat had been added to the system and no flooding had occurred. However, when the energy added increases, as
flooding occurs, the distillates purity decreases, as shown in Figure 7. This behavior is a measure of the loss in
efficiency caused by flooding occurrence. With the other solutions, that behavior was not observed due to the
presence of the azeotrope mixture. In addition, the azeotrope mixtures of both solutions were easily reached,
since thery were observed at the 7th or 8th plates, not needing the whole column.

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Methyl Alcohol
Heating Power 300 KW

Heating Power 600KW

180

Tirs2S[3]
Tirc1

240

Tir8

160

Tir7

120

160

Tir6

120

Tir4

Temperature, C

Temperature, C

200

140

100
80
60
40

Tir5
Tir3

80
40

20
0

20

40

60

80

100

120

10

20

Time, min

Heating Power 900 KW

40

50

Heating Power 1200 KW

220

260
220

Temperature, C

180

Temperature, C

30

Time, min

140

100

60

180
140
100
60

20

10

20

30

20

40

12

Time, min

16

20

24

28

Time, min

Fig. 3. Temperature profile of methyl alcohol solutions.

Ethyl Alcohol
Heating Power 300 KW

Heating Power 600 KW

180

Tirs1
Tirc2
Tir8
Tir7
Tir6

240

160
200

Temperature, C

120

Temperature, C

140

100
80
60
40

160

Tir5
Tir4
Tir3

120
80
40

20
0

20

40

60

80

100

120

140

20

40

Time, min

80

Heating Power 1200 KW

240

200

200

Temperature, C

160

Temperature, C

Heating Power 900 KW

240

120
80
40
0

60

Time, min

160
120
80
40

10

20

30

40

50

60

20

Time, min

40

60

80

Time, min

Fig.4. Temperature profile of ethyl solutions.

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Isopropyl Alcohol
Heatig Power 300 KW

Heating Power 600 KW

180

240

Tirs1

160
200

Tirc2

160

Tir7

Tir8

Temperature, C

120

Temperature, C

140

100
80
60
40

Tir6

120

Tir5
Tir4
Tir3

80
40

20
0

20

40

60

80

100

120

140

20

40

Time, min

80

Heating Power 1200 KW

260

200

220

Temperature, C

160

Temperature, C

Heating Power 900 KW

240

120
80
40
0

60

Time, min

180
140
100
60

12

16

20

20

Time, min

12

16

20

24

28

Time, min

Fig.5. Temperature profile of isopropyl alcohol solutions.

18
16

Vaporization rate, ml/min

14
12
10
8
6
Isopropyl
Ethanol
Methanol

4
2
0
200

400

600

800

1000

1200

Heating Power, kW

Fig.6. Vapor amount collected in one minute for each heating power.

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Methyl Alcohol

1200

Heating Power (kW)

1000

800

600

400

200
80

84

88

92

96

100

Distillate (%mol)

Fig.7 Heat added versus distillate purity

With the data measured, it was not possible to estimate the percentage of flooding in each case, for the height
of the liquid seal formed has not varied a lot with the vaporization rate. However, when analyzing the purity of
the top product, when distilling methanol solution at the different heating power tested, one could verify the loss
in efficiency more than 10% - due to flooding occurrence, when the maximum heat was added to the system.

4.Conclusions
This work was an attempt to estimate the amount of flooding and relate it to the heat input to the
system, in order to establish the maximum amount of energy to be added so that flooding would be avoided. The
amount of flooding, as function of the reboiler duty could not be established. However, it should be pointed out
that flooding did not occur when 300 kW (25% of the maximum heating power) had been used, for any of the
solutions tested. The decrease in efficiency due to flooding was evidenced for the methyl alcohol solutions as
the product purity obtained at the top of the column varied according to the heat reboiler rate and to the height of
the liquid film formed. However, the time for the mixture to reach the boiling point is quite long for a laboratory
class (circa 90 minutes). Therefore, we suggest the use of 40 60% of the maximum heating power, controlling
it in order to prevent flooding occurrence, slowly decreasing the power as flooding becomes eminent.

References
Bolles, W., L. in B. D. Smith (1963). Design of Equilibrium Stage Proceses, McGraw-Hill, New York.
Fair, J. R. and R. L. Matthews (1958). Pet. Refiner, 37, 4, 153.

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Kister, H. Z. (1990). Distillation Design, McGraw-Hill, Inc.

Kister, H. Z. and J. R. Haas (1990). Chem. Eng. Progress, 86, 9, 63.
Plant Documentation of QVF Engineering GMBH (2001). Contract no. 115293 MEC Brasilia
Souders, M. Jr. and G. G. Brown (1934). Ind. Eng. Chem., 26, 1, 98.
Wankat, P. C.(1988). Separations in Chemical Engineering: Equilibrium Staged Separations, Elsevier Publishing
Co.

Acknowledgements
The authors would like to thank the Director of Escola de Qumica/UFRJ for giving permission to use the
Multidisciplinary Laboratory.