MASS TRANSFER Nandana Chakinala

CONTINUOUS COUNTER CURRENT EXTRACTION

WITH REFLUX
Extract is further enriched with
solute C using reflux
Raffinate section of cascade does
not change and all the principles of
counter current extraction applies
Extract section is changed as reflux
is provided
Reflux provided by removing the
solvent from extract E1 to produce
solvent free stream (E’), part of
which is removed as product PE and
part returned as reflux
DESIGN-SOLVENT FREE BASIS, EXTRACT ENRICHING SECTION
Balance over A+C at solvent separator:
∆ represents the net rate of flow outwards from this section, So
for A+ C : ∆E’ = PE’ and for its C content X∆E = XPE
For its B content BE = ∆E’ N∆E
Balance (A+C) over all stages until e:
where ∆’E represents a difference point whose co-od are (net
concentration of B flowing out, net concentration of C flowing
out) (N∆E, X∆E )
Net B flowing out = B out/(A+C) out
Net C flowing out = C out/(A+C) out
Solute (C) and solvent (B) balance equations (all stages until e)
can also be written based on solvent free basis
Internal reflux ratio at any stage

External reflux ratio

If Solvent is pure B, then this diagram is

analogous to H-x-y Diagram of distillation
EXTRACTION EQUIPMENT
Bringing two immiscible or partially miscible liquid phases into intimate contact
Creating conditions for effective mass transfer
Separation of two liquid phases
Recovery of solute from the extract
Recovery of solvent from both the phases
DIFFERENCES IN EXTRACTION AND DISTILLATION EQUIPMENT

1. Dispersing one liquid in other is more difficult than dispersing gas/vapour in liquid
2. Viscosity of gas is smaller compared to liquid, which causes high bubble rise velocity, thus
creating turbulence, rapid bubble breakage and coalescence and a large interfacial area
3. Density differences between L-L smaller compared to G/V-L. Hence difficult to separate
two clear liquid layers
4. Substantially higher mechanical energy per unit volume of medium is required to create L-
L dispersion
For all the reasons above, design and construction features of extraction equipment is
different from distillation/absorption columns
EXTRACTION EQUIPMENT
Equipment similar to that used for distillation, absorption and stripping can be
inefficient unless the liquid viscosities are low and differences in phase densities high

Dispersion carried out by mechanical agitation

Phase separation carried out either by gravity or centrifugal force on the two phases
CLASSIFICATION OF EXTRACTORS
Stage wise contactors: Equipment consists of single stage or a series of stages in
which phases are mixed and separated
Differential contactors: Equipment in which phases are continuously brought into
contact and phase separation takes place only at the exit of equipment
CLASSIFICATION OF EXTRACTORS
CHARACTERISTICS OF COMMON EXTRACTORS
 PULSED COLUMN
Reciprocating pump is used to create pulses of short
amplitude that are superimposed on the usual flow of the
liquid phases
Low axial mixing
No moving parts, suitable for corrosive liquids
CONTACTOR SELECTION
 PHASE DISPERSION BY MECHANICAL AGITATION-STAGE
WISE CONTACT
I. Mixer settler
Mixer for contacting two liquids and settler for separating two
phases. In batch processes, same tank acts as both
For continuous operations, the vessel is first filled with liquid
intended to be continuous and with agitation in progress, both
liquids are introduced in desired ratio
Different types of impeller used
Drop sizes: 0.1 to 1 mm
Preliminary estimate of settler diameter

Application: Extraction of uranium salts or copper salts

from aqueous solution
PHASE DISPERSION BY MECHANICAL AGITATION-STAGE
WISE CONTACT
Settler
Dispersion leaves mixer almost like emulsion
Coalescence of liquid droplets required to be separated in to two
liquid phases
Higher interfacial tension between the liquids enhances the
coalescence rate
To improve separation efficiency and to reduce holding times, and
volume of settler, settling aids are used
Advantages
 High stage efficiency, operational flexibility, scale up with more reliability, can
handle high viscous liquids

Disadvantages
 Considerable pump and piping costs, larger floor area, more solvent cost as
larger volumes retained in settling vessels
II. ROTARY AGITATED EXTRACTION - SCHEIBEL EXTRACTOR
PHASE DISPERSION BY MECHANICAL AGITATION - DIFFERENTIAL
CONTACT
I. Rotating Disc Contactor
 PHASE DISPERSION BY GRAVITY – STAGE WISE

I. Perforated plate column

Tray efficiency

0.352𝑇 0.5 0.42

𝐸𝑜 = 𝑉𝐷 /𝑉𝐶
𝜎𝑑𝑜0.35
VD and VC superficial velocities
do hole diameter
T tray spacing
 PHASE DISPERSION BY GRAVITY – DIFFERENTIAL
CONTACT
Heavy liquid enters the top and fills as
I. Spray column continuous phase
Light liquid through distributor nozzle causes
dispersion
Light liquid coalesces as it flows to the top
In some cases, heavy liquid is sprayed
downward in to rising light liquid phase
PHASE DISPERSION BY GRAVITY – DIFFERENTIAL
CONTACT
II. Packed column
Packed tower is more effective, causing droplets to coalesce and redisperse at frequent
intervals through out the tower
Tower is filled with heavy liquid, which largely occupies the void spaces between
packings
The remaining void space is then filled with dispersed light liquid
The dispersed phase should not preferentially wet the packing since interface is smaller
Application: Removal of aromatics from naphtha
PHASE DISPERSION BY PULSATION – STAGE WISE
I. Perforated Plate Pulsed Column
Perforated plates without the downcomers
Pulsations generated by a reciprocating
device force alternately light and heavy liquid
through perforations
Can be done in packed towers as well
Effective in small sizes

Application: Processing Radioactive solutions

IMPORTANT PARAMETERS IN AGITATED LIQUID
DISPERSIONS
Drop size Applicable for packed towers

Impeller power requirement

Mass transfer coefficient

MASS TRANSFER COEFFICIENT
Dispersed phase mass transfer coefficient (Assume drop to be rigid if smaller than 1
mm and interfacial tension > 15 dyne/cm)

Continuous phase mass transfer coefficients

If solute distribution in two phases follows linear relationship

MASS TRANSFER IN L-L DISPERSION
Two important factors of mass transfer between bubble
and surrounding liquid
1. Internal circulation
• Shear stress at the interface gives rise to internal circulation

2. Marangoni effect
• Due to interfacial tension gradient created by
differences in solute concentrations/temperatures
DESIGN OF PACKED EXTRACTION COLUMNS

Packed columns are used when few stages are required and when interfacial tension
of about 10 dyne/cm
Flooding occurs when increasing the dispersed or continuous flow rates causes both
phases to leave at the outlet of the continuous phase
Diameter of packed tower calculated from flooding correlation. Normally 50% of
flooding velocities are used.
PACKED TOWERS
Change in concentration of either liquid is
differential
Transfer of solute from one phase to other phase
causes change in mutual solubility of the
contacted liquids, in general all components of
system transfer from one phase to other
Mass transfer correlations are poorly develop in
LLE. Hence, correlations of gas absorption taken
as first estimate.
Consider solute is transferred from feed to extract
phase and both the solvents are insoluble
All correlations of gas absorption apply in in this
case
 PACKED TOWERS
All correlations of gas absorption apply in in this
case
CRAWFORD AND WILKE CORRELATION
0.2 1.5
𝜎 𝜇𝑐 𝑎
𝜌𝐶 ∆𝜌 𝜀

𝑉𝐶0.5 + 𝑉𝐷0.5 𝜌𝐶
𝑎𝜇𝐶
BACK UP
FRACTIONAL EXTRACTION
Applies if two solutes has to be extracted using different solvent

Feed containing two solutes B and C extracted using two solvents A and D flowing
counter currently
Based on distribution coefficients, B is extracted in to solvent A and C is extracted in
to solvent D