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International Journal of Heat and Fluid Flow 65 (2017) 266–276

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International Journal of Heat and Fluid Flow


journal homepage: www.elsevier.com/locate/ijhff

Two-phase pressure drop and flooding characteristics in a


horizontal-vertical pulsed sieve-plate column
Pouria Amani a, Jaber Safdari b,∗, Hossein Abolghasemi a, Mohammad H. Mallah b,
Amin Davari a
a
School of Chemical Engineering, College of Engineering, University of Tehran, P.O. Box: 11155-4563, Tehran, Iran
b
Nuclear Fuel Cycle Research School, Nuclear Science and Technology Research Institute, P.O. Box: 11365-8486, Tehran, Iran

a r t i c l e i n f o a b s t r a c t

Article history: In this paper, an experimental investigation on the two-phase pressure drop has been carried out in a
Received 19 September 2016 novel class of extractors entitled "horizontal-vertical pulsed sieve-plate column". The liquid-liquid sys-
Revised 29 November 2016
tems used in this work are toluene–water, n-butyl acetate–water and butanol-water. The effects of op-
Accepted 8 January 2017
erating parameters including the dispersed and continuous phases flow rates and pulsation intensity on
Available online 1 February 2017
total pressure drop under and at the flooding points have been studied. It is achieved that the pressure
Keywords: drop is strongly affected by the continuous and dispersed flow rates as well as pulsation intensity. In
Pressure drop fact, the column experiences higher pressure drop with an increase in the values of Af, Q c and Q d . The
Flooding point interfacial tension is a physical property which has significant impact on pressure drop. Two theoretical-
Horizontal-vertical pulsed plate column experimental correlations for prediction of pressure drop under and at the flooding in the column, and
one correlation for maximum throughput are proposed by using dimensional analysis method with Av-
erage Absolute Relative Error (AARE) values of 2.15%, 3.56 and 6.85% respectively. Moreover, a particular
approach for preventing flooding in pulsed extraction columns is developed based on evaluation of pres-
sure drop through the column length.
© 2017 Elsevier Inc. All rights reserved.

1. Introduction another classification, the columns are divided into two major cat-
egories: vertical columns and horizontal columns. Vertical columns
Solvent extraction is one of the important processes of energy meet the needs for various industrial applications, but when space
and mass transfer with wide application in petroleum and petro- constraints are concerned it is required to use the horizontal type.
chemical industries, metal salt extraction, pharmaceutical indus- In addition, mass transfer efficiency in both types of the columns
tries, metallurgy and other areas (M.W.P., 1956). Various types of is comparable (Hanson, 2013). The main features of horizontal and
agitation and internals have been presented for liquid-liquid ex- vertical types of extraction columns in identical conditions have
traction columns over many years (Lewis, 2007). In particular, the been studied by different investigators (Hussain et al., 1988; Logs-
efficiency of liquid-liquid contactors is primarily dependent on the dail and Thornton, 1959; Melnyk et al., 1992; Procházka and Hafez,
degree of turbulence in the system and interfacial area available 1972; Vdovenko and Kulikov, 1966). The horizontal-vertical pulsed
for mass transfer. Accordingly, pulsed columns have a clear advan- sieve-plate column is a new type of extraction columns that its
tage over other mechanical contactors due to their high separation main advantages and disadvantages in comparison to vertical and
efficiency by increasing the drop breakage and coalescence rate horizontal types in industrial conditions can be presented as fol-
along with decreasing axial mixing (Jaradat et al., 2011; Peŕez et al., lows:
2005; Samani et al., 2014; Walzel, 2013). Pulsed columns for the
1. Throughput of one is more than horizontal type and less than
first time were introduced by Van Dijck (1935) and nowadays are
vertical type.
extensively used in various industries because of high efficiency
2. The required surface area and installation height for this type
and low space requirements as well as the fact that the pulsing
as indoor are less than those in horizontal and vertical types.
unit can be remote from columns. Pulsed extraction columns are
3. In horizontal-vertical columns, the amount of energy consumed
designed and built in packed, plate and disc and doughnut form. In
to create pulsation will be a value between that of vertical
and horizontal columns and for the same condition (structure)

Corresponding author. flooding occurs earlier in the horizontal column due to lack of
E-mail address: jsafdari@aeoi.org.ir (J. Safdari). use of maximum force of gravity caused by the density differ-

http://dx.doi.org/10.1016/j.ijheatfluidflow.2017.01.003
0142-727X/© 2017 Elsevier Inc. All rights reserved.
P. Amani et al. / International Journal of Heat and Fluid Flow 65 (2017) 266–276 267

 
ences. For horizontal-vertical columns due to the increase of
nρc 1.5 − 2.5α + α 2 + 1−ββ2 +
2
0.316s  2
this driving force, flooding will occur at higher flow rates than dRe0.25 dy
P = (3)
those for horizontal types. 2α 2 dt
An extraction column should provide high efficiency of separa- where s represents the plate thickness, Reo denotes the velocity in
tion and a large throughput. However, indefinitely increasing the the open area, d is the diameter of plate hole, and β = 0.65 is the
flow rate of the phases is not possible and the amount of one contraction coefficient.
phase which can be dispersed in another phase has a maximum Din et al. (2010) presented the following expression for pressure
value. By exceeding the flooding points, dispersed phase drops are drop in pulsed sieve-plate extraction column by modeling perfo-
no longer able to move against the flow of the continuous phase rated plates as a porous medium with 25% fractional free area in
and operation of the column becomes unstable. Consequent accu- computational fluid dynamics (CFD):
mulation of the dispersed phase appears at initial section of the
column and blocks the counter-current flow or the phases inver-
P = 107 × V − 2190.5 (4)
sion may be observed (Rincón-Rubio et al., 1993; Torab-Mostaedi Based on Eq. (4), it is surprisingly obtained that the pressure
et al., 2012). Therefore, the maximum volumetric capacity of the drop is linear function of the velocity V.
column, which is called flooding throughput, plays an important Stockfleth and Brunner (2001) by using modified models from
role in the design of an extraction column (Berger and Walter, normal pressure operation, correlated the dry pressure drop along
1985). A survey of previous investigations on flooding velocity is with the dispersed phase holdup below the loading point in a
presented in section 2. countercurrent randomly packed column with Raschig rings and
In all extraction columns, there is a need to predict design pa- Berl saddles. Yang et al. (1986) investigated the pressure drop, gas
rameters such as pressure drop in order to determine the operating holdup and interfacial area in a reciprocating-plate Karr extraction
status and provide information about energy consumption and the column and revealed that the frictional loss is closely related to the
required dimension of the column for particular purposes. Noh and circulation of liquid phase through the column. Jamialahmadi et al.
Baird (1984) and Rao and Baird (1988) studied the pressure drop (2005) experimentally and theoretically studied the pressure drop
for water flow in a 5-cm-diameter reciprocating plate column with for single- and two-phase flow through unconsolidated porous me-
cocurrent and countercurrent flow respectively and evaluated the dia. They described the single-phase pressure drop using the con-
variation of mass transfer with pressure drop under well-agitated servation equations and the Kozeny-Carman equation and also pro-
conditions. Thornton (1957) proposed a correlation for pressure posed a correlation for prediction of two-phase pressure drop and
drop with no flow under sinusoidal pulsation of a single phase in gas holdup. Khooshechin et al. (2013) have studied the two-phase
a perforated plate columns as follows: pressure drop in a pulsed packed column with ceramic packs of
   Raschig ring type of 0.63 cm in diameter for three liquid-liquid sys-
ρ 1 − α 2 dy 2 tems and suggested the modified form of the correlation of Varma
P = n (1)
2Cd2 α 2 dt et al. (1997) to calculated the two-phase frictional pressure drop in
packed columns as follows:
where ρ represents the flow density, α is fractional free area of
plates, Cd = 0.6 denoted discharge coefficient, n is the number of  σ 0.8446  μ4 g 0.187
plates which can calculated from L/h and dy/dt instantaneous flow Pf = 229.15Re−0 .6595 .612
Re0m,d d
m,c
μcVc ρc σ 3
velocity.
 0.1579  1
Jealous and Johnson (1955) proposed a correlation for power (A f )4 ρc ρc LVc2
× (5)
required for pulsation in a liquid-liquid extraction column by de- gσ 2d p
termination of static head of the liquid systems, the deceleration
and acceleration forces along with the fractional losses. The equa- Liu (2014) have studied the negative frictional pressure drop in
tion of Thornton (1957) can be also deduced from the expres- vertical two-phase flow and revealed that the energy dissipation
sion of Jealous and Johnson (1955), if considering only fractional is associated with a buoyancy-like term as well as the frictional
losses. In fact, according to what has been found by Noh and Baird pressure drop in vertical two-phase flow. In another study, Angelov
(1984) and Harikrishnan and Varma (1992) for the commonly-used and Gourdon (2012) studied on the pressure drop in a pulsed discs
combinations of agitation intensity and plate geometry, the pres- & doughnuts column and calculated local pressures by resolving of
sure drop fractional component is more than 2 orders of magni- turbulent flow model based on Reynolds equations coupled with
tude greater than the inertial component. The general expression k–ε model of turbulence.
of Jealous and Johnson (1955) is also used as a basis by other re-
(2A f )2 Lρc
searchers such as Hafez and Baird (1978). P = 0.21 α −2.80 h−0.85lnα−2.74 (6)
D
Harikrishnan and Varma (1992) proposed an expression for
pressure loss in terms of the relative velocity between liquid phase The experimental data of Angelov and Gourdon (2012) can also
and plates, in which by considering no flow, their correlation will be used for determination of pressure drop and developing a cor-
become identical to Eq. (1). relation for pressure drop as a function of pulsation parameters,
However, it should be noted that no pressure recovery down- inter-plate distance and fractional free area. Moreover, in many
stream of the plate is considered in above-mentioned correlations. research the application of CFD in measurement of the pressure
Accordingly, a modified expression is proposed by Miyauchi and drop in extraction columns is investigated (Fernandes et al., 2009;
Oya (1965) in order to take into account the pressure recovery in Langewisch and Buongiorno, 2015). One of the applications of mea-
each compartment of the column as follows: surement of pressure drop in extraction columns is to determine
   the flooding points (Robbins and Cusack, 1997), which is discussed
ρ (1 − α ) 1 − α 2 dy 2 in Section 2.1.
P = n (2) The objective of this work is the examination of hydrodynamic
2Cd2 dt
behavior of a novel horizontal-vertical pulsed sieve-plate column
In another work, Hafez and Procházka (1974) by studying the (HVPSPC), including pressure drop and its applicability for prevent-
pressure drop in a reciprocating plate column, proposed an empir- ing flooding in this column. Moreover, new correlations are devel-
ical correlation for fractional losses in turbulent regime as follows: oped for prediction of pressure drop under and at flooding points
268 P. Amani et al. / International Journal of Heat and Fluid Flow 65 (2017) 266–276

and a correlation is proposed to predict flooding points in terms of sation intensity leads to an increase in the capacity of the column,
operating variables and physical properties of the systems. reaching to a maximum value and then decreasing.
Berger and Walter (1985) calculated flooding for different sys-
tems as well as different geometrical parameters. Based on their
2. Previous work on flooding observations, as the ratio of phases flow rate (Vd /Vc ) rises, the peak
of the flooding curve declines, taking place at smaller frequencies.
Flooding in pulsed columns may be defined as the flow con- It can be due to the fact that an increase in the flow rate of the
dition when the fluid of one phase entering at one end of the dispersed phase, provides more fluidic resistance to the flow of the
column is not able to leave at the opposite end and must exit continuous phase flow rate. With respect to the interfacial tension,
through the effluent line intended for the second phase (Ragland smaller drops are formed in a smaller interfacial tension, which
et al., 1989; Sege and Woodfield, 1954). It can occur either due can easily pass through perforations. Accordingly, interfacial ten-
to inadequate pulsation in which plates act as a physical barrier sion along with the phase ratio plays an important role to pre-
in prohibiting counter-current flow of the two phases, or due to dict the maximum frequency where flooding happens. However,
passing the upper limit of the pulsation in which mechanical agi- the fractional free area of plates is ineffective on fm . Berger and
tation becomes excessive and emulsion flooding occurs (Smoot et Walter (1985) by comparing the correlations developed by Smoot
al., 1959). et al. (1959) and McAllister et al. (1967) with their own experi-
The flooding in pulsed columns is a function of different ge- mental data, have found that these correlations are able to neither
ometrical and operating parameters. For example, increasing hole predict the shape of the flooding curve nor provide accurate pre-
diameter, fractional free area, and plate spacing delays flooding diction in the emulsion regime.
in the column and leads to an increase of maximum throughput Tribess and Brunello (1998) studied the impact of mass trans-
along with a reduction in shear forces on drops, thereby influenc- fer (d→c) on the flooding behavior of pulsed columns. According
ing the mass transfer efficiency of the extraction column. Regard- to their results, the maximum capacity of the column increases
ing to operating parameters, the pulsation intensity (Af) and the in the presence of mass transfer and consequently hold-up occurs
direction of mass transfer have strong impact on flooding. Increas- at higher flow rates. They also showed that the maximum capac-
ing the pulsation intensity leads to an increase of the approach to ity of the column increases with plate spacing due to the reduc-
flooding. Moreover, mass transfer from dispersed phase to contin- tion of shear forces by increasing the plate spacing. Furthermore,
uous phase produces larger drops due to Marangoni effect which they modified the correlation of Berger and Walter (1985) to cover
leads to a reduction of the hold-up and consequently delays the the influence of mass transfer along with plate spacing. In Table 1
flooding tendency of the column as well as increasing maximum research that are implemented so far to calculate the velocity of
throughput (Komasawa and Ingham, 1978; Tribess and Brunello, flooding are listed.
1998). Conversely, the column shows the opposite manner in the
case of the reverse direction of mass transfer (Bender et al., 1979; 2.1. Measurement methods for the flooding points
Berger and Walter, 1985).
Numerous correlations have been proposed for prediction of Measurement methods for the flooding points can be derived
the flooding in extraction columns (Yadav and Patwardhan, 2008). from the events in the swarm of drops on flooding. As flooding oc-
Thornton (1957) and Logsdail and Thornton (1957) have conducted curs, the dispersed phase accumulates at initial sections of the col-
a comprehensive study of flooding for six different liquid systems. umn and internals act as a barrier for the counter-current flow. At
Thornton (1957) has investigated the impact of plate spacing, plate this time, the phase reversal would happen which called flooding.
geometry (i.e., hole-size and fractional free area), and the pulse The first approach was determination of flooding points through
wave-form on the flooding points of a pulsed plate column. He has direct measurement of holdup. In fact, holdup was measured at
differentiated the slip velocity (Vs ) relation to achieve the flood- two particular steady state condition in the constant operating pa-
ing capacity of the column in terms of the dispersed and the con- rameters; if two holdups were different or in other word experi-
tinuous phase velocities and derive a correlation to determine the enced an increasing trend through the time, it could be concluded
characteristic velocity (V0 ). It should be noted that his presented that flooding occurs in the column. However, flooding points can
correlation did not include the variation of the physical properties be recognized in many different ways. Some of these methods have
of the continuous phase. mentioned as follows:
Smoot et al. (1959) by using 665 flooding experiments of four
previous investigations, have developed a correlation for emul- 1. In glass column, the accumulation of the dispersed phase in the
sion flooding, in which the majority of dimensionless groups were initial parts of the column during the flooding can be visually
identical to those derived by Logsdail and Thornton (1957). How- observed. For more accurate measurement regarding this point,
ever, he did not proposed a criteria to classify the operating the assessment of the behavior of drops is required.
regimes of the used experimental data. In addition, McAllister et 2. Measuring discharge rate of both phases is another method. In
al. (1967) have revealed that the correlations proposed by Smoot steady state condition, mass flow rates of the continuous and
et al. (1959) and Thornton (1957) give very similar curves of mea- the dispersed phases during experiments are constant values,
sured (Vc + Vd )f versus Af. but because of the fact that after reaching the flooding points,
McAllister was the first researcher who have represented the the counter-current is disrupted, the output rate of the dis-
fundamental relationship between the pulsation intensity and the persed phase reduces and the continues phase output rate in-
limiting throughput which is called flooding curve. Moreover, creases. Such measuring of flow rate is a highly sensitive signal
Kagan et al. (1965) have described this curve as a parabolic curve for the beginning of the flooding.
which starts at the origin of the coordinates. 3. The third method is an indirect method of measuring the flood-
As achieved by Kagan et al. (1965), the maximum capacity of a ing points by differential pressure. At the flooding points, in
pulsed plate column declines with increasing in the ratio of phases spite of constant operating conditions, pressure is continuously
flow rate (Vd /Vc ). They have also indicated that the pulsation inten- rising. Differential pressure measurement is an accurate and
sity can be used instead of the frequency and amplitude individu- rapid diagnostic method for measuring the flooding points. It
ally for describing the behavior of the extraction column. Accord- is commonly used for the columns in which the drop patterns
ing to their results, in mixer-settler regime, an increase in the pul- cannot be observed (Robbins and Cusack, 1997). When accumu-
P. Amani et al. / International Journal of Heat and Fluid Flow 65 (2017) 266–276 269

Table 1
Equations provided by previous researchers to predict the velocity of flooding in pulsed extraction columns.

Reference correlation Remark

- It can been used for calculating emulsion flooding. Vc f = V0 (1 − 2ϕ f )(1 − ϕ f )2 (Thornton, 1957)
- This correlation does not cover the influence of the physical Vdf = 2V0 ϕ f 2 (1 − ϕ f )
0.5
properties of the phases and geometrical and operating parameters ϕ f = ( (R +8R ) −3R
2

4(1−R )
)
of the column on flooding due to the fact that the proposed
R = ( VVdc ) f
correlation considers holdup at flooding as a function of flow ratio
of the two phases only.
- It is derived from 665 experiments of four investigators and can (Vc f +Vdf )μc (Smoot et al., 1959)
σ =
been used only for calculating emulsion flooding.
0.527 VVc −0.014 ρρc 0.63 ( ερmc σμ4c )−0.207
5
( ) ( )
- Total flooding velocity was found to be independent of the d
σ ρc 0.458 D 0.0 gμ4c
column diameter. × dμ( 2 ) d
( ) (
ρc σ 4 )0.81 ( μμdc )−0.20
c
π 2 ( 1 −α 2 )
- Based on this correlation, the required column diameter can be εm = 2α 2 C 2 h Af 3 ( )
0
calculated from the following relationship, in which F is the
fraction of flooding velocity and W is the design capacity of the
column.

D( f t. ) = π F (V4cW+V )
d f

- C0 is orifice constant and is equal to 0.6.


- It is obtained from 1106 data points without considering mass (McAllister et al., 1967)
ln( Vcc +Vd
+ d
) = −3.471 + 0.2568lnX
transfer and it is applicable only for small hole diameter such that
−0.07194(ln(X ) )2 + 0.006191(ln(X ) )3
there is no flow due to density difference.
−1.034 ln(Y ) − 0.09096(ln(Y ) )2
- It can been used in the insufficient-pulsation region of flooding.
−0.0 0 08898(ln(Y ) )3 + 0.1424 ln( VVc )
- The equation is supposedly able to represent the complete d
−0.1807 ln( Ah ) + 0.07198 ln( YX )
flooding curve as a closed line, including the upper and lower
X = ρρ dπα2 g , Y = μασ c πv
2
flooding limits (Groenier et al., 1966). c M

- Physical significance of the different terms in the equation is 1 −λ 2
πD = 5π A f [ π −arcsin λ − λ], f t/hr
given in a report by Groenier et al (Groenier et al., 1966). 2

1 −λ 2
πc = 5π A f [ π +arcsin λ + λ], f t/hr
2

πM2 = 12 (πD2 + πC2 ), ( f t/h )2


πv = 12 (π√ D + πc ), f t/hr
c = A f [ √1 − λ2 + λ( π2 + arcsin λ)], f t/h
d = A f [ 1 − λ2 − λ( π2 − arcsin λ )], f t/h
λ = V5c fπ+AVfdf
2
- The first equation is presented for ascending part of flooding Vd
gD
= 2.5 × 10−2 ( VVc )1.1 ( DA )1.0 ( f gD )1.1 ( Dh )0.5 (Kagan et al., 1965)
d
curve and the second equation is presented for descending part of Vd
= 3.0 × 10 ( V ) ( D )
2
( g ) (D)
−9 Vc 1.1 A −1.75 f D −1.3 h 0.5
gD d
flooding curve.
- These correlations don’t cover the impact of variation of
physicochemical properties of the liquid systems.
- The applicability of the equations is limited to liquid systems
which have physical properties similar to kerosene–water.
- Studies have been done in absence of mass transfer. (Vc f + Vdf )m = (6.81 × 10−3 + 0.7047σ − 15.222σ 2 ) (Berger and Walter, 1985)
- The correlation does not cover the influence of mass transfer and × (1 − 4.55α + 3.247α 2 ) + 0.1778 ln( VVc )
d
plate spacing on flooding behavior of the pulsed columns. + 0.0437(ln( VVc ) )2
d
- fm is the maximum frequency at which flooding occurs and it is f m = 0.4908 + 1.11 × 102 σ − 1.80 × 103 σ 2
highly influenced by interfacial tension. − (3.44 × 10−2 + 7.1σ ) ln VVdc
- The system used was toluene-water with acetone as the mass (Vc f + Vdf )m = (6.81 × 10−3 + 0.7047σ − 15.222σ 2 ) (Tribess and Brunello, 1998)
transfer agent (d→c direction). × (1 − 4.55α + 3.247α 2 ) + 0.1778 ln( VVdc ) +
- The equation takes into account the effect of mass transfer and 0.0437(ln Vd
)2 (0.2115D0.20 h0.18 )[1 + ( VVdc dh Ct )]0.09
Vc
plate spacing.
f m = 0.4908 + 1.11 × 102 σ − 1.80 × 103 σ 2 −
- Column diameter was very small (D= 0.0394 m)
(3.44 × 10−2 + 7.1σ ) × ln( VVdc )(2.464A−1 D0.20 h−0.01 )
- Ct is weight fraction of solute in the feed at inlet.
× [1 + ( VVc h
C
d t
)]0.07
d

Vdf = 2.31( A fσμc )−0.41 ( σgμρ4c )−0.5 ( μ


μc −0.08
3
- Studies have been done for 4 different liquid-liquid systems in ) d
(Asadollahzadeh et al., 2011)
c
the absence of mass transfer
× ( eαg )0.127 ( ρσ2ραc )0.35 (1 +
3 Vd
Vc
)−0.43
d

lation occurs in the column, the pressure drop across the active was introduced to the liquid level and amplitude and frequency
section of the column increases considerably and continuously. were adjusted using setting movement amplitude of the liquid and
Therefore, similar to liquid-gas systems, any fracture in numeri- a digital controller, respectively. The diameter and length of active
cal graph of pressure difference in terms of the dispersed phase parts of the column are 6 cm and 296 cm, respectively. The active
flow rate is known as a starting point of flooding (Ousaka et al., part of the column is a pipe housing an internal plate cartridge
2006). This method was used to determine the flooding points consisting of 24 pairs of sieve plate in the horizontal section as
in this study. well as 29 individual sieve plates in the vertical section. An in-
verted U-tube manometer partially filled with toluene was used for
3. Experimental investigation measuring the pressure drop along the column in all experiments.
The column detailed geometrical characteristics and materials are
3.1. Description of equipment presented in Table 2.

A schematic diagram of experimental apparatus is shown in 2.2. Liquid-liquid system


Fig. 1. The setup has been consisted of vertical and horizontal parts
as active sections of the column, upper settler, bottom settler, four Liquid-liquid systems used in this work were toluene/water,
storage tanks, two dosing pumps, two rotameters, one U-shaped n butanol/water and n-butyl acetate/water in order to cover a
manometer and air pulsating system called pulsator. The pulsation wide range of interfacial tension. These systems have been recom-
270 P. Amani et al. / International Journal of Heat and Fluid Flow 65 (2017) 266–276

Fig. 1. A schematic diagram of the horizontal-vertical pulsed plate column.

mended by the European Federation of Chemical Engineering as of- At this time, the static two-phase pressure drop through the col-
ficial test systems for extraction investigations (Míšek et al., 1985). umn length was measured by using a manometer as can be seen
The Physical properties of these systems are listed in Table 3. All in Fig. 1. The next experiments were conducted at the same con-
experiments were carried out at the 20 ± 1 °C. tinuous phase flow rate and pulsation intensity, with increasing
dispersed phase flow rate. During the experiments, the manome-
2.3. Experimental procedure ter showed an increasing pressure drop as the flow rate of the
dispersed phase increased. This procedure is repeated 281 times
Before carrying out the experiments, both phases were mutu- in different pulsation intensities and the continuous and dispersed
ally saturated. The amplitude and frequency of pulsation were next phase flow rates for different liquid systems in order to study the
adjusted to the desired values and then, the column was filled with effect of operating and physical parameters on the pressure drop
the continuous phase from a storage tank, followed by the intro- through the column. Table 4 exhibits the experimental range of the
duction of the dispersed phase at the initial part of the horizontal operating parameters which has been studied.
section of the column. The interface position in upper settler was The average absolute value of the relative error (AARE) is used
then maintained at desired level, and liquid-liquid system was al- to compare the predicted results with the experimental data. This
lowed to reach steady state under a particular pulsation intensity.
P. Amani et al. / International Journal of Heat and Fluid Flow 65 (2017) 266–276 271

Table 2
Geometrical characteristics and material used for the column and plates.

Material used for settlers, column and pulsator Glass

Material used for plates Stainless steel

Main parts of the column Horizontal section Vertical section

Active parts length of the column (cm) 146 146


Active parts internal diameter of the column (cm) 6 6
Upper settler internal diameter (cm) – 9
lower settler internal diameter (cm) 9 –
Upper settler length (cm) – 90
Lower settler length (cm) 60 –
Plate thickness (mm) 1 1
Hole diameter (mm) 2 2
Hole pitch (mm) 4 4
Spacing between two plates (cm) 1∗ , 5∗∗ 5
Free area fraction (–) 0.11 0.22

spacing between two individual plates in a pair
∗∗
spacing between two pairs in a cell

Table 3 and dispersed phase outlets. In extraction columns, three differ-


Physical properties of system studies at 20 ± 1 °C.
ent flooding limits can be defined to characterize the permissible
Physical property Toluene–water n Butyl acetate–water Butanol-water working-area (Schilp and Blass, 1984):
ρ c (kg/m3 ) 998 997.6 985.6 1. Flooding at the light phase outlet, with discharging the heavy
ρ d (kg/m3 ) 864 880 846
phase.
μc (mPa s) 0.963 1.027 1.429
μd (mPa s) 0.586 0.734 3.36 2. Flooding at the heavy phase outlet, with discharging the light
σ (mN/m) 35.4 13.5 1.9 phase.
3. Flooding in both light and heavy phase outlets due to sig-
nificantly high total throughput of dispersed and continuous
Table 4
Operating parameters used. phases.

Biphasic system Af(cm/s) Qc (l/h) Qd (l/h) In this study, the two-phase pressure drop characteristics and
the visual flooding points (the second flooding limit due to its im-
Toluene-water 0.8,0.95,1.1,1.3 4.5–18 2.5–25
Butyl acetate –water 0.8,0.95,1.1 4.5–18 2.5–20 portance from the industry point of view), corresponding to the
n-butanol-water 0.8,0.95,1.1 4.5–18 2.5–20 loading curve have been evaluated. Furthermore, two correlations
for prediction of pressure drop under and at the flooding points,
and one correlation for determination of the flooding velocity have
is defined as follows: been proposed, which can be used for characterizing the operating
region of the column.
1 [Cal cul ated val ue − Experimental value]
NDP
AARE% = (7) 3.1. Pressure drop and flooding in counter-current two-phase flow
NDP Experimental value
i=1

in which NDP is number of points. In this study, the effect of the flow rates of the dispersed and
continuous phases on the static pressure drop for constant pulsa-
tion intensity of 1.1 cm/s is given in Fig. 2(a, b and c) for toluene–
3. Result and discussion
water, n butyl acetate–water and n butanol-water. As can be seen
from the graph, the pressure drop increases, with an increase in
For fully developed flow, the static pressure drop (P) for
the flow rates of the dispersed and the continuous phases for three
counter-current liquid–liquid flow through the active part of the
liquid systems. It is observed that under flooding points, the pres-
column can be calculated by Eq. (8):
sure drop gradually increases with an increase in the flow rate of
P = (ρc − ρd )gl (8) the dispersed phase. However, after reaching the flooding points,
further increase of the liquid throughput leads to a continuous in-
where l is height shown by the manometer, ρ c is the density of crease of the pressure drop. Increasing the flow rates of the dis-
the heavy phase and ρ d is the density of the light phase. The total persed and the continuous phases results in a rise of the interfa-
pressure drop (Pt ) through the active part of the column can be cial area between the coalesced phases due to the interfacial dissi-
determined by Eq. (9): pation as well as an increase in the dispersed phase holdup. Con-
Pt = PB − PA = ρc gH + (ρc − ρd )gl (9) sequently, this phenomenon delays the flooding tendency of the
column as well as increasing throughput.
where L represents the vertical distance between pressures taps, Fig. 3 (a, b and c) presents typical variation of the static pres-
H = 1.8 m represents the vertical distance between the points A and sure drop with the dispersed phase flow rates as well as pulsation
B, and (Pt is the total pressure drop that experimentally mea- intensity for the three systems of toluene–water, n butyl acetate–
sured. water and n butanol-water. It can be seen that the static pressure
One of the main objectives of this work is to clarify a suitable drop increases with increasing the pulsation intensity along with
method for the prediction of flooding conditions in a horizontal- the enhancement of the interfacial area between two phases. It is
vertical pulsed sieve-plate column. The flooding capacity or limit- clear that a rise in pulsation intensity results in the higher values
ing flow can be determined by observation of the possible range of shear stress and thus more drop breakage. Moreover, the spe-
of interface location until cloudiness appears in the continuous cific interfacial area is a function of the mean diameter as well
272 P. Amani et al. / International Journal of Heat and Fluid Flow 65 (2017) 266–276

Fig. 2. Variation of static pressure drop with continuous and dispersed flow rate for
Fig. 3. Variation of static pressure drop with pulsation intensity for the constant
constant pulsation intensity of 1.1 cm/s: (a) toluene–water (b) n-butyl acetate–water
continuous phase flow rate of 6.75 lit/hr: (a) toluene–water (b) n-butyl acetate–
(c) n-butanol-water.
water (c) n-butanol-water.

as the hold-up of the dispersed phase in the column. Therefore, continuous phase flow rate, the flooding occurs at lower values of
as the pulsation intensity increases, the mean drop diameter de- the dispersed phase flow rate, which indicates the reduction of the
clines along with a consequence increase in the value of the hold- throughput of the column in higher pulse velocities.
up, which leads to an increase in the interfacial area between the The effect of pulsation intensity on the throughput of the col-
continuous and the dispersed phases. It can be concluded that in- umn for different liquid-liquid systems with different interfacial
creasing the pulsation intensity brings forward the flooding ten- tension is illustrated in Fig. 4 for the constant continuous flow rate
dency of the column as well as decreasing the maximum through- of 9 lit/hr. According to Fig. 4, with increasing the pulsation in-
put. As can be observed in Fig. 3, increasing the pulsation intensity tensity, throughput of column decreases. Moreover, the flooding is
leads to an increase of the approach to flooding, and in constant reached with lower dispersed phase flow rate in the same con-
P. Amani et al. / International Journal of Heat and Fluid Flow 65 (2017) 266–276 273

Fig. 5. Comparison of experimental pressure drop under flooding with those calcu-
lated from Eq. (11).

other types of extraction columns and new predictive correlations


Fig. 4. Variation of the flooding points of the column with pulsation intensity at are needed to evaluate the performance of such columns. In the
different flow ratio (R) for toluene-water (T-W), butyl acetate-water (BA-W) and n following, two predictive correlations, considering the effect of the
butanol-water (B-W).
operating parameters and physical properties, are proposed one for
the case under flooding points and another one for the case at the
tinuous phase flow rate. In addition, it can be obtained that in flooding points in order to determine the static pressure drop in
the liquid systems with lower interfacial tension, the maximum the experimental setup.
throughput of the column has lower values. In fact, with a decline a) Pressure drop below the flooding points:
in interfacial tension, pulsation produces smaller drops and conse- As shown in Figs. 2-4, the pressure drop under flooding is a
quently the maximum holdup of the dispersed phase increases to function of Qc , Qd , and Af as well as physical properties of the sys-
the higher values and the maximum capacity of the column will tems which can be presented by Eq. (10):
increase.
P = f (Qc , Qd , ρc , ρd , μc , μd , A f, σ ) (10)
Fig. 4 also exhibits that the maximum throughput of the col-
umn increases with the enhancement of the dispersed to continu- For prediction of the pressure drop, a theoretical-experimental
ous phase flow ratio (R). It is clear that the rising velocity of the correlation is proposed in terms of the operating parameters and
dispersed phase drops relies upon the drop diameter and on the the physical properties of the liquid systems by the dimensional
other hand, the interfacial tension is the physical property which analysis method as follows:
has the strong influence on the drop diameter. Therefore, increas-
 −0.006  −0.004  −9.788
ing the flow ratio leads to the formation of larger drops and since P −4 A f Vd ρ
the buoyancy forces on larger drops have greater values compared = 2.98 × 10
(A f )2 ρc Vd Vc ρc
to smaller drops, the residence time of the dispersed phase drops
 μ 3.994  σ 1.985
will decrease and consequently the capacity of the column in- d
× (11)
creases. Fig. 4 also indicates that the flooding points change with μc A f μc
the variation of interfacial tension. In fact, chemical system with
high interfacial tension results in larger drops, lower residence The comparison of the experimental data for the three chem-
time, the higher relative velocity between the continuous and dis- ical systems with those calculated by Eq. (11) is shown in Fig. 5.
persed phases, following by a reduction in holdup of the dispersed The experimental values of P which were obtained from the ex-
phase which leads to more stable operating condition. Therefore, periments showed very good agreement with those calculated by
higher total allowable throughput can be achieved in systems with Eq. (11) and it was clear that the presented correlation is able to
higher interfacial tension. give satisfactory prediction of the static pressure drop under flood-
ing in the horizontal-vertical pulsed sieve-plate column. The AARE
was 2.15%.
3.2. Predictive correlation for pressure drop
b) Pressure drop at the flooding points:
For prediction of the pressure drop at flooding points, another
The literature provides a few developed equations on the pres-
correlation is derived in terms of the operating parameters and
sure drop in the pulsed sieve-plate columns and most of them do
physical properties of the liquid systems by the dimensional anal-
not consider all operating parameters and physical properties of
ysis method as follows:
chemical system into account. Therefore, there is still a lot to do
in this field. In particular, the horizontal-vertical pulsed sieve-plate  −0.002  −0.002  ρ −9.819
P f Af Vd
column is a novel type of the extractors which is investigated for = 2.64 × 10−4
the first time in this work. In fact, in horizontal section of the (A f )2 ρc Vd Vc ρc
horizontal-vertical column, the influence of the gravitational ac-  μ 4.007  σ 1.992
d
celeration and consequently buoyancy forces on drops movement × (12)
μc A f μc
is limited, while in vertical section, similar with other standard
vertical pulsed columns, these forces are considerable. Therefore, A comparison of the experimental results for the three chemical
a horizontal-vertical pulsed column will operate differently from systems with the values predicted by Eq. (12) is shown in Fig. 6. It
274 P. Amani et al. / International Journal of Heat and Fluid Flow 65 (2017) 266–276

3.3. Predictive correlation for flooding velocity

Operating parameters including pulsation intensity and flow


rates of continuous and dispersed phases as well as geometrical
and physical properties affect the flooding in the pulsed column.
Increase in the pulsation intensity has been found to enhance the
approach to flooding. Moreover, an increase in the plate parame-
ters, e.g., percentage free area, perforation diameter, or plate spac-
ing increase the maximum throughput and consequently delay the
flooding in the column. However, with increasing these parame-
ters, the mass transfer performance of the column decreases due
to the reduction of shear forces.
Regarding the prediction of flooding, two approaches are avail-
able in the literature: one is prediction of the entire flooding curve
(Logsdail and Thornton, 1957; McAllister et al., 1967; Smoot et
al., 1959) and another one is prediction of only the maximum in
the flooding curve (Berger and Walter, 1985; Tribess and Brunello,
1998). In this study, the former approach is used for the experi-
Fig. 6. Comparison of experimental pressure drop at flooding with those calculated mental data.
from Eq. (12). Fig. 7(a and b) exhibits the predictive ability of the correla-
tions from the work of Smoot et al. (1959) and McAllister et al.
(1967) respectively. It is achieved that none of the correlations are
in good agreement with experimental data. Since the available cor-
relations are not general enough to determine the entire flooding
reveals the accuracy of the derived equation in order to evaluate curve for a liquid–liquid system in different columns, a compre-
the pressure drop at flooding points in the column. The AARE was hensive experimental investigation is still required. However, it is
3.56%. recommended to investigate on fluid dynamic and mass transfer
In addition to the application of two-phase pressure drop for for three liquid-liquid systems including n butanol–succinic acid–
design and scale-up of an extraction column, it can been used for water, n butyl acetate–acetone–water and toluene–acetone–water
evaluation of operating parameters based on the flooding points. (Míšek et al., 1985) in order to cover a wide range of interfacial
Accordingly, operating parameters including pulsation intensity tension which leads to lower required cost (Lorenz et al., 1990).
and flow rate of phases can be set on the initial values. Then, pres- Since the determination of flooding is primarily for extraction
sure drop can be calculated using Eqs. (11) and (12) in the ba- columns, based on 54 flooding velocity data points, a theoretical-
sis of these parameters along with physical properties of the liq- experimental correlation is proposed for prediction of flooding
uid system. Regarding the comparison between the calculated val- curve in terms of the operating parameters and physical proper-
ues of two-phase pressure drop obtained from Eqs. (11) and (12), ties of the liquid systems by the dimensional analysis method as
if the pressure drop from Eq. (11) is less than 80% of that calcu- follows:
lated by Eq. (12), the initial operating conditions can be applied for  −0.109  −0.095
the steady-state column operation. On the other hand, if the pres- (Vd + Vc ) f μc Af Af
= 2.086 × 10−8
sure drop from Eq. (11) is greater than 80% of that obtained from σ Vc Vd
Eq. (12), the specified parameters are not appropriate for operating  −6.586  2.582 
under steady-state condition and flooding probably happens in the ρ μd σ 0.404
× (13)
column. Therefore, at this condition the initial operating parame- ρc μc A f μc
ters should be modified and this procedure have to be repeated
until the pressure drop obtained from Eq. (11) becomes less than A comparison of the experimental results for the three chemi-
80% of that of Eq. (12), thereby operating under steady-state con- cal systems with the values predicted by Eq. (13) is illustrated in
dition. Fig. 8. This figure shows good agreement between the calculated

Fig. 7. Testing the predictive ability of different correlations for flooding in horizontal-vertical pulsed sieve-plate columns: (a) Smoot et al., (1959) correlation and (b)
McAllister et al., (1967) correlation.
P. Amani et al. / International Journal of Heat and Fluid Flow 65 (2017) 266–276 275

V Velocity, m/s
Vc Superficial velocity of continuous phase, m/s
Vd Superficial velocity of dispersed phase, m/s
Vs Slip velocity, m/s
V0 Characteristic velocity, m/s
ʋ Kinematic viscosity, m2 /s
y Change of position along the column length, m

Greek Symbols
P Pressure drop, pa
P f Frictional pressure drop, pa
α Fractional free area
ɛ Power dissipated per unit mass of fluid, W/kg
ϕ Hold-up
μ Viscosity, N s/m2
ρ Density, kg/m3
ρ̄ Density of mixture of phases, kg/m3
Fig. 8. Comparison of experimental flooding velocity of dispersed phase with those σ Interfacial tension between two phases, N/m
calculated from Eq. (13).
Subscripts
c Continuous phase
values and the experimental data of the flooding velocity of dis- d Dispersed phase
persed phase. The average absolute of the relative error was 7.22%. f Flooding

4. Conclusion References

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