05-02-2021

Mass Transfer II
Prepared by
Dr. Krushna Prasad Shadangi
Assistant Professor
Department of Chemical Engineering
Veer Surendra Sai University of Technology, Burla, Odisha. India

Course
• Objective
• To study the principles and applications of drying of
solids in chemical industries
• To study the principles and applications of adsorption
techniques
• To study the fundamental principles and application of
liquid-liquid extraction techniques
• To study the fundamental principles and application of
Solid-liquid extraction techniques
• To study the working principles of various mass
transfer equipment

1
 05-02-2021

Syllabus
• Module – I: Drying
Drying Equilibria, Drying rate curve, Batch and continuous drying.
Time of drying and calculations, mechanism of batch drying.
• Module – II: Adsorption
Theory of adsorption, Industrial absorbents, adsorption equilibria,
freundlich equation, single and multistage operations, Ion - Exchange.
• Module – III: Liquid - liquid Extraction
Introduction, liquid - liquid equilibria, analytical and graphical
solutions for single and multistage operations, continuous, counter current
operation without reflux, fractional extraction.
• Module – IV: Solid-Liquid Extraction
Operation of solid, steady and unsteady state operation, analytical
methods for single and multistage operations.
• Module – V: Mass Transfer Equipments
Drying equipment: Equipment for batch and continuous drying
operations. Adsorption equipment: Liquid-liquid extraction equipment: single
stage, multistage and continuous contacting equipment. Solid liquid
extraction equipment

Text Books:
• 1. R. E. Treybal, Mass Transfer Operations,
McGraw and Hills, 1980.
• 2. B. K. Dutta,Principles of Mass Transfer and
Separation Processes, PrenticeHall, 2005
• Reference Books:
• 1. W. L. McCabe &J. C. Smith, Unit
Operationof Chemical Engineering, McGraw&
Hills, 2005.

2
 05-02-2021

Course Outcomes:
• Students will learn the mechanism of drying
operations
• Understanding of fundamentals and
applications of adsorption and
chromatographic separation process
• Understanding of fundamentals of separation
of components by liquid-liquid extraction
• Understanding the principle of leaching
• Student will understand about working
principle of various mass transfer equipment

Module 1

Drying in Mass Transfer

3
 05-02-2021

Introduction
• Drying is an operation in which a liquid usually water is
removed from a wet solid in a equipment is termed as dryer.
• Drying does not mean only removal of the moisture but
during the process, physical structure as well as the
appearance
• Governed by the principles of transport of heat and mass
• The hot gases supplies the energy for drying
• Drying doesn’t ensure the complete removal of moisture
• The final product is solid from this process

Physical mechanism
• Drying is a diffusional process in which the transfer of moisture to the
surrounding medium takes place by the evaporation of surface moisture, as
soon as some of the surface moisture vaporizes, more moisture is
transported from interior of the solid to its surface.
• This transport of moisture within a solid takes place by a variety of
mechanisms depending upon the nature and type of the solid and its state of
aggregation.
• Mechanism of moisture transport
 transport by capillary force
 Vapour diffusion
 pressure induced transport

• Depends on the nature of the solid, its pore structure and the rate of drying.

4
 05-02-2021

Transport by capillary force

• For granular or porous solid the moisture

transport occurs due to the capillary force so long
as there is enough moisture in the bulk phase.
• Larger capillaries empty first
• Smaller capillary supplies the liquid continuously
to the surface
• The drying gas enters to the solid through the
cracking and occupied by the hot gas and
increases the drying rate

Pressure induced transport

• If the drying rate is high outer layer dries up first and contract
and there by generate a compressive force to squeeze out the
moisture from the interior

5
 05-02-2021

Vapour diffusion
• The water concentration near the surface decreases as drying
proceeds.
• This creates a driving force for water diffusion from the
medium to the exposed surface
• At low moisture content, drying generates pores and
vaporization occurs below the surface.
• The vapour produced is diffused out from the solid and the
process is known as. ..

Resistance in drying
• Due to

– Liquid or vapour transport inside the solid

– Convective mass transport of vapour from the surface of

the solid to the bulk of the gas

– Convective heat transfer from the bulk of the drying gas to

the solid surface

6
 05-02-2021

Fundamental terms
• Moisture content in dry basis: X
Weight of moisture per unit weight of bone dry substance = × 100 { }
• Moisture content in wet basis: x
Weight of moisture per unit weight of wet substance = × 100 { }
• Equilibrium moisture content: X*
At a particular temperature the moisture content of a solid that can remain in
equilibrium with the drying medium of a given relative humidity.
• Bound moisture content:
Moisture content of a substance which exerts as equilibrium vapor pressure less than
of the pure liquid at the same temperature is referred to as bound moisture.
• Unbound moisture content:
Moisture content of the solid which exerts an equilibrium vapor pressure equal to
that of pure liquid at the given temperature is the unbound moisture.
• Free moisture:
The moisture content of solid in excess of the equilibrium moisture content.
• Critical moisture content: at which the constant rate drying period ends and
the falling rate drying period starts

Moisture above the equilibrium moisture content

Moisture that can be removed by drying under the given % relative
humidity
X = Xt – X*

7
 05-02-2021

Drying rate curve

It gives a relationship between rate of drying ,
expressed as moisture evaporated per unit
time per unit area of drying surface and
moisture content on dry basis.
Constant drying condition:
The condition under which temperature,
humidity, velocity and direction of flow of
gas are constant during operation.
Critical moisture content:
The moisture content at which constant
rate period ends and falling rate period
starts means unsaturated drying of
surface starts is called as CMC.
First falling rate period:
The drying patches start. Rate of drying
decreases for unsaturated persons.
First falling rate period:
At second falling rate period the surface is
completely dry. Only internal movement
of moisture starts coming to the surface
till reaching the equilibrium moisture
content.

Change in moisture content with

drying

8
 05-02-2021

Factors affecting on drying rate

• Gas velocity: increases with the gas velocity

• Humidity of gas: lesser the humidity more the drying rate

• Area of drying: more with the area

• Temperature: more with temperature, decreases the relative

humidity, increases the driving force.

Drying rate curve

Liquid or vapor transport inside the solid

Convective mass transport of vapor
from the surface of the solid to the
bulk of the gas

Total drying time = tc + tf =

Time of drying at constant rate period
+ Time of drying at falling rate period

R is drying rate in kg moisture /h.m2

WS kg of bone-dry solid
A exposed surface area for drying in m2

9
 05-02-2021

Calculation of Drying time

• Constant rate period: [Xi, Xf > Xc]

• We know N= -
unbound moisture content is removed
=> ∫ 𝑑𝑡 = - ∫

=> t = (Xi - Xf)

𝑾𝒔
=> t = (Xi - Xc)
𝒂

Calculation of Drying time

• For Falling rate period: [Xi, X2 < Xc]

• t= ∫ 𝑑𝑡 = - ∫ Graphical method

The value of the integration can be obtained

by plotting X vs. 1/N and the area under the
graph will give the value

Analytical method

when N varies linearly with X, then the drying rate N = m (Xc – X*)
∗
- = 𝑚 (𝑋𝑐 − 𝑋 ) N= -

∗
- = ∗ 𝑋𝑐 − 𝑋
( )

×
∗ = dt
∗
∗ ∗
× 𝑿𝒄 𝑿 𝑾𝒔(𝑿𝒄 𝑿 )
=∫ ∗ = ∫ 𝑑𝑡 => tf = 𝐥𝐧
∗ 𝑿𝟐 𝑿∗ 𝑵× 𝒂

10
 05-02-2021

Total drying time

• t = tc + tf
∗ ∗
𝑾𝒔 𝑾𝒔(𝑿𝒄 𝑿 ) 𝑿𝒄 𝑿
• t=- (Xi - Xc) + 𝐥𝐧
𝒂 𝑵× 𝒂 𝑿𝟐 𝑿∗
•

Numericals

11
05-02-2021

12
05-02-2021

13
 05-02-2021

Classification of dryer

• Batch Type Dryers

– Tray Dryer
– Pan Dryer
– Agitated Vacuum Dryer
• Continuous Dryer
– Rotary Dryer
– Drum Dryer
– Flash Dryer
– Fluidized Bed Dryer
– Screen Conveyor Dryer

14
 05-02-2021

• NOVEL DRYING TECHNOLOGIES

• Microwave Drying
• Supercritical Fluid Extraction and its
application to Drying

Spray dryer

• Used in spray drying

• Can dry a product very quickly compared to
other methods

15
 05-02-2021

Spray dryer
• Spray drying is a method of producing a dry powder from a liquid or slurry
by rapidly drying with a hot gas.
• Spray drying is a one-step continuous unit operation that employs liquid
atomization to produce droplets that are dried to individual particles when
moved in a hot gaseous drying medium.
• A spray dryer consists of
– a feed pump, atomizer, air heater, air dispenser, drying chamber and systems
for exhaust air cleaning and powder recovery/separator.
• The three stages that occurs in a spray dryer before drying is accomplished
includes.
– Atomization
– Spray-air mixing and moisture evaporation.
– Dry product separation from the exit air.
• The nature of the final product obtained after drying in a spray dryer
depends on;
– The design and operation of the spray dryer.
– The physicochemical properties of the feed.

16
 05-02-2021

Uses of Spray dryer

• Spray dryer is used in drying pharmaceuticals like penicillin, blood products,
enzymes, vaccines etc.

• It is used in the production of excipient and co-processed excipient with increased

flow ability, compatibility and tablet disintegration.

• To improve drug compressibility and reduce capping tendencies in crystals.

• It is equally used in the preparation of matrix microcapsule containing drugs

substances and a biodegradable polymer in order to obtain controlled drug release
formulation.

• It is employed in enhancing solubility and dissolution rates of poorly soluble drugs

by formation of pharmaceutical complexes or via the development of solid
dispersion thus increasing bioavailability.

• It is used in the production of dry powder formulation/dry powder aerosol

Uses
• Chemical industries e.g. phenol-formaldehyde resin, catalysts, PVC emulsion type,
amino acids etc.
• Ceramic industries e.g. aluminium oxide, carbides, iron oxides, kaoline etc.
• Dye stuffs and pigments e.g. chrome yellow, food colour, titanium dioxide, paint
pigments etc.
• Fertilizer production e.g. nitrates, ammonium salts, phosphates etc.
• Detergent and surface active agents e.g. detergent enzymes, bleach powders,
emulsifying agents
• Food industries e.g. milk, whey, egg, soya protein etc.
• Fruits and vegetables e.g. banana, tomatoes, coconut milk etc.
• Beverage e.g. coffee, tea etc.
• Biochemical industries e.g. algea, fodder antibiotics, yeast extracts, enzymes etc.
• Environmental pollution control e.g. flue gas desulfurization, black liquor from
paper-making etc.

17
 05-02-2021

Advantages of Spray Dryers

• Product quality and properties can be effectively controlled and maintained
through the entire drying operation.
• Pharmaceutical can be dried at atmospheric pressure and low temperature.
• Spray dryer permits high- tonnage production in continuous operation and it is
relatively simple to operate.
• Feed stock in solution, slurry, emulsion, paste and melt form can be dried if
pumpable.
• Corrosion problem is minimal and the selection of materials of construction of
spray dryer is simplified since the dried material comes in contact with the
equipment surfaces in an anhydrous condition.

• Spray dryer produces dry powder particle of controllable particle size, shape, form,
moisture content and other specific properties irrespective of dryer capacity and
heat sensitivity.

• Spray dryer handles a wide range of production rate and provides extensive
flexibility in its design that is product specification are readily met through the
selection of appropriate spray dryer design and its operation from a wide range of
available design.
• It is an energy intensive equipment because;
– Specific heat of evaporation can be supplied in a short time.
– The temperature difference across the drying chamber is relatively small and
– An appreciable amount of heat is lost with exhaust air.

Disadvantages of spray dryers

• Spray dryer is bulky and also expensive to
install.
• It is difficult to clean after use.
• It has a low thermal efficiency that is a lot of
heat is wasted during operation.
• Solid materials cannot be dried using spray
dryers.
• Product degradation or fire hazard may result
from product deposit on the drying chamber.

18
 05-02-2021

Rotary Dryer
• The rotary dryer also known as tumbling dryer is an equipment
employed to minimize the moisture content of a feed material by
bringing it in direct contact with a heated gas.
• It consists of an inclined long drum or cylinderical shell often fitted
with internal flights or lifters; rotated slowly upon bearings through
which the material to be dried flow with a tumbling/cascading
action in concurrent (for heat sensitive materials) or counter-
current flow with the heating air or gases.
• The movement of the material is due to combined effect of
inclination of the shell to the horizontal and the internal tumbling
action or mechanical turn over thus the name tumbling dryer.
• The nature of the feed determines the directions of gas flow
through the cylinder and it is relative to the solid. This drying
equipment can also perform batch or continuous processing of the
wet feed.

19
 05-02-2021

• The material held up time is determined by;

– The speed of rotation.
– The angle of inclination.
– The air velocity.
• Based on the method of heat transfer, rotary
dryer can be classified into;
– Direct-heated rotary dryer.
– Indirect- Direct rotary dryer.
– Indirect rotary dryer.
– Special type.

20
 05-02-2021

• A rotary dryer is said to be of the direct type if by virtue of its

design, heat is added to or removed from the solids by direct
exchange between the gas and solids. The direct heat dryer are the
simplest and the most economical class.
• They are used when a direct contact with the hot gas or air is not
detrimental to the fed. When high temperature is required for
drying process in a direct-heated rotary dryer, a combustion
chamber is used and when low temperature is required on the
other hand, for thermolabile materials, steam coil is used.
• Rotary dryer can also be said to be indirect when the heating
medium is separated from contact with the solid by a metal wall or
tube.
• Although there is an infinite variation of rotary dryers, which
present characteristics suitable for drying, chemical reactions,
mixing, solvent recovery, thermal decompositions, sintering and
agglomeration of solids, the main types or rotary dryers include;

Advantages of Rotary Dryer

• Rotary dryers are less sensitive to particle size.
• It can accept the highest flue gasses of any
type of dryer.
• Low maintenance cost; thus economical.
• It has the greatest capacity than any type of
dryer.

21
 05-02-2021

Disadvantages of Rotary dryer

• Excessive entrainment losses in the exist gas
stream is possible especially if the material
contains extremely fine particles due to the
large gas volumes and high gas velocities that
are usually required.

Fluidized Bed Dryer

• A typical fluidized bed dryer consists of the
following components.
– Air preparatory unit.
– Product container.
– Exhaust filter.
– Exhaust blower.
– Control panel.
– Air distribution plate.
– Spray nozzle.
– Solution deliver.

22
 05-02-2021

• In fluidized bed dryer, hot air is passed at high pressure

through a perforated bottom of the container containing
the wet solids.
• The wet solids are lifted from the bottom and suspended
in a stream of air (fluidized state).
• The hot air then surrounds every granules.
• Heat transfer is accomplished by direct contact between
the wet solid and hot gases.
• The vapourized liquid is carried away by the drying
gasses. Sometimes to save energy, the exit gas is partially
recycled.

Uses
• They have also found use in the drying of
suspension, slurries, solutions, dilute paste or
sludges.

23
 05-02-2021

Parameters to be controlled in
fluidized bed dryers (system)
• In order to improve operation, efficiency and reproducibility
of a fluidized bed dryer, some parameters need to be
controlled.

• These parameters are categorized into:

– Apparatus parameters: Those controlled by equipment.
– Process parameters: These controlled by process.
– Product parameters: Those controlled by product.

Apparatus/Equipment Parameter
• Position of the air distribution plate:
– This parameter influences the pattern.
• Shape of the instrument:
– The annular based design gives better product.
• Nozzle height:
– Nozzle height plays a vital role when fluidized bed
dryer is used as a coating machine. The atomized
coating solution should not get dried before
reaching the tablet surface.

24
 05-02-2021

Process/Operating Parameter
• Temperature:
– Increased temperature leads to increased moisture
diffusivity and hence increased drying rate and decreased
drying time. The nature of the material plays an important
role in the choosing operating temperature.
• Humidity:
– Faster drying is achieved when the moisture content of the
inlet air is maintained at its minimum.
• Air flow rate/gas velocity:
– Increasing gas velocity increases drying rate but should be
maintained at optimized rate (not to fast or too slow). Gas
velocity has no effect on particles with high internal
resistance to moisture transfer

Product Parameters
• Moisture content of the feed material.
• Feed rate/batch size.
• Product moisture content.
• Particle size, shape and diameter.

25
 05-02-2021

Types of fluidized bed dryer

Conventional fluidized bed dryers

• Batch fluidized bed dryers.
• Semi-continuous fluidized bed dryers.
• Well-mixed, continuous fluidized dryers.
• Plug flow fluidized bed dryer.

26
 05-02-2021

Advantages of Fluidized bed Dryer

• High rates of moisture removal due to excellent
gas-particle constant which results to high heat
and mass transfer rates.
• High thermal efficiency is usually achieved if part
of the thermal energy for drying is supplied by
internal heat exchanger
• Lower capital and maintenance cost
• Reduced contact time for drying.
• Ease of control.

Disadvantages of Fluidized Dryer

• High pressure drops results as a result of the need to suspend the
entire bed in gas which equally leads to high energy consumption.
• Requires increased gas handling due to extensive recirculation of
exhausts gas for high thermal efficiency operation.
• Poor fluidization and low flexibility especially if the feed is too wet.
• Not the best choice of equipment when organic solvents need to be
removed during drying.
• Non uniform product quality for certain types of fluidized bed dryer.
• Entertainment of fine particles.
• High potential of attrition; and in some cases agglomeration of fine
particles.
• The conventional hot air fluidized bed dryer is not a good choice of
dryer when handling toxic or flammable solids since there is danger
of fire or explosion of flammability limits are exceeded.

27
 05-02-2021

Tray Dryer
• operate in batch mode
• use racks to hold product
• circulate air over the material
• It consists of a rectangular chamber of sheet metal
containing trucks that support racks.
• Each rack carries a number of trays that are loaded with the
material to be dried.
• Hot air flows through the tunnel over the racks.
• Sometimes fans are used to on the tunnel wall to blow hot
air across the trays.
• Even baffles are used to distribute the air uniformly over
the stack of trays.
• Some moist air is continuously vented through exhaust
duct; makeup fresh air enters through the inlet.
• The racks with the dried product are taken to a tray-
dumping station.

Tray Dryer
• Uniform flow rate is required for uniform drying
• Controlling parameter is gas flow rate

28
 05-02-2021

Uses
• useful when the production rate is small.
• Drying of filter cake, fine chemicals, fragile
materials and pasty substances
• Disadvantages
– have high labor requirement for loading and
unloading the materials, and are expensive to
operate
– Non-uniform drying due to stagnant air pockets

Advantages
• Low cost
• Less space requirements
• Ease of cleaning
• Good control of drying conditions

29
 05-02-2021

Drum Dryer
• liquid containing dissolved solids or slurry
carrying suspended solids forms a thin layer
on the outside surface of a large rotating
drum.
• For a single drum unit thickness of the film
can be controlled by an adjustable scraping
blade.
• For double drum unit thickness can be
controlled by the gap between the drums

30
 05-02-2021

Flash Dryer /Pneumatic dryer

Flash Dryer
• Operating principle to spray dryer.

• The materials that are to be dried (i.e. solid or semisolid) are dispersed in finely
divided form in an upward flowing stream of heated air.

• The wet materials that are to dried can be passed into a high-temperature air
stream that carries it to a hammer mill or high-speed agitator where the exposed
surface is increased.

• The drying rate is very high for these dryers (hence the term flash dryers), but the
solid temperature does not rise much because of the short residence time.

• The fine particles leave the mill through a small duct to maintain the carrying
velocities (drying gas) and reach a cyclone separator.

• A solid particle takes few seconds to pass from the point of entry into the air
stream to the collector. The inlet gas temperature is high and varies from 650oC to
315oC, for example, in 2 seconds, or from 650oC to 175oC in 4 seconds.

31
 05-02-2021

• The thermal efficiency this type of dryer is generally low.

• A material having an initial moisture content of 80 % may

be reduced to 5 or 6 % in the dried product.

• These types of dryer are mainly used for drying of heat

sensitive or easily oxidizable materials

• The special advantage of this type of dryer is that no

separate arrangement is required for transporting the
dried product.

Screen Conveyor Dryers / belt conveyor

dryer
• A direct heat continuous type dryer
• The solid to be dried are fed on to endless, perforated,
conveyor belt through which hot air is forced.
• The belt is housed in a long rectangular drying
chamber or tunnel (figure 2.6).
• The chamber is divided into series of separate sections,
each with its own fan and air heater.
• Air may be recirculated through, and vented from each
section separately or passed from one section to
another counter current to the solid movement.
• The solid is carried through the tunnel and discharged
at the opposite end.

32
 05-02-2021

• In order to prevent the higher flow rate of hot

air through thinner regions of the bed a
uniform feeding rate and distribution of the
material over the conveyor is necessary.
• Coarse granular, flakey, or fibers materials can
be dried by through circulation without any
pretreatment and without loss of material
through the screen.

Advantages and Drawbacks

• High drying rate can be achieved with good product quality control.
• Thermal efficiency of this type of dryer is high and with steam heating, the
steam consumption for heating the drying gas can be as low as 1.5 kg per
kg of water evaporated.
• Only disadvantage of this type of dryer are high initial cost and high
maintenance cost due to the mechanical belt.

33
 05-02-2021

NOVEL DRYING TECHNOLOGIES

• Microwave Drying
• Microwave heating is a direct drying method.
• High-frequency radio waves are utilized in microwave drying.
• A high-frequency generates the waves and wave channel guides them in
to an oven that is designed to prevent the waves from leaving the
chamber.
• In microwave drying, heat is generated by directly transforming the
electromagnetic energy in to kinetic molecular energy, thus the heat is
generated deep within the material to be dried.
• In case of microwave drying the waves bounce from wall to wall, until the
product absorbs eventually all of the energy, generating heat within the
material, resulting in dehydration.
• Vapour from the liquid evaporating inside the product is emitted through
the pore structure of the solid material‟s macro-capillary system, resulting
in a high drying rate.
• This type of dryer is highly efficient and power utilization efficiencies are
generally greater than 70 %.

Microwave Drying
• Selection of proper wavelength is necessary to ensure thorough
penetration into the material.

• Material type and depth of material being exposed also affect the
penetration.

• Therefore, selection of proper wavelengths and dehydration

condition for each product is selected individually.
• Important commercial aspects of this dryer includes the ability to
maintain colour, moisture and quality of the natural food.

34
 05-02-2021

Advantages
• This type of heating is instantaneous, uniform
and penetrating throughout the material,
which is a great advantage for the processing
of pharmaceutical compounds.

Supercritical Fluid Extraction and its application

to Drying
• The supercritical fluid (SCF) is a substance at a temperature
and pressure above its critical point.
• It can effuse through solids like a gas, and dissolve
materials like a liquid.
• Supercritical fluids possess unique properties that enable
them to extract components selectively from a mixture.
• This ability has been investigated as an alternative to
currently used separation processes such as distillation or
liquid extractions.
• In addition, close to the critical point, small changes in
pressure or temperature result in large changes in density,
allowing many properties of a supercritical fluid to be "fine-
tuned".
• Above the critical point, this increased density produces
enhanced solvency, approaching that of a liquid. It is this
solvency that makes SCF extraction a feasible alternative.

35
 05-02-2021

SCFED
• An application of SCF extraction that has seemingly gone unexplored is to the
drying of food products.

• Since moisture content influences texture, chemical reactions, and susceptibility to

microbial spoilage, drying is a way to retain quality and prolong shelf life.

• A complication associated with drying of food products is that they may undergo
changes that alter the physical or chemical structure, thus changing the integrity of
the product.

• SCF extraction avoids this problem because it allows the food product to be
dehydrated without undergoing a phase change from liquid water to water vapour.

• Also, if a solvent such as supercritical carbon dioxide is used, it will not be

necessary to heat the product above ambient temperatures.

36