ADIGRAT UNIVERSITY

COLLEGE OF ENGINEERING AND TECHNOLOGY

DEPARTEMENT OF CHEMICAL ENGINEERING
PROJECT ON MASS TRANSFER UNIT OPERATION

Course code: (ChEng3114)

PREPARED BY NETWORK -4-(four)
SECTION ONE (1)
Year 3rd (third)
NETWORK MEMBER

ID

1. G/georgs Berhe.RET 0569/06

2. Jemal Seid.RET 0834/06
3. Rigbey Kidey.RET 1242/06
4. Te-ame G/Tsadik.....................................RET 1406/06
5. T/haimanot Abraha.....................................RET 1443/06
6. Tesfaye BayleRET 1499/06

Submitted to instructor
H/Mikael Tsegay
Email:hailush2006@gmail.com

Submission Date 01/09/2008 E.C

Table content

Page

Acknowledgement.....
1) Drying of solids.1
1.1) Fundamental principles of drying1
1.2) Field of application.2
1.3) Basic principles of drying2
1.4) Thermodynamic properties of air-water mixtures and moist solids2
1.4.1) Psychrometry....2
1.4.2) Psychrometric terms.........................................................................3
1.5) Mechanism of drying...4
1.6) Types of dryers..6
1.7) Dryer efficiency...10
2) Crystallization11
2.1) Definition Crystallization11
2.2) Types of Crystallizers..12
2.3) Solid-Liquid-Equilibria..13
2.3.1) Solubilities and Phase Diagrams.13
3) Extraction...15
3.1) Solid-Liquid Extraction....................16
3.1.2) General principles.16
3.2 Liquid-liquid extraction ...17
3.2.1) Extraction Processes.....18
3.2.2) General principles.........18
3.2.3) Equilibrium Data.......19
3.2.4) Factors influencing extraction performance..19
3.3 Liquid-Gas Extraction (absorption)...20
4) References21

Figure content

Page

1) Figure1. Segment AB of the graph represents the constant-rate drying period, while
segment BC is the falling-rate period4
2) Figure2 spray dryer.9
3) Figure3; Simplified representation of liquid-liquid extraction.18

Acknowledgement
First and for most we would like to say great thank you for our God, and We would like to
say thank you to all support for us during doing this project and our teacher in case of giving
or guiding us how to write our project.

CHAPTER ONE
DRYING OF SOLIDS
1.1) FUNDAMENTAL PRINCIPLES OF DRYING
Introduction
The separation operation of drying converts a solid, semi-solid or liquid feedstock into a
solid product by evaporation of the liquid into a vapour phase via application of heat.
Drying is an essential operation in the chemical, agricultural, biotechnology, food, polymer,
ceramics, pharmaceutical, pulp and paper, mineral processing, and wood processing
industries.
Drying is perhaps the oldest, most common and most diverse of chemical engineering unit
operations.
Over four hundred types of dryers have been reported in the literature while over one hundred
distinct types are commonly available.
Drying of various feed stocks is needed for one or several of the following reasons: need for
easy-to-handle free-flowing solids, preservation and storage, reduction in cost of
transportation, achieving desired quality of product, etc.
In many processes, improper drying may lead to irreversible damage to product quality and
hence a non-saleable product.

OBJECTIVE
Drying is defined as the application of heat under controlled conditions, to remove the
water present in liquid foods by evaporation to yield solid product. It differs from
evaporation, which yields concentrated liquid products. The main purpose of drying is to
extend the shelf life of foods by reducing their water activity.

1.2) FIELD OF APPLICATION

Typical applications for drying techniques include dairy products (milk, whey, creamers),
coffee, coffee surrogates, tea, flavours, powdered drinks, and processed cereal based foods.

1.3) BASIC PRINCIPLES OF DRYING

Drying is a complex operation involving transient transfer of heat and mass along with
several rate processes, such as physical or chemical transformations, which, in turn, may
cause changes in product quality as well as the mechanisms of heat and mass transfer.
Physical changes that may occur include: shrinkage, puffing, crystallization, glass
transitions. In the manufacture of catalysts, for example, drying conditions can yield
significant differences in the activity of the catalyst by changing the internal surface
area.
Drying occurs by effecting vaporization of the liquid by supplying heat to the wet
feedstock. As noted earlier, heat may be supplied by convection (direct dryers), by
conduction (contact or indirect dryers), radiation or volumetrically by placing the wet
material in a microwave or radio frequency electromagnetic field.
Over 85% of industrial dryers are of the convective type with hot air or direct
combustion gases as the drying medium. Over 99% of the applications involve
removal of water.
All modes except the dielectric (microwave and radio frequency) supply heat at the
boundaries of the drying object so that the heat must diffuse into the solid primarily by
conduction.
Transport of moisture within the solid may occur by any one or more of the following
mechanisms of mass transfer:
Liquid diffusion, if the wet solid is at a temperature below the boiling point of the
liquid
Vapor diffusion, if the liquid vaporizes within material
Knudsen diffusion, if drying takes place at very low temperatures and pressures, e.g.,
in freeze drying.
Surface diffusion (possible although not proven)
Hydrostatic pressure differences, when internal vaporization rates exceed the rate of
vapour transport through the solid to the surroundings.
Combinations of the above mechanisms
Note that since the physical structure of the drying solid is subject to change during drying
the mechanisms of moisture transfer may also change with elapsed time of drying.
1.4. Thermodynamic Properties of Air-Water Mixtures and Moist Solids

1.4.1. Psychrometry
Psychrometry is the science of various properties of air, method of controlling its
temperature and moisture content or humidity and its effect on various material and
human beings.
The term air conditioning means treating of air or conditioning the air to change its
temperature or the moisture as per the requirements of various applications. They are the
devices or machine that condition or alter the state of the air by changing its temperature and
the humidity level.

As noted earlier, a majority of dryers are of direct (or convective) type. In other words, hot air
is used both to supply the heat for evaporation and to carry away the evaporated moisture
from the product.
Notable exceptions are freeze and vacuum dryers, which are used almost exclusively for
drying heat-sensitive products because they tend to be significantly more expensive than
dryers operate near to atmospheric pressure.

1.4.2. Psychrometric terms

Dry and wet bulb temperature, specific volume, humidity, enthalpy and more.
Psychrometry is the science of studying thermodynamic properties of moist air and the use of
those to analyse moist air conditions and processes.
Air conditioning processes can be determined with psychrometric charts or Moller Diagrams.
Common properties in the charts includes
Dry-bulb temperature
wet-bulb temperature
relative humidity (RH)
humidity ratio
specific volume
dew point temperature
enthalpy
With at least two known properties it is possible to characterize the air in the intersection of
the property lines the state point. With the intersection point located on the chart or
diagram other properties can be read directly.

1.4.3. Equilibrium Moisture Content

The moisture content of a wet solid in equilibrium with air of given humidity
and temperature is termed the equilibrium moisture content (EMC). A plot of
EMC at a given temperature versus the relative humidity is termed sorption
isotherm.
An isotherm obtained by exposing the solid to air of increasing humidity gives
the adsorption isotherm.
Water Activity
In drying of some materials, which requires careful hygienic attention, e.g., food, the
availability of water for growth of microorganisms, germination of spores, and participation
in several types of chemical reaction becomes an important issue. This availability, which
depends on relative pressure, or water activity, aw, is defined as the ratio of the partial
pressure, p, of water over the wet solid system to the equilibrium vapour pressure, pw, of
water at the same temperature. Thus, aw, which is also equal to the relative humidity of the
surrounding humid air, is defined as: aw=

Different shapes of the X versus aw curves are observed, depending on the type
of material (e.g., high, medium or low hygroscopicity solids).
3

1.5) MECHANISM OF DRYING

Drying may be defined as the vaporization and removal of water or other liquids from
a solution, suspension, or other solid-liquid mixture to form a dry solid. It is a
complicated process that involves simultaneous heat and mass transfer, accompanied
by physicochemical transformations.
Drying occurs as a result of the vaporization of liquid by supplying heat to wet
feedstock, granules, and filter cakes and so on. Based on the mechanism of heat
transfer that is employed, drying is categorized into direct (convection), indirect or
contact (conduction), radiant (radiation) and dielectric or microwave (radio
frequency) drying.
Heat transfer and mass transfer are critical aspects in drying processes.
Heat is transferred to the product to evaporate liquid, and mass is transferred as a
vapour into the surrounding gas.
The drying rate is determined by the set of factors that affect heat and mass transfer.
Solids drying is generally understood to follow two distinct drying zones, known as
the constant-rate period and the falling-rate period. The two zones are
demarcated by a break point called the critical moisture content. In a typical graph
of moisture content versus drying rate and moisture content versus time (Figure 1),
section AB represents the constant-rate period. In that zone, moisture is considered to
be evaporating from a saturated surface at a rate governed by diffusion from the
surface through the stationary air film that is in contact with it. This period depends
on the air temperature, humidity and speed of moisture to the surface, which in turn
determine the temperature of the saturated surface.
During the constant rate period, liquid must be transported to the surface at a rate
sufficient to maintain saturation.

Figure1. Segment AB of the graph represents the constant-rate drying period, while segment
BC is the falling-rate period.

At the end of the constant rate period, (point B, Figure 1), a break in the drying curve occurs.
This point is called the critical moisture content, and a linear fall in the drying rate occurs
with further drying. This section, segment BC, is called the first falling-rate period.
As drying proceeds, moisture reaches the surface at a decreasing rate and the mechanism that
controls its transfer will influence the rate of drying. Since the surface is no longer saturated,
it will tend to rise above the wet bulb temperature. This section, represented by segment CD
in Figure 1 is called the second falling-rate period, and is controlled by vapor diffusion.
Movement of liquid may occur by diffusion under the concentration gradient created by the
depletion of water at the surface. The gradient can be caused by evaporation, or as a result of
capillary forces, or through a cycle of vaporization and condensation, or by osmotic effects.
The capacity of the air (gas) stream to absorb and carry away moisture determines the drying
rate and establishes the duration of the drying cycle. The two elements essential to this
process are inlet air temperature and air flow rate. The higher the temperature of the drying
air, the greater its vapour holding capacity. Since the temperature of the wet granules in a hot
gas depends on the rate of evaporation, the key to analysing the drying process is
psychometric, defined as the study of the relationships between the material and energy
balances of water vapour and air mixture.

1.5.1) DRYING END POINT

There are a number of approaches to determine the end of the drying process. The most
common one is to construct a drying curve by taking samples during different stages of
drying cycle against the drying time and establish a drying curve.
When the drying is complete, the product temperature will start to increase, indicating the
completion of drying at specific, desired product-moisture content. Karl Fischer titration and
loss on drying (LOD) moisture analysers are also routinely used in batch processes.
The water vapor absorption isotherms are measured using a gravimetric moisture-sorption
apparatus with vacuum-drying capability.
For measuring moisture content in grain, wood, food, textiles, pulp, paper, chemicals, mortar,
soil, coffee, jute, tobacco, rice and concrete, electrical-resistance-type meters are used.
This type of instrument operates on the principle of electrical resistance, which varies
minutely in accordance with the moisture content of the item measured.
Dielectric moisture meters are also used.
They rely on surface contact with a flat plate electrode that does not penetrate the product.

1.6) TYPES OF DRYERS

Adiabatic dryers are the type where the solids are dried by direct contact with
gases, usually forced air.
With these dryers, moisture is on the surface of the solid.
Non-adiabatic dryers involve situation where a dryer does not use heated air or
other gases to provide the energy required for the drying process. Dryer
classification can also be based on the mechanisms of heat transfer as follows:
Direct (convection)
Indirect or contact (conduction)
Radiant (radiation)
Dielectric or microwave (radio frequency) drying.

 With adiabatic dryers, solid materials can be exposed to the heated gases
via various methods, including the following:
Gases can be blown across the surface (cross circulation)
Gases can be blown through a bed of solids (through-circulation); used
when solids are stationary, such as wood, corn and others
Solids can be dropped slowly through a slow-moving gas stream, as in a
rotary dryer
Gases can be blown through a bed of solids that fluidize the particles. In
this case, the solids are moving, as in a fluidized-bed dryer.
Solids can enter a high-velocity hot gas stream and can be conveyed
pneumatically to a collector (flash dryer).
Direct, or adiabatic, units use the sensible heat of the fluid that contacts the solid to provide
the heat of vaporization of the liquid.
Non-adiabatic dryers (contact dryers) involve an indirect method of removal of a liquid phase
from the solid material through the application of heat, such that the heat-transfer medium is
separated from the product to be dried by a metal wall.
Heat transfer to the product is predominantly by conduction through the metal wall and the
impeller. Therefore, these units are also called conductive dryers.

Although more than 85% of the industrial dryers are of the convective type,
contact dryers offer higher thermal efficiency and have economic and
environmental advantages over convective dryers.
A. BATCH DRYERS
The following are descriptions of various types of batch dryers.

a) Tray dryers. This dryer type operates by passing hot air over the surface of a wet solid
that is spread over trays arranged in racks. Tray dryers are the simplest and least-expensive
dryer type. This type is most widely used in the food and pharmaceutical industries. The
chief advantage of tray dryers, apart from their low initial cost, is their versatility. With the
exception of dusty solids, materials of almost any other physical form may be dried. Drying
times are typically long (usually 12 to 48 h).
b) Vacuum dryers. Vacuum dryers offer low-temperature drying of thermo labile
materials or the recovery of solvents from a bed. Heat is usually supplied by passing steam or
hot water through hollow shelves. Drying temperatures can be carefully controlled and, for
the major part of the drying cycle, the solid material remains at the boiling point of the
wetting substance. Drying times are typically long (usually 12 to 48 h).
c) Fluidized-bed dryers. A gas-fluidized bed may have the appearance of a boiling
liquid. It has bubbles, which rise and appear to burst. The bubbles result in vigorous mixing.
A preheated stream of air enters from the bottom of the product container holding the product
to be dried and fluidizes it. The resultant mixture of solids and gas behave like a liquid, and
thus the solids are said to be fluidized. The solid particles are continually caught up in eddies
and fall back in a random boiling motion so that each fluidized particle is surrounded by the
gas stream for efficient drying, granulation or coating purposes. In the process of fluidization,
intense mixing occurs between the solids and air, resulting in uniform conditions of
temperature, composition and particle size distribution throughout the bed.
d) Freeze dryers. Freeze-drying is an extreme form of vacuum drying in which the water
or other solvent is frozen and drying takes place by subliming the solid phase. Freeze-drying
is extensively used in two situations:
(1) When high rates of decomposition occur during normal drying; and
(2) With substances that can be dried at higher temperatures, and that are thereby changed in
some way.
Microwave vacuum dryers, High-frequency radio waves with frequencies from 300 to 30,000
MHz are utilized in microwave drying (2,450 MHz is used in batch Microwave processes).
Combined microwave-convective drying has been used for a range of applications at both
laboratory and industrial scales. The bulk heating effect of microwave radiation causes the
solvent to vaporize in the pores of the material. Mass transfer is predominantly due to a
pressure gradient established within the sample. The temperature of the solvent component is
elevated above the air temperature by the microwave heat input, but at a low level, such that
convective and evaporative cooling effects keep the equilibrium temperature below
saturation. Such a drying regime is of particular interest for drying temperature-sensitive
materials. Microwave-convective processing typically facilitates a 50% reduction in drying
time, compared to vacuum drying.

B. CONTINUOUS DRYERS
Continuous dryers are mainly used in chemical and food industries, due to the large volume
of product that needs to be processed.
Most common are continuous fluid-bed dryers and spray dryers.
There are other dryers, depending on the product, that can be used in certain industries for
example, rotary dryers, drum dryers, kiln dryers, flash dryers, tunnel dryers and so on. Spray
dryers are the most widely used in chemical, dairy, agrochemical, ceramic and
pharmaceutical industries.

a) Spray dryer. The spray-drying process can be divided into four sections:
atomization of the fluid, mixing of the droplets, drying, and, removal and
collection of the dry particles.
The flow of the drying gas may be concurrent or counter current with respect to
the movement of droplets.
Good mixing of droplets and gas occurs, and the heat- and mass-transfer rates
are high.
In conjunction with the large interfacial area conferred by atomization, these
factors give arise to very high evaporation rates. The residence time of a droplet
in the dryer is only a few seconds (530 s).
Since the material is at wet-bulb temperature for much of this time, high gas
temperatures of 1,508 to 2,008C may be used, even with thermo labile
materials. For these reasons, it is possible to dry complex vegetable extracts,
such as coffee or digitalis, milk products, and other labile materials without
significant loss of potency or flavour.
The capital and running costs of spray dryers are high, but if the scale is
sufficiently large, they may provide the cheapest method.

Figure2 spray dryer

1.7) DRYER EFFICIENCY

With increasing concern about environmental degradation, it is desirable to
decrease energy consumption in all sectors.
Drying has been reported to account for anywhere from 12 to 20% of the energy
consumption in the industrial sector. Drying processes are one of the most
energy-intensive unit operations in the CPI.
One measure of efficiency is the ratio of the minimum quantity of heat that will
remove the required water to the energy actually provided for the process.
Sensible heat can also be added to the minimum, as this added heat in the
material often cannot be economically recovered.
Other newer technologies have been developed, such as sonic drying,
superheated steam, heat-pump-assisted drying and others.
1.8) Summary
Drying is an essential unit operation used in various process industries.
The mechanism of drying is well understood as a two-stage process and
depends on the drying medium and the moisture content of the product being
dried.
Batch dryers are common in chemical and pharmaceutical industries, while
continuous dryers are routinely used where large production is required.
Since the cost of drying is a significant portion of the cost of manufacturing a
product, improving efficiency or finding alternative drying routes is essential.

10

CHAPTER TWO
CRYSTALLISATION
Introduction
Crystallization is a thermal separation, and therefore a purification process that yields a solid
product from a melt, from a solution or from a vapour. As for all thermal separations, nonequilibrium conditions are required as a driving force for the process. Here, evaporation of
solvent or temperature reduction (cooling) is the most frequent. Means employed to establish
the required non-equilibrium conditions. Pressure can, in principle, also be used to enforce
the non-equilibrium state necessary for a phase change. However, in industrial applications
this parameter is most frequently kept constant. The main feature distinguishing
crystallization from other thermal separation processes is the fact that it leads to a solid
product. This is one of the key reasons why it lags behind separation techniques involving
liquid-liquid or liquid-gaseous phase change processes in terms of research effort expended
and knowledge available. Crystallization is a highly selective process and operates at lower
temperatures when compared to a separation by distillation for the same material.
Melt crystallization has the additional advantage of not requiring a solvent, although it is not
a method suitable for all materials. Manifold reasons exist for the growing importance of
crystallization as an industrial separation process. Two processes are important in
crystallization, both with their own characteristic kinetics.
One of these processes is nucleation [Kashehiev], the other is crystal growth. Both of these
phenomena are dependent on a large number of variables that in some cases may be
illustrated.

Objective
Crystallisation is the formation of solid crystals from a solution. Crystals solidify in a definite
geometric form. The objective of crystallisation is to separate a solute from a solvent. Any
impurities in the liquid are usually not incorporated in to the lattice structure of the desired
crystal. Accordingly crystallisation is also purification processes.
Finally crystals possess an internal structure, an external shape and consequently a finite size
(or size distribution in the case of a quantity of crystals).
These parameters determine many bulk properties of a given crystalline material, such as
dissolution rate, bio-availability, color, flow properties etc. A general overview of these
properties will also be provided.

2.1. Definition Crystallization

Crystallization is a process which consists of mixing the massecuite for certain time after
dropping from the pans, and before passing to the centrifugals. The process is with the aim of
completing the formation of crystals and forcing further exhaustion of the mother liquor. The
massecuite when discharged from the pan is at a high super saturation.
If it is allowed to stand, the sugar still contained in the mother liquor will continue to be
deposited as a crystal, but this masscuite is very viscous. Therefore the masscuite must be
kept in motion in order to change constantly the relative positions of the particles of mother
liquor and crystals until the mother liquor becomes a substantially exhausted molasses
11

2.2) Types of Crystallizers

There are crystallizer of batch and continuous operation. Depending on the system of
cooling there are1. Air Cooled Crystallizers
2. Water Cooled Crystallizers

1. Air-Cooled Crystallizers
The massecuite is cooled by the circulation of air from the walls of crystallizers and from the
surface of the massecuite.
The cooling effect is slow. Nowadays the air cooled crystallizers are commonly used for
storing high grade massecuite and their use for cooling low grade massecuite is not favored

2. Water Cooled Crystallizers

These crystallizers have three arrangements: Water jacketed
Cooling coil of rotating type
Water jacketed crystallizers are not found very satisfactory, recently they are not used.
The cooling coil of stationary type is less efficient due to poor contact of the massecuite with
the cooling surface. They are only used because of lower cost.

12

2.3. Solid-Liquid-Equilibria
2.3.1. Solubilities and Phase Diagrams
A solution is a homogeneous mixture of two or more chemical species. For a liquid solution
saturation is reached when the liquid phase, in contact with the solid phase, no longer
changes its composition. A saturated solution therefore has a constant composition that is not
changed by the addition of further amount of the dissolved material. For a two component
system, the solubility of one component in the other is dependent on temperature and
pressure. For three and more component systems the solubility of one component also
depends on the relative amounts of the other components present. For liquid solutions the
pressure dependence is negligible if the pressure difference is small (which is the case in
most applications) and will not be considered here.
It is common terminology for solutions of solids in liquids to denote the liquid component as
the solvent and the solid component as the solute, even if the amount of solute in the solution
exceeds the amount of solvent. Various measures of composition are in use to report
solubilities and the use of a particular set of units should be carefully selected to suit the
purpose the data are required for. The most common measures are
Mass of solute per unit mass of solvent (kg/kg)
Mass of solute per unit mass of solution (kg/kg)
Mass of solute per unit volume of solvent (kg/m3 or g/L)
Molar amount of solute per unit volume of solvent (kmol/m3 or mol/L)
From the above list it is clear that, for the first two cases, it has to be stated explicitly whether
composition reported refers to the solvent or the solute in order to avoid confusion. Moreover, it
is often necessary to mention the initial state of the solute, as many substances can exist as
solvated or un solvated solids (vide infra). For example, two solutions of sodium carbonate in
water will have different compositions if in one case the decahydrate is used as starting material
and in the other the same mass of monohydrate is employed.
Ambiguity arises if this is not accounted for.
The solubility of most materials increases with temperature. However, a number of examples
exist, where the solubility shows the reverse trend (sodium sulfate, calcium carbonate, iron
sulfate dehydrate, to name but a few).
The dependence of the solubility upon temperature is best represented graphically in the form of a
solubility curve, which maps the composition of a solution at the solubility limit onto the
temperature.
Solubilities are determined experimentally and any convenient analytical technique that provides
a quantitative measure of composition can be employed. Not every technique.
The driving force for crystallization (both nucleation and crystal growth, see section on kinetics
below) increases with increasing super saturation.
Super saturation can be achieved in a number of ways, most commonly by cooling a saturated
solution (for solutes where solubility increases with temperature, solutes with reverse temperature
dependence must, of course, be heated) or by evaporation of solvent. As is the case for solubility,
several measures exist to express super saturation.

13

These are the difference between the equilibrium composition at the temperature of the
supersaturated solution C and the actual composition in the supersaturated solution C.
C=C-C (1)
The ratio of these two concentration
S=C/C . .......................................................................... (2)
=C/C =S-1 ... (3)
For melts, the driving force is usually expressed in terms of the super cooling
= -, (4)
Which represents the difference between the equilibrium temperature of the melt * and the
actual temperature . occasionally supercooling also finds use in solution crystallization.
Quantifying the super saturation is important for two reasons. As mentioned above the super
saturation is a measure of the driving force for the crystallization process.
The second reason concerns the theoretical yield of the process.

Summary
Crystallization as a separation process yields a solid product from a solution or a melt. The
process itself, the product characteristics and the temporal behaviour are determined by
thermodynamics, i.e. solubility of the materials, and crystallization kinetics, respectively.
The thermodynamics of solutions and melts are dependent on a range of physical parameters
as discussed within. Crystallization kinetics can be divided into two separate processes,
nucleation and crystal growth. Both play a significant role in the design of equipment for a
given process and are treated in detail below.
Additional factors such as the effect of crystallization on product properties as well as the
effect of solid-state properties on the crystallization process are discussed in section 4.
Section 5 provides details on commonly used crystallizer designs and highlights the
distinction between solution and melt crystallization.

14

CHAPTER THREE
EXTRACTION
Introduction
Extraction is a widely used method for the separation of a substance from a mixture.it
involves the removal of a component of a mixture by contact with second phase. Solid-liquid
and liquid-liquid extraction are commonly performed by batch and continuous process. The
removal of caffeine from coffee beans with dichloromethane is an example of solid-liquid
extraction.
In numerous applications, extraction is a more efficient, selective and cost-effective
alternative to competing separating methods such as distillation, evaporation and diaphragm
technology. Applications of this method include obtaining oil from oil seeds or leaching of
metal salts from ores

Objective
The objective of extraction is to recover valuable soluble components from raw materials by
primarily dissolving them in a liquid solvent, so that the components can be separated and
recovered later from the liquid.

15

3.1 Solid-Liquid Extraction

The Solid-Liquid Extraction experimentation stand separates solid mixtures using solidliquid extraction (leaching). Solid-liquid extraction allows soluble components to be removed
from solids using a solvent.
The range of experiments covers the following areas:
Familiarisation with the fundamental principles of solid-liquid extraction
Demonstration of solid-liquid extraction as a continuous and discontinuous process
Investigation of a single, two and three stage process
Influence of solvent flow rate and temperature on the extraction process
Influence of extraction material mass flow and extractor speed on the extraction
process.
Function
The unit works on the counter flow principle,
I.e. fresh solvent is fed to leached extraction material. With this operating method, the
concentration gradient is the driving force for the mass transfer.

3.1.2 General principles

Solid-liquid extraction involves dissolving soluble components out of solid mixtures
using an solvent.
In the simplest form of this method, the extraction material and the solvent are mixed
well. The solvent and the dissolved usable substance are then removed and processed.
Processing of the solvent with dissolved usable substance normally involves evaporation. The
solvent is evaporated and the usable substance remains as a product.
The solvent is condensed and can then be reused.
A day-to-day example of solid-liquid extraction is the preparation of coffee. Here,
water (solvent) dissolves the colours and flavourings (usable substance) out of the
coffee powder (extraction material, consisting of the solid carrier material and the
soluble components). Ideally, drinkable coffee is obtained (extract) and the leached
coffee powder (extraction residue) remains in the coffee filter.
Solid-liquid extraction is mainly carried out as percolation extraction and immersion
extraction discontinuously or, preferably, continuously.
Percolation extraction:
The crushed and solubilised solid is passed through the extraction apparatus and sprayed
with solvent in stages. The solvent must flow effectively through the solid.

Solvent requirements
There is no universal solvent. The required solvent must be identified specifically for the
relevant extraction task.
The solvent can either be identified experimentally using solution experiments or from the
results of extraction tasks already investigated.

16

 There are particular requirements of the solvent: Selectivity

It should only dissolve the usable substance, otherwise a subsequent separating method is
required to separate the usable substance from the extract.
Solubility
It should dissolve the usable substance as quickly as possible and dissolve the maximum
possible amount of usable substance
Chemical reaction properties
It should not react chemically with the components of the extraction material
Boiling properties
The boiling point of the solvent should not be too high and the evaporation heat should be as
low as possible, to ensure efficient recovery of the solvent.

3.2 Liquid-liquid extraction

Introduction
The separation of the components of a liquid mixture by treatment with a solvent in which
one or more of the desired components is preferentially soluble.
Three stages are involved:
(a) Bringing the feed mixture and the solvent in to intimate contact,
(b) Separation of the resulting two phases,
(c) Removal and recovery of the solvent from each phase.
It is complementary to distillation and is preferable in the following cases:
(a) Distillation requires excessive amounts of heat.
(b)The formation of azeotropes limits the degree of separation obtainable.
(c) Heating must be avoided.
(d)The components to be separated are quite different in nature.
Liquid-liquid extraction refers to the dissolving out of one or more components of a liquid
mixture using a solvent.
Examples of liquid-liquid extraction are
Separation of aromatic compounds from crude oil fractions.
Separation of vitamins from aqueous solutions.
Removal of lecithin from vegetable oil.
Therefore liquid-liquid extraction involves at least three liquids.
Names such as solution, solvents, etc. often lead.

Important applications include

The separation of aromatics from kerosene-based fuel oils to improve their burning
qualities.
The separation of aromatics from parafn and naphthenic compounds to improve the
temperature-viscosity characteristics of lubricating oils.
To obtain pure compounds such as benzene, toluene, and xylene from catalytically
produced reformates in the oil industry.
In the production of un hydrous acetic acid.
In the extraction of phenol from coal tar liquors.
In the metallurgical and biotechnology industries.
The extraction operation may be either a physical or a chemical operation.
Chemical operations have been classied as follows:
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(a) Those involving cat ion exchange such as, for example, the extraction of metals by
carboxylic acids;
(b) Those involving anion exchange, such as the extraction of anions involving a metal with
amines
(c) Those involving the formation of an additive compound, for example, extraction with
neutral oregano-phosphorus compounds.
A new technology -the use of supercritical or near supercritical uid as solvent.
In biotechnology, many of the usual organic solvents will degrade a sensitive product.

3.2.1. Extraction Processes

It can be carried out either as a batch or as a continuous process.
See the single-stage batch process illustrated in the fig below.
Mixing and separation occur in the same vessel.U-LIQUID EXTRACTION

3.2.2. Basic principles

To misunderstandings, especially in comparison to different sources. these

experiment instructions use the following designations for the liquids involved.
Transition component
Carrier liquid
Solvent
Liquid-liquid extraction in a beaker, with the following simplifications:
Only three liquids are involved.
The transition component transfers completely from the carrier liquid into the
solvent.
On the left is the beaker with two liquid phases. Carrier liquid and solvent
together form the solvent system.
The carrier liquid and solvent together form a phase boundary. They are
insoluble in one another. This is the condition so that separation into two
phases can occur after the actual extraction. Also required is a clear
density difference between the carrier liquid and solvent.

Before
Mixing
Settling
Figure3; Simplified representation of liquid-liquid extraction.

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After

In this example, the solvent is specifically heavier than the carrier liquid. Therefore the
carrier liquid floats on the solvent.
The carrier liquid "carries" the transition component; the transition
component is dissolved in the carrier liquid. The next step shows is the
mixing of the two liquid phases.
Droplets are formed; the specific surface area increases and the three liquids
are brought into intensive contact. In doing so, the transition component
transfers from the carrier liquid into the solvent.
Another condition for extraction is that the transition component is soluble in
the solvent.
After mixing, two further liquid phases form.

3.2.3 Equilibrium Data

The equilibrium condition for the distribution of one solute between two liquid phases is
conveniently considered in terms of the distribution law.
The ratio of the concentrations of the solute in the two phases is given by CE/CR =K.
Applicable only if both solvents are immiscible and if there is no association or dissociation
of the solute.
The addition of a new solvent to a binary mixture may lead to several mixtures: For low
concentration, the distribution law holds for non- reactive components.
(a)A homogeneous solution may be formed.
(b)The solvent may be completely immiscible with the initial solvent.
(c)The solvent may be partially miscible with the original solvent resulting in the formation
of one pair of partially miscible liquids.
(d)The new solvent may lead to the formation of two or three partially miscible liquids.

3.2.4 Factors influencing extraction performance

Extraction performance is the amount of usable substance extracted per unit of time. It
can be influenced by the following factors:

Differences in concentration
The greater the difference in concentration of the usable substance in the extraction material
and in the solvent, the greater the driving force when extracting. The difference in
concentration is increased by rapidly removing the dissolved extract from the surface of the
extraction material and frequently replacing the loaded solvent with fresh solvent.

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 Extraction surface area

The surface of the extraction material is proportional to the extracted quantity of
material.
The extraction performance increases as the extraction surface area rises. In practice,
this is achieved by crushing the extraction material.

Diffusion resistance
The diffusion resistance depends on the size of the particles, the porosity and the
penetrability of the extraction material for the solvent. The diffusion resistance
countering the dissolving of the extraction material should be as low as possible.

Temperature
The extraction performance is increased by higher temperatures. Higher temperatures
increase the thermal agitation, reducing the viscosity and thus accelerating the
dissolving of the usable substance.

3.3 Liquid-Gas Extraction (absorption)

Absorption is a basic procedure in thermal process engineering. Absorption is used to
separate one or more gas components from a gas flow using a solvent (detergent).
The Absorption unit provides a clear method of separating a gas mixture containing air and
CO2 by absorption in water.

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REFERENCES
Brockmann, M.C., 1973, Intermediate Moisture Foods, in W.B. van Arsdel, M.J. Copley,
A.I. Morgan (Eds.) Food Dehydration, The AVI Publishing Co., Westport.
Bruin, S., Luyben, K.Ch.A.M., 1980, Drying of Food Materials: A Review of Recent
Developments, pp. 155-216, in A.S. Mujumdar (Ed.) Advances in Drying, Vol. 1,
Hemisphere, Washington.

Book: principles of Refrigeration boy Roy J. Dossat

www.google.com
Process text book etc.

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