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Corresponding author. Tel.: +91 22 2414 0865; fax: +91 22 2414 5614.
E-mail address: jbj@udct.org (J.B. Joshi).
(Imamura et al., 1993), synthesis of silica particles (Ogihara et
al., 1995), and heterogeneous catalytic reactions (Sczechowski
et al., 1995).
The schematic diagram of coaxial cylinders [(1) and (2)] is
shown in Fig. 1. The immiscible feed liquids enter at points
(3A) and (3B) into the annular region of the two cylinders. The
rotating impeller imparts power (in the range of 1500kW/m
3
)
which results into a very ne dispersion of the two immisci-
ble liquids. The dispersion ows downwards in the annular
region (where the mass transfer occurs) and then ows radi-
ally inwards in the region below the rotating cylinder [(points
(4A) and (4B) in Fig. 1)] and nally enters the central open-
ing of the rotating cylinder (point 5). Bafes (6) are provided
in the bottom region which are either attached to the base
of the outer cylinder (as shown in gure) or attached on the
bottom of the rotating cylinder (the role of these bafes will
be explained later). The dispersion entering the central hole
gets deected towards the wall by the horizontal bafe (7) pro-
vided close to the entrance. Above the level of (7) the rotor is
provided with vertical bafes [(8) shown in plan] so as to cre-
ate several chambers ranging from4 to 8. The rotating cylinder
0263-8762/$ see front matter 2007 The Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.
doi:10.1016/j.cherd.2007.10.020
234 chemi cal engi neeri ng research and desi gn 8 6 ( 2 0 0 8 ) 233244
Nomenclature
a centrifugal acceleration (r
2
) (m/s
2
)
u
-
effective interfacial area (m
2
/m
3
)
[A*] solubility of ester in NaOH solution (kgmol/m
3
)
[A
0
] concentration of ester in NaOH solution
(kgmol/m
3
)
b bafe height (m)
[B
0
] concentration of NaOH (kgmol/m
3
)
c bottom clearance (m)
C constant in Eq. (16)
C
1
constant in Eq. (2)
C
2
proportionality constant in Eq. (3)
C
3
constants in Eq. (4)
d annulus gap width (m)
D diameter of cylinder
E extraction efciency (%)
g acceleration due to gravity (m/s
2
)
H dispersion height in the annulus (m)
j factor dened in Eq. (7)
k individual phase mass transfer coefcient (m/s)
k
2
second order reaction rate constant
(m
3
/kgmol s)
k
C
u
-
volumetric continuous phase mass transfer
coefcient (1/s)
m partition coefcient
N rotor speed (r/s)
N
D
dispersion number
P mean rate of energy dissipation in uid (W)
Q ow rate (m
3
/s)
r radius of the cylinder (m)
r
m
(r
i0
+r
0i
)/2 mean radius of the annulus (m)
R
A
rate of extraction (kgmol/m
2
s)
Re Reynolds number
t batch time or average residence time for break-
ing the dispersion (s)
[U
E
] uranium concentration in aqueous efuent
after equilibrium with an equal volume of
organic efuent (kgmol/m
3
)
[U
F
] uranium concentration (kgmol/m
3
)
[U
R
] uranium concentration in aqueous efuent
(kgmol/m
3
)
V volume (m/s)
V
C
continuous phase supercial velocity (m/s)
V
D
dispersed phase supercial velocity (m/s)
V
N
characteristic velocity (m/s)
V
Z,
,
C
1.5
4r
2
io
,
C
j
C
0.18
g
2r
io
1.1
r
oi
r
io
1.2
(1)
The characteristic velocity was found to depend upon the
vortex pattern occurring in the annulus. The authors also
investigated the mass transfer coefcient using toluene and
butyl acetate as the organic phase, water as the aqueous phase
and acetone was used as a solute being transferred fromwater
to organic phase, and vice-versa. The overall mass transfer
coefcient was correlated with the equipment geometry and
the rotor speed as
k
C
u
-
=
V
D
C
1
r
oi
r
oi
2
g
0.74
r
io
r
oi
2.31
(2)
Fig. 4 Effect of rotor speed, annulus gap width on
continuous phase mass transfer coefcient in ACE-30 (),
2mm WOB; () 6, mm WOB; (), 6mm WB; (), 10mm
WOB; (), 10mm WOB.
The constant C
1
was found to depend on the physical prop-
erties of the two systems investigated.
Davis and Weber (1960) used 5Mnitric acid and 2.5%TBP in
ultrasene as the two phases. The rotor diameter was varied in
the range of 20.2132mm and the annular gap between 1 and
7mm the authors measured the fractional dispersed phase
hold-up (c
D
) and correlated by the following equation:
Table 2 Physical properties of systems used in separation capacity
No. System Density difference
(gm/cc)
Interfacial tension
(dyn/cm)
Continuous phase
viscosity (cp)
1 Hexanewater 0.34 58.3 1
2 (Hexane+10% CCl
4
)water 0.25 56.5 1
3 (Hexane+20% CCl
4
)water 0.15 55 1
4 (Hexane+58% CCl
4
)water 0.20 45 1
5 (Hexane+69% CCl
4
)water 0.30 42 1
6 Butanolwater 0.19 3 1
7 Toluenewater 0.22 35.5 1
8 Butyl acetatewater 0.12 16.2 1
9 Butyl acetate25% DEG 0.145 15 3
10 Butyl acetate50% DEG 0.17 14 6.5
11 Kerosenewater 0.22 48.5 1
12 Carbon tetrachloridewater 0.6 45 1
chemi cal engi neeri ng research and desi gn 8 6 ( 2 0 0 8 ) 233244 237
Fig. 5 Effect of rotor speed and annulus gap width on
mass transfer coefcient in ACE-75 (), 5mm; (), 9mm; (),
13mm; (), 16mm.
c
D
= C
2
r
0.5
m
d
1.5
,
C
r
io
r
oi
j
C
2
V
0.5
D
d
3
(3)
The proportionality constant was stated to be dependent
upon the physical properties of the system under considera-
tion. The authors also measured the values of mass transfer
coefcient and the following correlation was proposed:
k
C
u
-
= C
3
d
3.65
V
D
(r
0.5
m
d
1.5
,
C
r
io
,r
oi
j
C
)
2.2
(m(V
D
,V
C
) 1)
ln(m(V
D
,V
C
))
(4)
Fig. 6 Effect of rotor speed on mass transfer coefcient in
ACE-250.
Fig. 7 (A) Effect of power per unit volume on mass transfer
coefcient in ACE-30, 75 and 250. (B) Parity plot for
continuous phase mass transfer coefcient (Eq. (15)).
Bernstein et al. (1973a) studied the separating capacity
of 31.8mm size rotor ACE and the rotor speed was varied
in the range of 33.3358.33r/s, total (organic plus aqueous)
throughput range from 3.3310
4
m
3
/s to 1.13310
3
m
3
/s
with a ow ratio of 0.254 of organic to aqueous phase.
They used 0.5M HNO
3
as aqueous phase and 30% tri-n-butyl
phosphate (TBP) as the organic phase. They estimated the
extraction efciency using the following form of the equa-
tion:
E =
[U
F
] [U
R
]
[U
F
] [U
E
]
100 (5)
They also studied the effect of solids by using aqueous feed
solutioncontaining MnO
2
up to 1600ppm. At steady state con-
ditions, no MnO
2
appeared in the efuent streams. The solids
were found to get accumulated in the rotor, and no signicant
effect on the performance of the unit was observed up to an
accumulation of 50gm.
238 chemi cal engi neeri ng research and desi gn 8 6 ( 2 0 0 8 ) 233244
Fig. 8 Effect of rotor speed and annulus gap width on separating capacity in ACE-30 (), 2mm; (), 6mm; (), 16mm.
Fig. 9 Effect of density difference and interfacial tension on separating capacity at different rotor speed (), Hexane-water;
(), hexane+69%CCl
4
water; (), hexane+10% CCl
4
water; (), hexane+58% CCl
4
water; (), hexane+20% CCl
4
water; O,
toluenewater; (), butyl acetate; (+), butanolwater.
chemi cal engi neeri ng research and desi gn 8 6 ( 2 0 0 8 ) 233244 239
Fig. 10 Effect of continuous phase viscosity on separating capacity in ACE-30: (), 1 cp; (), 3 cp; (), 6.5 cp.
Leonard et al. (1981) used rotor diameter in the range of
30250mm, rotor speed in the range of 10100r/s and the
annular gap 3.323.6mm the authors investigated the separa-
tioncapacityof the rotor. Theyalsoinvestigatedthe separation
of dispersion under gravity conditions. The effectiveness of
separation was expressed in terms of the following dimen-
Fig. 11 Effect of rotor speed on separating capacity in
ACE-250 (), 19rps; (), 23.75rps; (), 26.8rps; (), 30.87rps.
sionless number:
N
D
=
1
t
LZ
u
(6)
where t is the time required for complete separation for batch
or continuous conditions. LZ is the initial height (or thickness
in the case of rotor as can be seen at level 1 in Fig. 2) and a is
either g or r
2
depending upon the conditions of separation.
The value of N
D
was found to be independent of ow ratio
(O/A), rotor speed, annular gap, rotor diameter, liquid level in
the annulus, feed point position and method of separation (i.e.
over a wide range of a (from 1 to 100g)). The authors analysed
their own and literature data and found the value of N
D
to be
in the range of 0.00010.02 depending upon the liquidliquid
system.
Arafat et al. (2001) theoretically derived equation for power
consumption which is given by
P = 0.0261Hr
3.75
io
(j)
2.75
,
0.75
C
j
C
d
0.25
(7)
where
j = 0.0554(logRc) +1.368 (3 10
3
- Rc - 1 10
6
) (7A)
Rc =
2j,
C
r
io
d
j
C
(7B)
240 chemi cal engi neeri ng research and desi gn 8 6 ( 2 0 0 8 ) 233244
Fig. 12 Effect of rotor speed on dispersion number in
ACE-30.
3. Experimental set-up and procedure
3.1. Experimental set-up
Experiments were performed in 30, 75 and 250mm rotor size
centrifugal extractors henceforth we call them as ACE-30,
ACE-75 and ACE-250, respectively. A schematic diagram of the
experimental set-up is shown in Fig. 3. All the three exper-
imental set-ups were similar except motor in ACE-250 was
ange mounted and aligned vertically. The rotor heights in
the respective equipment were 75, 100 and 390mm. For ACE-
30 and ACE-76 the annular gap was varied by selecting outer
cylinders with appropriate diameters.
3.2. Determination of ooding rates
Flooding rates have been determined in all the three extrac-
tors; ACE-30, ACE-75 and ACE-250. Rotor speed was varied
Fig. 13 Effect of rotor speed on dispersion number in
ACE-250.
from 1100 to 2400 under experimental conditions reported
in Table 1. Experiments are performed with organic phase
as a dispersed as well as continuous phase. Organic solvents
like butyl acetate, toluene, butanol, cyclohexanol, cyclohex-
anone, kerosene and carbon tetrachloride were used whereas
the aqueous phase consisted of water or aqueous solution of
diethylene glycol.
Initially, the solvent and aqueous phases were saturated
with respect to one another so that no mass transfer occurs
during dispersion and separation and practically no change in
the physical properties of both the phases. In order to deter-
mine the ooding rates, the extractor was lled with aqueous
phase and the rotor speed and the aqueous phase ow rate
were adjusted to the predetermined values. The dispersed
phase ow rate was increased in small steps and sufcient
time (>10 times residence time) was provided for attaining
the steady state. The outlet aqueous and organic phases were
analysed for the presence of the other phase and ooding con-
dition was designated when any phase exceeds more than
0.05% of the other phase (Table 2).
3.3. Determination of mass transfer coefcient
Chemical method as suggested by Doraiswami and Sharma
(1984) were used for the measurement of k
C
u
-
. For the mea-
surement of k
C
u
-
, it is important that the overall rate depends
(at least partially) on the mass transfer coefcient. This condi-
tion can be achieved if the rates of mass transfer and chemical
reaction are comparable. This condition is mathematically
expressed as
k
C
u
-
c
C
k
2
[B
0
] (9)
D
A
k
2
[B
0
]
k
C
-- 1 (10)
The second condition given by Eq. (10) conrms that no
reaction occurs in the diffusion lm and the steps of mass
transfer and chemical reaction occur in series and the follow-
ing rate equations hold:
R
A
u
-
= k
C
u
-
([A
] [A
0
]) (11)
R
A
u
-
= c
C
k
2
[A
0
][B
0
] (12)
Eliminating of [A
0
] from Eqs. (11) and (12) we get:
[A
]
R
A
u
-
=
1
k
C
u
+
1
c
C
k
2
[B
0
]
(13)
Eq. (13) was used for the estimation of k
C
u
-
. For this pur-
pose, batch mode of operation was selected. Predetermined
quantities of aqueous NaOH and organic phase (butyl acetate,
iso-amyl acetate, hexyl acetate) were taken in the annular
space, and for a given rotor speed, the NaOH concentration
[B
0
] was monitored with respect to time. A plot based on Eq.
(13) gives the value of k
C
u
-
from the intercept. The values of
solubility [A*], diffusivity D
A
were estimated according to the
procedure given by Danckwerts (1970).
chemi cal engi neeri ng research and desi gn 8 6 ( 2 0 0 8 ) 233244 241
Fig. 14 Effect of annulus gap on dispersion number in at different rotor speed.
Fig. 15 Effect of density difference on dispersion number at different rotor speeds.
242 chemi cal engi neeri ng research and desi gn 8 6 ( 2 0 0 8 ) 233244
4. Results and discussion
4.1. Mass transfer coefcient
The value of k
C
u
-
from ACE-30, 75 and 250 are shown in
Figs. 46, respectively. It canbe seenthat, k
C
u
-
increases withan
increase in the rotor speed, increase in the rotor diameter and
a decrease in the annulus gap. This is mainly because of the
corresponding variation in the power consumption per unit
annular volume (P/V). The relationship between k
C
u
-
and P/V
is shown in Fig. 7 where the following correlation can be seen
to hold in the range from 1 to 500kW/m
3
with a correlation
coefcient of 0.96.
k
C
u
-
= 0.64
P
V
0.22
(14)
when the P/V in range of 0.41kW/m
3
, the exponent in the
above equation was found to be 0.45. The value of P/V in com-
mercial practice is expected to be always above 50kW/m
3
and
the correlation given by Eq. (14) is expected to be useful for the
design purpose. The above correlation is valid for extractors
having c/Dof about 0.1 andb/Dof about 0.08. Experiments were
also performed over a wider range of (0.088<c/D<0.43) and
bafe height (0.02<b/D<0.2). Data is analysed using multiple
regression technique in POLYMATH-5.1. For the entire range,
following dimensionless correlation found to hold with a cor-
relation coefcient of 0.95 and standard error for all indices of
tted dimensionless parameters were less than 7%
k
C
u
-
N
S.E.:
= 10.2
D
io
Nj
C
o
0.04
0.81
b
D
io
0.012
0.2
d
D
io
0.013
0.19
g
D
io
N
2
0.026
0.61
j
C
,
C
D
C
0.024
0.53
(15)
Fig. 7 shows a parity plot (average deviation 5.2%).
It may be pointed out that, though the P/V range is
50500kW/m
3
, the largest annular volume was 10l. Therefore,
at a P/Vvalue of 500 the actual power consumptionfor 250mm
extractor is 5kWwhichhandles the capacity of combined ow
rate in the range of 510m
3
/h. For a similar capacity, typi-
cal mixer-settler needs a volume of about 25m
3
and power
consumption is 5kW. Thus it can be seen that the annular
centrifugal extractor does the same job of the mixer-settler
with about 500 times less volume and practically for the same
power consumption. It may be reminded at this stage that
a centrifugal extractor gives much cleaner separation than a
mixer-settler.
4.2. Separation capacity
The separation capacity was found to increase with an
increase in the rotor speed and the corresponding increase in
the centrifugal force (r
2
). Further, the separationcapacity was
found to increase with an increase in the annular gap which
increases the volume and hence decreases P/V value for the
same rotor speed. A decrease in P/V means larger dispersed
phase drops and the ease for separation
The effect of density difference and the interfacial tension
was studied together and results are shown in Fig. 8. It can be
seen that the separation capacity increases with an increase
in the density difference as well as the interfacial tension.
Table 3 Values of indices in Eq. (16)
No. N (r/s) C a b
1 23.3 40 0.14 0.59
2 30 40 0.14 0.53
3 36.7 40 0.15 0.49
4 43.3 7 0.286 0.189
Fig. 8 shows that, at relatively low rotor speed, the separa-
tion capacity is a strong function of interfacial tension and is
a weak function of density difference. The reverse was found
to be true at relatively high impeller speed. The permissible
capacity of both phases together was correlated by the follow-
ing equation where the values of a and b are given in Table 3
(Fig. 9).
Q
C
+Q
D
= CL,
u
o
b
(16)
The effect of continuous phase viscosity (j
C
) on the effec-
tiveness of the separation is shown in a Fig. 10. It can be
seen that the separation capacity decreases with an increase
(j
C
) due to the corresponding decrease in the slip veloc-
ity of drops. Further, from Fig. 10 it can be seen that the
Fig. 16 Effect of continuous phase viscosity on dispersion
number at different rotor speed.
chemi cal engi neeri ng research and desi gn 8 6 ( 2 0 0 8 ) 233244 243
Fig. 17 Effect of interfacial tension on dispersion number at different rotor speed.
dependence of separation capacity on (j
C
) remains practi-
cally the same over the range of rotor speed covered in this
work.
Experiments of separation capacity were also carried out
in ACE-250 and the results for kerosenewater system are
shown in Fig. 11. These data were used to estimate the value
of dispersion number (N
D
) given by Eq. (6). It can be seen
from Fig. 12 that as the rotor speed increases, the value of
(N
D
) decreases. In the case of ACE-250, there is a slight (10%)
decrease in the dispersion number when the rotor speed
was varied in the range of 1730.9r/s. It is also seen from
Figs. 12 and 13, that in ACE-30, for different ow ratios (varied
over a factor of 16), the dispersion number (N
D
) remains
almost constant except at rotor speed 30r/s it changes by
15% and in ACE-250 this difference is less than 5%. As the
annular gap increases, the dispersion number increases and
in ACE-30 (Fig. 14), it increases by 17% when the annular
gap increases from 2 to 16mm (Fig. 12). In addition, a it was
observed that 15% drop in dispersion number was observed
when the density difference decreased from 340 to 100kg/m
3
.
Further, similar extent of the change was observed at all the
rotor speeds (Fig. 15). It can be seen that the value of N
D
sub-
stantially decreases with an increase in j
C
. Further, the value
of N
D
was found to increase with an increase in interfacial
tension. It is interesting to note that (Figs. 16 and 17), the
dependence of N
D
on j
C
and o is practically independent of
the rotor speed covered in this work. It was thought desirable
to developa correlationfor the dispersionnumber (N
D
). Data is
analysed using multiple regression technique in POLYMATH-
5.1. Over the range of variables covered in this work
[0.03<D<0.25m, 2<d<25mm, 7<b<22mm, 16.6<N<50r/s,
50<L, <340kg/m
3
, 1.8<o <58mN/m, 1<j
C
<6.5mPas,
1<j
D
<6.5mPas] following dimensionless correlation found
to hold witha correlationcoefcient of 0.94 and standard error
for all indices of tted dimensionless parameters were less
than 10%
N
D
=0.037
Q
C
ND
3
ii
0.26
Q
D
ND
3
ii
0.41
c
D
ii
0.26
d
D
ii
0.062
g
D
ii
N
2
0.17
S.E. : 0.012 0.013 0.025 0.006 0.013
(17)
Fig. 18 shows a parity plot (average deviation 6.3%).
Fig. 18 Parity plot for dispersion number (Eq. (17)).
244 chemi cal engi neeri ng research and desi gn 8 6 ( 2 0 0 8 ) 233244
5. Conclusions
1. Mass transfer coefcient was measured in three annular
centrifugal extractors having rotor diameter of 30, 75, and
250mm. The following dimensionless correlation is pro-
posed for the estimation of mass transfer coefcient:
k
C
u
-
N
= 10.2
D
io
Nj
C
o
0.81
b
D
io
0.2
d
D
io
0.19
g
D
io
N
2
0.61
j
C
,
C
D
C
0.53
2. The separation capacity of 30, 75 and 250mm rotor diam-
eter annular centrifugal extractor was investigated over a
wide range of design and operating variables [0.03<D
<0.25m, 2<d<25mm, 8<c <22mm 1.5<b<20mm,
16.6<N<50r/s, 50<L, <340kg/m
3
, 1.8<o <58mN/m,
1<j
C
<6.5mPas, 1<j
D
<6.5mPas]. The results have been
correlated in the form of dispersion number (N
D
) for
which the following correlation was found to hold with a
correlation coefcient of 0.93:
N
D
=0.037
Q
C
ND
3
ii
0.24
Q
D
ND
3
ii
0.38
c
D
ii
0.26
d
D
ii
0.06
g
D
ii
N
2
0.17
r e f e r e nce s
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