Solvent Extraction Equipment

Pierre Trambouze

Liquid-liquid extractors are designed to accomplish separations between

molecular species based on their differences in solubility in a solvent.
Accordingly, the choice of solvent is of greatest importance for an efficient
operation (see Vol. 2) and the solubility equilibrium curve needs to be known
for the species to be extracted between the initial phase and the solvent
phase. The extractor carries out two processes which are opposed in their
principles:
Mix the solutions thoroughly. The more thoroughly dispersed one phase
is in the other, the better the solute transfer.
Separate the resulting phases. Separation is performed either in specially
designed zones at each end of the columns or in settlers.
Most extractors work in counter-current flow, but they differ essentially in
the way the contact is made between phases.
Following the presentation of the general characteristics of liquid-liquid
systems, the discussion will focus on the different types of extractors cur-
rently in use. The basic calculation elements used to forecast performance will
be given for the most common extractors.

3.1 General Hydrodynamic Features

of LiquidMLiquid Systems
The general concepts of mass transfer between phases (see Vol. 2) are also
applicable to liquid-liquid systems. However, these systems exhibit specific
characteristics which greatly influence their behavior. As such, the most
important parameters conditioning extractor behavior will be presented first.
82 Chapler 3 SOLVENT EXTRACTION
EQUIPMENT

The same as for gas-liquid contactors, the important hydrodynamic param-

eters are involved, i.e phase hold up, interfacial area, transfer coefficients and
back mixing. In systems with two liquid phases, however, the physicochemical
properties of the phases have a much greater influence on these parameters
than in gas-liquid systems. This is related to the complexity of liquid-liquid
interface behavior. Fundamentally, it is essentially a matter of turbulence
appearing at the interfaces due t o gradients in interfacial tension, which in
turn are the result of gradients in concentration (Marangoni effect). The phe-
nomena can be classified into two types:
(1) Occurrence of interfacial convection currents. By modifying the turbu-
lence at the interface, these currents increase the transfer coefficients. Even
though the interface itself may be distorted by the currents, the influence of
these distortions on the interfacial area is usually negligible.
(2) Under certain conditions, and more particularly if the transfer fluxes
are significant, the interface distortions can take on the appearance of genuine
eruptions of the dispersed phase in the continuous phase. Here there is obvi-
ously an increase in interfacial area.
The significance of these phenomena depends on a number of factors,
among which the following:
the direction of mass transfer,
the sign of the gradient do/dC (normally negative),
the ratio of diffusivities in each phase,
the ratio between the viscosities of the two phases.
These phenomena therefore make the interpretation of experimental
results more complicated. Their significance is mainly appreciable when the
concentration gradients are high at the interfaces, i.e. when the droplets are
being formed. They usually accelerate transfer rates.
Nature of the continuous phase
An initial problem is t o identify the continuous phase. The choice is in fact
not totally free. As a general rule, the phase exhibiting the greater surface ten-
sion will tend to remain continuous. It is often the polar phase. Nevertheless,
above a certain ratio between phases, a phase inversion occurs. The critical
ratio depends on the system under study, in particular on the stirring inten-
sity, and there is a certain domain of uncertainty.
Hold up and interfacial area
Hold up and interfacial area are the essential hydrodynamic parameters
which need to be estimated. This is frequently possible if the average droplet
size and a characteristic relative velocity can be determined.
When phase motion is essentially due to gravity (column-shaped contac-
tor), the following continuity equation can be written:
 Chapter 3 SOLVENT EXTRACTION EQUIPMENT 83

with:
+ counter-current system
- cocurrent system
V, superficial velocity (m.s-*) of continuous and dispersed phases (sub-
scripts c and d respectively)
E hold up of one phase (c or d)
E, + Ed = 1
u, relative overall velocity of the two phases (positive in the direction in
which the dispersed phase circulates)
The relative velocity u, is related to the rising (or falling) velocity of a cloud
of drops in a continuous, infinite and immobile medium. This velocity depends
essentially on the physicochemical properties of the system and on the dis-
persed phase hold up. This intrinsic velocity of a cloud is called the charac-
teristic velocity of the system (ug) or the slip velocity:

u r = ug E c (3.2)
Experimentally, if hold up is measured for different values of V,, and Vsc, an
approximate value for ug can be obtained by plotting V,, + V,,Ed/(l - E,) ver-
sus ~ , ( l- E,) (Eqs. 3.1 and 3.2) on a graph.
A number of relations have been suggested to link u, and ug, all of which
have the following form:
u, = ug&;exp (a.~,) (3.3)
In the absence of any specific experimental data, R = 1 and a = 0 can be
used as a rough approximation to obtain:

Between the interfacial areaA (m2/m3),the hold up E , and the average drop
diameter d, (m), the following relation is approximately valid:

Ed
A= (3.5)
d B

If correlations to estimate ug and dBare available, A can then be determined

since E, is given by Eq. 3.4.
The same as for gas-liquid contactors, the droplet size depends on the dis-
sipated energy and the physicochemical properties. However, Eq. 3.5 remains
valid in principle. The value of dBdepends largely on the fluid properties and
on the solute transfer direction. General correlations can therefore not be
expected and only approximate values can be given.
The coalescing tendency is one of the prime characteristics and deter-
mines the numerical values of interfacial area. Since coalescence phenomena
are still not understood very well, the estimating methods found in the litera-
84 ChaDter 3 SOLVENT EXTRACTION EQUIPMENT

ture can give only an approximate value. The presence of small amounts of sur-
factants sometimes increases t h e interfacial area significantly by reducing the
average drop size and inhibiting drop coalescence.
An important phenomenon that limits extractor performance is flooding,
which may or may not be related to phase inversion. Flooding can be defined
as when the velocity of the dispersed phase approaching zero, with hold up
then reaching an extreme value. Accordingly:

Combining Eqs. 3.1, 3.3 and 3.6, the result for n = 1:

with the subscript E corresponding to flooding conditions.

Another limitation on flow rates in an extraction column comes from the
entrainment of dispersed phase drops by the continuous phase.
Figure 3.1, developed by Misek (1974), attempts to gather these different
constraints together in the same graph. The ratio Vsd/Vsc is generally dictated
by the extraction process and the physical properties of the phases set an
upper limit for E ~ It. is usually recommended to have the extractor work well
below this limit, sometimes at 50% of flooding if experimental data are not pre-
cise. Recently a general correlation was developed t o calculate phase hold up
in the different extraction columns (Kumar et al., 1995).
Back mixing
The detrimental influence of back mixing on column performance is well
known. When extraction columns are designed, the models used are usually of
the “plug flow with turbulent axial diffusion” type. The flow must therefore be
characterized by a Peclet number. Despite the somewhat succinct nature of
this description, it is often sufficient.
Mass transfer coefficients
The mass transfers between two liquid phases are traditionally described
using the concept of resistances located in two zones or films either side of the
interface. The overall resistance to transfer is thus the sum of the two resis-
tances, located respectively in the dispersed and in the continuous phase.

3.2 Different m e s of Extractors

The different extractors available can be classified on the basis of whether
mechanical energy is added to the system or not in order to promote disper-
sion or accelerate settling.
 Chaoter 3. SOLVENT EXTRACTION EDUIPMENT 85

Flooding limits
-2 -1 0 a= 1 2

10

VSd1
VSC

0.5

0.2

-
0.1
0 0.1 0.2 0.3
E ~ dispersed
: phase fraction
Phase inversion
range

Figure
3.1 Graph showing the operating range of a counter-current extractor.

1. No contribution of outside energy:

spray tower
baffle column
sieve plate tower
packed tower.
2. Contribution of outside energy:
mixer settler
tower with rotating agitators
pulsed column
centrifugal extractor.

3.2.1 Extractors without Outside Energy Contribution

3.2.1.1 Spray Tower
This is a simple pipe with a liquid inlet and outlet as shown schematically in
Figure 3.2. The column is partially filled with a liquid (continuous phase) and
86 Chapter 3 SOLVENT
EXTRACTION EQUIPMENT

the other liquid passes through it in the form of drops (dispersed phase). The
drops come together in a homogeneous layer, separated from the continuous
phase by an interface. Depending on the position of the interface - at the top,
bottom or in the middle of the column -the light or the heavy phase can be
dispersed over the whole column or part of it.

Heavy Light
phase b phase
I

Light 11 Heavy

I phase phase

The mass transfer occurring in such a column is the result of two pro-
cesses:
extraction during drop formation and coalescence,
extraction during drop movement.
It is recommended for the column to be wider near the dispersed phase
inlet in order to keep the drops from coalescing prematurely. The extra width
must be such that the flow velocity of the continuous phase in the widened
section ranges between 20 and 90% of its value in the part with a normal cross-
sectional area.
The mass transfer occurring during drop formation and coalescence is
known to be substantial. Since formation and coalescence take place only at
the ends of the column, the low efficiency of these extractors is only logical
 Chapter 3 SOLVENT EXTRACTION EOUIPMENT 87

(especially tall columns) and the use of devices to redistribute the dispersed
phase is justified. Axial back mixing, which can be considerable, also tends to
reduce efficiency.
Even though spray towers are moderately efficient, simple, low cost and
capable of processing large amounts of products, they are used mainly for
easy separations.
In order to size a column it is necessary to obtain laboratory data on flood-
ing with the physical system under consideration. The boundary value of V,,
can be measured by experiments carried out in a small columns with flow rate
ratios corresponding to the planned extraction operation range. Then the col-
umn diameter can be estimated, using a margin as indicated earlier.
Dispersed phase drops must be formed by means of a multi-orifice distrib-
utor (pipe or perforated plate), distributing the drops over the whole column
cross-section. The orifice diameter and number are determined on the basis of
a critical velocity at the orifice outlet such that the stream breaks up into small
droplets.
For systems with an aqueous continuous phase, this critical velocity is cal-
culated from the equation below:

with:
d, the orifice diameter (m)
pd the dispersed phase density (kg/m3)
(Jthe interfacial tension (N/m)
The average drop diameter can then be estimated by the following relation:

d32
(3.9)
dN

with EO and We being the Eotvos and Weber numbers under orifice conditions,
i.e.:

with V, being the velocity through the orifice (m/s).

There can be two operating regimes depending on whether the dispersed
phase occupies a small or a large fraction of the column:
loose packing,
dense packing.
Correlations can be found in the literature that allow the hold up Ed and the
slip velocity u, to be calculated for each regime and the flooding conditions to
be determined (Kumar and Hartland, 1994).
88 Chapter 3 SOLVENT
EXTRACTION EQUIPMENT

3.2.1.2 Baffle Column

These are vertical columns equipped with screens laid out in a baffle pattern
designed to increase liquid turbulence. The screens may be of a variety of
shapes (Fig. 3.3). The contact between phases occurs essentially in the form
of films (under or on the screens) and in the form of drops (between two baf-
fles). The between-screen spacing ordinarily varies between 10 and 15 cm.
Despite their low efficiency (0.05 to 0.1 theoretical stage per baffle), these tow-
ers are often employed due to their simplicity and easy use to process a vari-
ety of products with a wide range of flow rates.

Figure
3.3 Diagram o f baffletowers.
A. Circular baffles. B. Sectoral baffle with linear downcomer.

3.2.1.3 Sieve=PlateTower
These columns are similar to the ones used in distillation as described earlier.
Here the dispersed phase is redistributed at several levels by passing through
perforated plates which are generally equipped with downcomers to facilitate
the continuous phase flow (Fig. 3.4). The same a s in distillation columns, one
or more downcomers can be incorporated, either circular or linear like the
chord of a circle. They can also operate without any downcomer.
The dispersed phase accumulates on or under each plate until sufficient
hydrostatic pressure is reached to allow the liquid to pass through the holes
 Chapter 3 SOLVENT EXTRACTION EQUIPMENT 89

Sieve tray

Diagram of a column
with sieve plates and I Coalescence
downcorners.

in the plate. The liquid streams formed in this way break up into droplets
which recoalesce on the following plate. The material making up the shell and
especially the plate must be preferentially wetted by the continuous phase.
Ordinarily, the plate spacing (Zp) varies between 0.10 and 0.50 m or more
and the hole diameter ranges from 2 to 10 mm. The perforated area is approx-
imately 5 to 25% of plates with a downcomer. Columns containing some twenty
plates are common with a column diameter of up to 4 m. The specific flow
rates can reach 70 m3/(m2.h).
These columns are well suited t o systems exhibiting the following physical
characteristics: Ap > 100 kg/m3 and o > 0.005 N/m. The average drop size is
approximately 2.5 to 4 mm, and velocities in the orifices range from 15 to
50 cm/s.
The pressure drop through the plate can be assessed from the equation:

il: ]’
[ -
ApI = 0.5 1 - +:
x pd x LI3.2 (3.10)

with:

Re,= -
uNdN Pd Reynolds number in an orifice with a diameter dN
pd

C(d viscosity of the dispersed phase (Pas)

The pressure drop in the downcomer is expressed by:
Ap2 = 2.47 x pc U& (3.1 1)
90 Chapter 3 SOLVENT EXTRACTION EQUIPMEN7

with ucDbeing the linear velocity of the continuous phase in the downcomer.
This velocity must be lower than the terminal velocity of fine droplets of
approximately 1 mm in diameter.
The thickness of the coalesced dispersed phase layer under the plate can
then be calculated by means of a hydrostatic balance around the plate.
Proper plate operation is characterized by the reduced phase velocities:

(3.12)

that must range between 0.4 and 0.8.

Qiis the flow rate of one phase and S the total column cross-section.
The overall plate efficiency can be estimated by means of the following
expression (Green et al., 1984):

(3.13)

Sieve-plate columns are widely used industrially because of their good effi-
ciency (0.6 to 0.9 theoretical stage per plate, for high flow rates) and large
capacity. They are used for example in processing lubricants.

3.2.1.4 Packed Tower

Here again the columns are similar t o those described for distillation (see
Chapter 2). A wide variety of packings are used, either random or structured
and made of ceramic or plastic.
For gas-liquid contact like in distillation or absorption, a film of liquid runs
down the packing elements, providing a large interfacial area for transfer. In
liquid-liquid extraction, the packing is usually preferentially wetted by the con-
tinuous phase and the dispersed phase flows in the form of droplets.
Accordingly, the function of the packing is to prevent continuous phase back
mixing rather than to provide interfacial area directly. As a result, packing per-
formance in liquid-liquid extraction differs little from one type to another
regardless of the shape.
The same as for gas-liquid operations, the concept of flooding is very
important, and the phenomenon is closely related to packing size. Moreover,
there is a critical packing size under which droplets tend to coalesce and slow
down. The critical size (dPJ is calculated from the following equation:

EO = d2,lXAPxg = 0.85 (3.14)

0
with:
0 interfacial tension
Ap difference in density between the phases
g acceleration of gravity
EO Eotvos number
 Chapter 3 SOLVENT EXTRACTION EQUIPMENT 91

It is recommended to select a packing size greater than d,, and such that
the ratio (column diameter/packing size) is greater than 8. Flooding is the
phenomenon that limits the capacity of these columns and it is important to
predict the conditions under which it occurs. A number of correlations have
been developed, among which the following can be mentioned (Godfrey, 1994):

1 + 0.835 (e) (< 0.25 V

= C, v& (z)
[( x) A, p F2 5 r ' 2 5
0°.25 (3.15)

The constant C, depends on the packing and is calculated as follows:

(3.16)

where a, b and c are three constants characteristic of the packing and given in
the table below:

Packing a b C

Raschig rings 1.21 0.006 8 0.043

Berl saddles 1.65 0.78 0.035
Lessing rings 1.42 0.006 8 0.043
Spheres 1.32 0.006 8 0.043

For the values of E, and A,, refer to Chapter 2 on packed columns.

The capacity of this type of column, expressed a s the sum of the flow rates
of the two phases, is approximately 30 m3/m2.h. The use of structured pack-
ings, such as those proposed by Sulzer, allows higher capacities (100 m3/m2.h)
to be achieved. The columns can be used only if Ap is greater than 150 kg/m3
and with interfacial tensions ranging between 0.005 and 0.015 N/m.
The efficiency of this type of extractor is quite variable and difficult to pre-
dict by means of correlations, since HETPs vary from 1 to 3 m. To improve the
efficiency of large diameter columns, zones without packing are incorporated
along with redistributors spaced 3 to 4 m apart. Packing heights of 6 to 15 m
are commonly employed. Note that the efficiency of these columns, usually
ranging from 2 to 4 stages, increases with the flow rate of products being pro-
cessed.
Due to their simplicity and low cost, packed columns have various appli-
cations in refineries, e.g.:

extraction of oil products, lubricants in particular, by furfural or SOz,

sweetening of petroleum cuts (gasolines, kerosine).
92 Chaoler 3 SOLVENT EXTRACTION EQUIPMENT

3.2.2 Extractors with Outside Energy Contribution

Added mechanical energy can be used in two different ways:
To maintain dispersion or redistribute the dispersed phase. This type of
extractor is increasingly frequently used a s it achieves high efficiencies.
To help carry out settling.

3.2.2.1 Mixer-Settler
This is the simplest type of extractor imaginable. The advantage is that it dis-
sociates the dispersion and settling steps, each of which requires conditions
opposite to the other. As such, the phases are mixed and dispersed in one ele-
ment and settling occurs in another one.
If the extractor works batch-wise, the mixing and settling can be performed
in the same vessel. In continuous processes, two vessels are necessary, one to
mix the phases (see Chapter 9 on mixers) and the other for the phases to sep-
arate out. The settler is a simple vessel, sometimes equipped with packing or
baffles. It must be wide enough to allow emulsions to break up. Figure 3.5
shows a series of mixer-settlers operating counter-currently. In order t o mini-
mize the number of pumps required, most industrial equipment attempts to
combine mixing and pumping of the phases. Figure 3.6 shows a close-up of this
type of system (Denver design) with two turbines on the same axis.
It is necessary to supply a certain amount of energy during mixing in order
to disperse the phases properly (Treybal, 1961). The traditional rotating agita-
tor correlations allow the amount of required energy to be evaluated. The
greater the energy supplied, the more the extraction efficiency approaches 1.
The difficulty resides in the fact that if the mixing is done too vigorously, an
emulsion may be created that is hard to settle out. As a result, experimental
data on settling times are necessary in order to size the settler, which is most
often the limiting element.

Light -Heavy
phase phase

Heavy L
,giht
phase phase

Settling Mixing zone

zone

Figure
3.5 Diagram of a battery of countercurrent flow mixer-settlers.
 Chapter 3 SOLVENT EXTRACTION EQUIPMENT 93

Heavy
phase 1-

Figure
3.6 Close-up of a mixing cell that also pumps the heavy phase.

The results obtained with industrial equipment show that an element

(mixer-settler) has an efficiency ranging from 0.80 to 0.95 of a theoretical stage.
The chief drawbacks of these extractors are the floor space they occupy, the
numerous mechanical parts they include and their large dead volume. Usually
made up of 4 to 10 stages, they are used in the mining and nuclear industries
(extracting ore, processing nuclear fuels). In the oil industry, sulfuric acid pro-
cesses (extraction of isobutene or alkylation of paraffins) employ the same
concept in an appropriate form (see Chapter 7 on reactors).

3.2.2.2 Column with Rotating Agitators

There are different versions of columns with rotating agitators, but their gen-
eral principle remains the same. Agitation is provided by a central shaft with
discs mounted on it (rotating disc contactor: RDC) or by agitators with blades
(Oldshue-Rushton, Scheibel, Kuhni). The mixing cells are separated by a
restriction designed to curb back mixing. It can consist of a baffle with a cen-
tral opening (RDC, Oldshue-Rushton, Scheibel2), a perforated plate (Kuhni) or
packing (Scheibel 1). Some constructors have attempted to make the segmen-
tation more efficient by directing the product mixture streams from the central
agitator (Kuhni, Scheibel 2). All these extractors allow a large number of theo-
retical stages in the same column. The most common type in the oil industry
is the RDC, used in particular in deasphalting and in furfural treatment of lubri-
cants (see Vol. 3).
94 Chapter 3 SOLVENT EXTRACTION EQUIPMENT

a . Rotating Disc Contactor 0 9

This is a column divided up into compartments partially closed by annular baf-
fles (Fig. 3.7). In the middle of each compartment, there is a solid rotating disc.
The solid discs are mounted on the same shaft and their diameter is slightly
smaller that the diameter of the opening in the stationary annular baffles. This
therefore facilitates installation operations appreciably.

Driver

Heavy
phase
inlet

Heavy
phase

Figure
3.7 Diagram o f a rotating disc contactor (ROC) with a close-up o f one stage and
identification of the main dimensions.
 Chapter 3 SOLVENT EXTRACTION EQUIPMENT 95

The characteristic dimensions are given in Figure 3.7 and the following ratios
are recommended:
DcJD, = 0.7-0.8 DRJD, = 0.45-0.625 H,/D, = 0.1 to 0.3
Correlations have been established linking the fraction of dispersed phase
and the slip velocity to operating variables (Godfrey et al., 1994). This allows
the flooding conditions to be calculated and the operating conditions to be
set: generally at 65% of flooding. The disc rotation speed, NR, is an important
variable, the energy dissipated and flooding depend on it.
As indicated in Chapter 9 on mixing systems, the power absorbed by an
impeller rotating in a liquid phase can be correlated by means of a dimension-
less number, the power number, which depends on the Reynolds number of
the impeller and under certain conditions on the Froude number. This function
obviously depends on the geometry of the system. This holds true for an RDC.

(3.17)

with:
NR rotation speed of the impeller in rps
D, disc diameter
p, mixture density

',=C ' ( ';,":;:)

Ed
I+- apparent viscosity of the mixture

Pc power dissipated in a compartment

The total absorbed power will therefore be equal to N,P,, where N, is the
number of compartments.
This type of column can accommodate high flow rates, up to 40 m3/m2.h,
for diameters of up to 8 m. The efficiency of a stage depends on the phases and
decreases when the size increases, e.g. approximately 0.3 for furfural extrac-
tion of lubricants in a column 3 m in diameter.
One version of the RDC features partial settling of the phases at each stage,
which allows mutual entrainment of the phases and axial mixing to be reduced
(ARDC: asymmetric rotating disc contactor) (Fig. 3.8). It can be employed for
systems whose density difference is smaller (Ap > 10 kg/m3, whereas Ap >
50 kg/m3 is recommended for the RDC). In contrast, the capacity is smaller:
20 m3/m2.h,while efficiency may reach 3 theoretical stages per meter.

b. Column with Agitated Compartments

Only the major ones will be mentioned:
Scheibel column (Fig. 3.9). Mixing is performed by an impeller with four
blades and conventional baffles. The compartments are separated by metal
mesh padding or by areas filled with packing. The height of the settling zone
is approximately three times that of the mixing zone. Another version is
96 Chapter 3 SOLVENT EXTRACTION EOUlPMEN7

Flow path of phases

Cutaway view

-
Figure
3.8 Diagram of a column with asymmetric rotating discs (ARDC).

Mixing zone Diagram of a Scheibel

type extraction column.
Settling zone

equipped with horizontal circular baffles surrounding the impeller. Efficiency

is from 3 to 5 theoretical plates per meter.

Oldshue-Rushton column (Fig. 3.10). Similar to the RDC, but the discs
are replaced by a standard Rushton turbine with 6 flat blades mounted on a
disc. The height of a compartment is roughly equal t o the diameter of the col-
umn. Efficiency is from 1 t o 3 theoretical plates per meter if the passage
between the compartments is narrowed down and only 0.8 t o 1 theoretical
plate per meter if the passage is wider. This type of column is marketed by
Lightnin.
 Chapter 3 SOLVENT EXTRACTION ECJUIPMENJ 97

Diagram of an
Oldshue-Rushtontype
of extraction column.
1
Figure

3.10
1

-Light
phase

Heavy
phase

Kuhni column (Fig. 3.1 1). The compartments, separated by perforated

discs, are agitated by centrifugal turbines somewhat similar to pump rotors.
The degree of between-compartment disc perforation is adjusted depending
on the physicochemical properties of the system. The compartment height
varies with the column diameter: approximately 10 cm for 1 m of diameter. The
rotation speed is an important control parameter. These columns are built in
diameters of up to 3 m, the maximum flow rate is 50 m3/m2.h,and efficiencies
can go up to 10 theoretical plates per meter.
The power required for agitation in all these columns is calculated in the
same way as for the RDC (Eq. 3.17), with the power number adapted to the type
of turbine used. For Scheibel and Oldshue columns, Np is approximately 1.85.
Some columns are actually a series of vertically stacked mixer-settlers,
thereby allowing the extractor to occupy less floor space. Lurgi uses a column
of this type for its Arosolvan aromatics extraction process. In this column
(Fig. 3.12), the settlers occupy almost all the cross-section and the two phases
pass from one stage to another via an outside transfer pipe.

3.2.2.3 Pulsed Columns

Liquid turbulence in a column can be increased by generating pulsations in
addition to the normal phase flow rates. The mechanical pulsing device (bel-
lows, pump without check valves or gas pressure) can be incorporated in an
existing packed column or may be part of a specially designed extractor such
as a sieve tray column without downcomers (Fig. 3.13).
98 Chapfer 3 SOLVENT EXJRACTION EQUIPMENT

------- /
Disc-shaped
baffles

,
Flat-bladed
-_----- turbine

1 Figuire
3.1 1 1IDiagram of a Kiihni type extraction column.

Figure
3.12 Simplified diagram of the Lurgi column.
 Chapter 3 SOLVENT EXTRACTION EQUIPMENT 99

Light

Pulsing
device

Figure
3.13 Diagram o f a pulsed column with perforated trays and pulsations generated by
compressed air.

Packed pulsed columns can utilize any type of random or structured pack-
ing. Packing size and type are chosen the same as for an ordinary packed col-
umn (see Chapter 2). The optimum capacity is approximately 20 m3/m2.h.The
difference in phase density must be greater than 80 kg/m3. Efficiency varies
between 4 and 8 theoretical stages per meter depending on the flow rates, for
amplitude values of between 6 and 10 mm and a frequency ranging between 1
and 2.5 s-I.
100 Chaoter 3 SOLVENT EXTRACTION EQUIPMENT

Plate columns ordinarily include plates spaced from 5 to 15 cm apart, per-

forated with holes of 2 t o 6 mm in diameter and the perforated surface area
varies from 5 to 40%. It is recommended to vary the perforated surface area
according to the interfacial tension of the system: 5% for high values and 40%
for low ones. Commonly employed pulsations correspond t o frequencies vary-
ing between 0.5 and 2.5 s-l and amplitudes from 5 to 15 mm (often a value of
8 mm has proved to be optimum). This type of column can reach a diameter
of 2.5 m. Performance is usually expressed as a function of the product of
amplitude x frequency (af), with a good operating range corresponding t o (af)
between 0.8 and 2 cm/s. Capacities can reach 60 m3/rn2.h.Efficiency increases
when the hole diameter decreases.
These extractors offer the following advantages:
High efficiency due to the increased turbulence and contact area between
the phases.
Great flexibility of operation because of additional operating variables
(amplitude and frequency) that can be adjusted to modify column per-
formance. This makes it easier to scale up results for the construction of
large columns.
The possibility of processing fluids loaded with fine solids.
Great mechanical simplicity and ease of use which is of critical impor-
tance in the nuclear industry where moving mechanical parts must be
eliminated in active cells.
The chief drawbacks are:
Capacity is limited. Flow rates are lowered by the increased resistance to
flow due to greater agitation. Plate columns have satisfactory capacities,
much greater than packed columns.
Pulsations of the liquid tend to favor emulsion formation.
The effects of axial mixing (back mixing) are severe enough to hinder the
counter-current operation of the extractor and consequently decrease its
efficiency.
Energy consumption is relatively high.
Another pulsed column design has been developed: the reciprocating-plate
column (Fig. 3.14). Here the plates can be equipped with a weir. The drawback
of this type of column is the presence of moving internal parts. Some industrial
examples can be found, mainly in petrochemistry, where columns 1.2 m in
diameter have been built.
These extractors should not be compared to towers that process enor-
mous amounts of products without a very high degree of extraction. Pulsed
columns are very effective mainly in implementing difficult separations. They
have found their principle application in the nuclear energy industry (refining
uranium, reprocessing nuclear fuels) and also in petrochemistry.
 Chapter 3 SOLVENT EXTRACTION EQUIPMENT 101

Figure Reciprocating
Principle o f a reciprocating- sieve plates
plate column.

3.2.2.4 Phase Separation by Centrifugal Force

Centrifugal extractors may be advantageous for systems with a small differ-
ence in density or a pronounced tendency to form emulsions. There are dif-
ferent types, with the most well known being undoubtedly the Podbielniak
extractor, where extraction takes place in a high-speed rotor (1000 to
5000 rpm). The rotor features a series of concentric cylinders connected to
each other by holes in a staggered pattern (Fig. 3.15). The heavy liquid is intro-
duced in the center while the light solution is injected at the circumference.
The centrifugal force causes radial counter-current phase flow, with the pro-
cessed light phase collected in the center and the processed heavy phase
recovered at the vessel periphery.

Figure
3.15 Simplified diagram of a “Podbielniak”type centrifugal extractor.
102 Chapter 3 SOLVENT EXTRACTION EQUIPMENT

The chief advantages of this extractor are:

Good efficiency and relatively great operating flexibility: 3 to 5 stages per
extractor, with a range of flow rates going from 0.3 to 130 m3/h.
Little hold up and steady state conditions are reached rapidly.
Very compact machine, allowing space and piping savings.
However, the drawbacks are its high price and running costs.
Luwesta extractors achieve what is actually a stack of mixer-settlers rotat-
ing at a speed of 4400 to 6500 rpm. Capacity varies from 1.25 to 120 m3/h.
Based on the same principle (axial counter-current), the SGN-Robatel extrac-
tor is built today with up to 7 stages (Fig. 3.16).
These various types of extractors have found particular applications, such
as in preparing pharmaceuticals (antibiotics, vitamins) and processing nuclear
fuels.

I I
I I
Driver

Stationary external wall

‘Y Light phase charnGer

Heavy phase outlet inlet

Figure
3.16 Diagram of a “Robatel”extractor.

3.3 Conclusion
There is a wide variety of extractors available for a liquid-liquid extraction
operation. Nevertheless, each type has characteristics and qualities that are
specific to it and equipment must be chosen on the basis of a number of cri-
teria that are specific to each application.
 Chapter 3. SOLVENT EXTRACTION EOUIPMENT 103

I I Selection criteria I
Type of extractor Phase
Capacity Number Flexibility
separation of stages

Spray 3
Baffle 3
Sieve plate 3 2 2
Packed 3
Mixer-settler 1
RDC, ARD 3
Agitated compartments 2
Pulsed plate 2
Pulsed packing 1 1
Centrifuge 4 2

__
Table
3.1 Selection criteria for a liquid-liquid extractor.

The four main criteria that can be mentioned are:

Capability of separating phases under difficult conditions, such as a
small difference in phase densities or ready emulsification.
Separation efficiency or the number of theoretical stages that can easily
be implemented.
Capacity, i.e. total volume of phases that can be processed.
Flexibility, i.e. capability of maintaining performance if the feed flow rate
varies.
Table 3.1 gives an indication of the behavior of each type of extractor that
has been discussed with respect to the selection criteria mentioned above.
The final choice will also obviously have to take into account the investment
and maintenance costs, which vary appreciably from one type to another.

References
Godfrey J.C., Slater M.J. (1994)Liquid-LiquidExtraction Equipment. John Wiley &
Sons.
Green D.W., Maloney J.O. (1984) Perry’s Chemical Engineers’ Handbook, 6th
Edn. McGraw-Hill Book Co.
Heimfort H. (1984) Separators, Documentation of Wesphalia Separator.
104 Chapter 3 SOLVENT EXTRACTION EOUtPMENT

Kumar A,, Hartland S. (1995) A unified correlation for the prediction of dis-
persed-phase hold-up in liquid-liquid extraction columns. I & EC Research 34,
11, 3925-3940.
Misek T. (1974) Int. Chem. Eng. 14, 107.
Robatel (1997) Batterie d’Extracteurs Centrifuges, Notice BXP.
Sattler K., Feindt H.J. (1995) Thermal Separation Processes. VCH Publishers.
Treybal R.E. (1961) Stirred tanks and mixers for liquid extraction. Ind. Eng.
Chem. 53, 8, 597-606.