ADIGRAT UNIVERSITY

COLLEGE OF ENGINEERING AND TECHNOLOGY

DEPARTMENT OFCHEMICAL ENGINEERING
PROJECT ON:DRYING OF SOLID, CRYSTALLIZATION AND
EXTRACTION
COURSE TITLE: MASS TRANSFER UNIT OPRATION
COURSE CODE: ChEg3114
PREPARED BY NETWORK THREE
NAME

IDNO

SECTION

1. ETAYHAILU ........................................................RET0457/06

ONE

2. H/MARIAM ASGEDOM .................................................RET0748/06

ONE

3. KIROS G/MEDHIN...........................................................RET0937/06

ONE

4. LETU DESALEGN ...........................................................RET0969/06

ONE

5. LICHIYA ALEM ...............................................................RET0971/06

ONE

6. WASIE KEBRIE ...............................................................RET1578/06

ONE

SUBMITTED TO:
INSTRUCTOR H/MICHAEL TSEGAY
SUBMISSION DATE:
WEDNSDAY25, 09, 2008 E.C

ACKNOWLEDGMENT
First and for most we would like to say thanks for our instructor H/MICHAEL T. to give this
project and the formats of the project. Moreover, for all group members and for our advisor that
supports by giving idea and economical aid until the project is complete.

ABSTRACT
The aim of this project is to understand the concept of drying of solids, crystallization, and
extraction. Drying is the removal of moisture from a substance. Psychrometry is that branch of
engineering science, which deals the study of moist air that dry air mixed with water vapor or
humidity. In addition, to discuss the psychrometric term like; humidity, wet bulb temperature,
dew point depression and so on. Crystallization is also a chemical solidliquid separation
technique, in which mass transfer of a solute from the liquid solution to a pure solid crystalline
phase occurs. In chemical engineering, crystallization occurs in a crystallizer. Finally,
Extraction is the withdrawing of active agent or a waste substance from a solid or liquid mixture
with a liquid solvent. The main area of extraction is for hydro metallic processes, for
pharmaceutical industry (producing active agent), for petroleum industry (production of
monomers and aromatic) and for cleaning of wastewater to separate solved compounds

II

LIST OF CONTENT
Contents ...................................................................................................................................... Page
Acknowledgment ............................................................................................................................... I
Abstract ........................................................................................................................................... II

List of figures ................................................................................................................................. III

1. Drying of solids ........................................................................................................................ 1
Introduction ............................................................................................................................... 1
Objectives .................................................................................................................................. 1

1.1 Gas vapor mixture ................................................................................................................ 2

1.2 psychrometric terms ............................................................................................................. 3
1.3 psychrometric chart .............................................................................................................. 4
Conclusion ........................................................................................................................... 6
2. Crystallization............................................................................................................................. 7
Introduction ............................................................................................................................... 7
Objective .................................................................................................................................... 7

2.1 Crystallization Fundamentals ................................................................................................ 8

2.2 Solid-Liquid equibria ........................................................................................................... 8
2.2.1

Solubility and Phase Diagrams ................................................................................. 8

2.2.2

Solubility and saturation ......................................................................................... 10

2.2.3

Crystal nucleation .................................................................................................. 10

2.2.4

Crystal growth....................................................................................................... 12

2.3 Crystallization from melts .................................................................................................. 13

2.3.1

Basic techniques .................................................................................................... 13

2.3.2

Multistage-processes ............................................................................................. 13
Conclusion ............................................................................................................ 14

3. Extraction ................................................................................................................................. 15
Introduction ............................................................................................................................. 15
Objectives ................................................................................................................................. 15

3.1 Definition of Extraction ..................................................................................................... 16

3.2 Selection of the solvent ...................................................................................................... 16
Conclusion ......................................................................................................................... 17
Reference .......................................................................................................................... 18

LIST OF FIGURE

PAGE

Figure1.1 Psychrometric chart ............................................................................................................. 4

Figure1.2 Various air-conditioning processes .................................................................................... 5
Fig 2.1 Solubility curves for substances with two polymorphs I and II (2) .................................... 10
Fig 2.2 Effect of super saturation on the rates of homogeneous and heterogeneous nucleation ... 12
Fig 2.3 Concentration driving forces for crystal growth from solution .......................................... 13

III

CHAPTER ONE
1. DRYING OF SOLID
Introduction
Drying is perhaps the oldest, most common and most diverse of chemical engineering
unit operations. Drying of solid is a mass transfer process consisting of the removal of water or
another solvent by evaporation from a solid, semi-solid or liquid. This process is often used as a
final production step before selling or packaging products. To be considered "dried", the final
product must be solid. The separation operation of drying converts a solid, semi-solid or liquid
feedstock into a solid product by evaporation of the liquid into a vapor phase via application of
heat. In the special case of freeze drying, which takes place below the triple point of the liquid
being removed, drying occurs by sublimation of the solid phase directly into the vapor phase.
The psychrometry is that branch of engineering science, which deals the study of moist air that
dry air mixed with water vapor or humidity. Generally drying is the removal of moisture from a
substance.

Objectives:

To remove water present in liquid foods by evaporation

To yield solid products
To extend the shelf-life of foods by reducing their water activity
Differentiate between dry air and atmospheric air.
Differentiate between the specific and relative humidity of atmospheric air.
Define the dew-point temperature of atmospheric air

1.1Gas vapor mixture

When we are dealing with a gasvapor mixture, however, the vapor may condense out of
the mixture during a process, forming a two-phase mixture. This may complicate the analysis
considerably. Atmospheric air normally contains some water vapor (moisture). The dry-air
contains no water. Although the amount of water vapor in the air is small, it plays a major role in
human comfort and thus in air-conditioning applications.
The psychrometry is that branch of engineering science, which deals with the study of moist air
that is dry air mixed with water vapor or humidity. It is also includes the study of behavior of dry
air and water vapor mixture under various sets of conditions. Though the earth's atmosphere is a
mixture of gases including nitrogen (N2), oxygen (O2), argon (Ar) and carbon dioxide (CO2),
yet for the purpose of psychrometry, it is consider a mixture of dry air and water vapor only.
Psychrometry is concerned with determination of the properties of gas-vapor mixtures. The airwater vapor system is by far the system most commonly encountered. The purpose of
psychrometry is a mixture of dry air and water vapor consider only.
The temperature of air in air-conditioning applications ranges from about -10 to 50C. In
that range both dry air and atmospheric air (including water-vapor) can be treated as ideal
gas, with negligible error. Thus the ideal-gas relation PV = RT can be applied. The partial
pressures of atmospheric air are:
Also, one can write:

Note that since air is considered as an ideal-gas, the enthalpy of air (both water-vapor and dry
air) is only a function of temperature, at the temperature range of interest, i.e., -10 to 50C.
Taking 0C as the reference temperature; with the constant-pressure specific for dry-air (in the
range of interest) cp= 1.005 kJ/kg.C; one obtains:
hdry air = cp T = (1.005 kJ/kg. C) T (kJ/kg)
2

1.2 Psychrometric Terms

Psychrometrics is the study of the physical and thermodynamic properties of air-water
mixtures. Some terms used in psychrometrics are:
Dry AirAir not containing any water vapor.
Moist AirA mixture of dry air and water vapor.
Air MixtureA mixture of dry air and water vapor.
Dry Bulb Temperaturethe temperature measured by an ordinary thermometer.
Wet Bulb Temperaturethe lowest temperature to which an air mixture can be cooled
solely by the addition of water.
Dew Point Temperaturethe temperature at which moisture starts to condense from air
cooled at constant pressure and humidity ratio.
Humidity RatioWeight of water vapor in pounds per pound of dry air or grains of
water vapor per pound of dry air or kilograms of water vapor per kilogram of dry air
expressed as a decimal. This quantity may also be called Absolute Humidity.
Relative Humidity (RH)the ratio of actual water vapor pressure to the vapor pressure
of saturated air at the same dry bulb temperature. RH is expressed as a percentage.

1.3 Psychrometric Chart

The state of the atmospheric air at a specified pressure is completely specified by two

independent intensive properties. Psychrometric charts present the moist air properties;
they are used extensively in air-conditioning
conditioning applications.

Figure1.1 Psychrometric chart.

Basic features of psychrometric chart are:

The dry bulb temperatures are shown on the horizontal axis.
The specific humidity is shown on the vertical axis.
The curved line at the left end of the chart is the saturation line. All the saturated air
states are located on this curve. Thus, it also represents the curve of relative
humidity100%.
100%. Other constant relative humidity curves have the same general shape.

 Lines of constant wet-bulb

bulb temperature have a downhill appearance to the right.
Lines of specific volume also have downhill
downhill appearance to the right with steeper slopes.
Lines of constant enthalpy lie very near to the constant wet-bulb
bulb temperature, thus ((in
some charts) lines of constant wet-bulbs
wet
are used as constant-enthalpies.
enthalpies. For saturated
air, the dry-bulb, wet-bulb,
bulb, and
an dew-point temperatures are identical.
Thus the dew-point
point temperature of atmospheric air can be determined by drawing a
horizontal line to the saturated curve.

Air-conditioning
conditioning processed
Maintaining a living space or an industrial facility at the desired temperature and humidity
requires some processes called air-conditioning
air conditioning processes. These processes include simple
heating (raising the temperature), simple cooling (lowering the temperature),
re), humidifying
(adding moisture), and dehumidifying (removing moisture).

Figure1.2 Various air-conditioning

conditioning processes
Most air-conditioning
conditioning processes can be modeled as steady-flow
steady
processes,
and thus the mass balance relation mn
= moutcan be expressed for dry air and water as
Mass balance for dry air: m ain = m aout
Mass balance for water:

m win = m wout

(kg/s)
or ma
in = ma out
out

Conclusion
Drying is a mass transfer process consisting of the removal of water or another solvent by
evaporation from a solid, semisolid, or liquids. Generally drying is defined as the application of
heat under controlled condition. Psychrometry is that branch of engineering science, which deals
the study of moist air that dry air mixed with water vapor or humidity. There are so many
psychrometric terms; like humidity, relative humidity, absolute humidity, wet bulb dispersion,
and so on. Psychrometric charts present in a graphical form physical property data for gas
systems involving one or more non-condensing gas components and a single condensing vapor
component.

CHAPTER TWO
2.CRYSTALLIZATION
Introduction
Crystallization is a separation and purification technique employed to produce a wide variety
of materials. Crystallization may be defined as a phase change in which a crystalline product is
obtained from a solution. A solution is a mixture of two or more species that form a homogenous
single phase. Solutions are normally thought of in terms of liquids, however, solutions may
include solids suspension. Typically, the term solution has come to mean a liquid solution
consisting a solvent, which is a liquid, and a solute, which is a solid, at the conditions of interest
.The solution to be ready for crystallization must be supersaturated. A solution in which the
solute concentration exceeds the equilibrium (saturated) solute concentration at a given
temperature is known as a supersaturated solution. There are four main methods to generate
super saturation that are the following:

Temperature change (mainly cooling),

Evaporation of solvent,

Chemical reaction, and

Changing the solvent composition

Objective
To separate a solute from a solvent
For purification and separation process
For recovery of solid materials
To form a liquid solution based on difference in solute concentration and its solubility at
a certain temperature.

2.1 Crystallization Fundamentals

Crystallization may be defined as a phase change in which a crystalline product is obtained
from a solution. A solution is a mixture of two or more species that form a homogenous single
phase. Solutions are normally thought of in terms of liquids, however, solutions may include
solids suspension. In evaluating a crystallization operation, data on phase equilibria are important
as this indicates the composition of product that might be anticipate and the degree of super
saturation gives some idea of the driving force available. The rates of nuclei formation and
crystal growth are equally important as these determine the residence time in, and the capacity of
a crystallizer. These parameters also enable estimates to be made of crystal sizes, essential for
the specification of liquor flows through beds of crystals and also the mode and degree of
agitation required.

2.2 Solid-Liquid equilibrium

This section provides an overview of solid-liquid equilibrium and the type of information useful
to crystallization that can be glean from their representation in the form of phase diagrams.
Different types of idealized phase and solubility diagrams shall be discuss together with
associated phenomena.

2.2.1 Solubility and Phase Diagrams

A solution is a homogeneous mixture of two or more chemical species. For a liquid
solution, saturation is reach when the liquid phase, in contact with the solid phase, no longer
changes its composition. A saturated solution therefore has a constant composition that 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. However, the
temperature dependence (and the pressure dependence providing the difference is sufficiently
large, see [Moritoki] of the solubility can be considerable and it is therefore important to state the
temperature for which the solubility is reported even under normal conditions. In the
following, the discussion will focus on two component systems only.
Phase transformations
Metastable crystalline phases frequently crystallize to a more stable phase in accordance with
Ostwalds rule of stages, and the more common types of phase transformation that occur in
crystallizing and precipitating systems include those between polymorphs and solvates.
Transformations can occur in the solid state, particularly at temperatures near the melting point
of the crystalline solid, and because of the intervention of a solvent. A stable phase has a lower
solubility than a metastable phase.

Fig 2.1 Solubility curves for substances with two polymorphs I and II (2)

Whilst transformation cannot occur between the metastable (I) and (I) in the monotropic system
in the temperature range shown, it is possible above the transition temperature in an enantiotropy
system.

2.2.2. Solubility and saturation

Super saturation
A solution that is in thermodynamic equilibrium with the solid phase of its solute at a given
temperature is a saturated solution, and a solution containing more dissolved solute than that
given by the equilibrium saturation value is said to be supersaturated.
supe
Solution concentrations
may express as mass of anhydrate/mass of solvent or as mass of hydrate/mass of free solvent.

2.2.3. Crystal nucleation

Nucleation, the creation of crystalline bodies within a supersaturated fluid, is a complex event,
since nuclei may be generate by many different mechanisms. The most nucleation classifications
scheme distinguishes between primary nucleation - in the absence
nce of crystals and secondary
nucleation - in the presence of crystals.
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Primary nucleation
Classical theories of primary nucleation are bases on sequences of bimolecular collisions in
addition, interactions in a supersaturated fluid that result in the build-up of lattice-structured
bodies which may or may not achieve thermodynamic stability. Such primary nucleation is knows as
homogeneous, although the terms spontaneous and classical have also been used. Primary nucleation

may be initiating by suspended particles of foreign substances, and this mechanism has referred
to as heterogeneous nucleation. In industrial crystallization, most primary nucleation is almost
certainly heterogeneous, rather than homogeneous, in that it is induced by foreign solid particles
invariably present in working solutions.
Homogeneous nucleation
Is a consideration of the energy involved in solid-phase formation and in creation of the surface of an
arbitrary spherical crystal of radius r in supersaturated fluids.

Heterogeneous nucleation
The presence of foreign particles or hetero nuclei enhances the nucleation rate of a given
solution, and equations similar to homogeneous nucleation have been propose to express this
enhancement.
Secondary nucleation
Secondary nucleation can be the definition, take place only if crystals of the species under
consideration are already present. Since this is usually the case in industrial crystallizers,
secondarynucleation has a profound influence on virtually all industrial crystallization processes.

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Fig 2.2 Effect of super saturation on the rates of

of homogeneous and heterogeneous nucleation

2.2.4. Crystal growth

In simple terms, the crystallization process may be consider to take place in two stages a
diffusional step ions or molecules at the crystal surface are deposited in which solute is
transported from the bulk fluid through the solution boundary
boundary layer adjacent to the crystal
surface, and a deposition step in which adsorbed solute and integrated into the crystal lattice.

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Fig 2.3 Concentration driving forces for crystal growth from solution

2.3. Crystallization from melts

2.3.1. Basic techniques
A melt is a liquid or a liquid mixture at a temperature near its freezing point and melt
crystallization is the process of separating the components of a liquid mixture by cooling until
crystallized solid is deposited from the liquid
liquid phase. Where the crystallization process is used to
separate, or partially separate, the components, the composition of the crystallized solid will
differ from that of the liquid mixture from which it is deposited
Two basic techniques of melt crystallization
crystalli
are:
(a) Gradual deposition of a crystalline layer on a chilled surface in a static or laminar flowing
melt, and
(b) Fast generation of discrete crystals in the body of an agitated vessel

2.3.2. Multistage-processes
processes
A single-stage
stage crystallization process may not always achieve the required product purity and
further separation, melting, washing, or refining may be required. Two approaches are used:
a) A repeating sequence of crystallization, melting, and re-crystallization;
re
b) A single crystallization step followed by countercurrent contacting of the crystals with a
relatively pure liquid stream.
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Conclusion
Crystallization is a thermal separation, and purification process that yields a solid product from a
melt, from a solution or from a vapor. As for all thermal separations, non-equilibrium conditions
are required as a driving force for the process. Crystallization is used as some stage in nearly all
process industries as a method of production, purification, or recovery of solid materials.
Crystallization provide a comprehensive over view of the subject and will prove in valuable to
all chemical engineer and industrial chemists in the process industries are well as crystallization
workers and students in industry and academia. Two basic techniques of melt crystallization are
gradual deposition of a crystalline layer on a chilled surface in a static or laminar flowing melt
and Fast generation of discrete crystals in the body of an agitated vessel.

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CHAPTER THREE

3.EXTRACTION
Introduction
Extraction is a separation of the constituents of a liquid solution by contact with another
insoluble liquid. The liquid which is added to the solution to bring about the extraction is known
as the solvent. Extraction is a separation process aiming to purify the feed or to recover one or
more compounds from it. Since the mass transfer is much slower than the reaction rate. The
liquid-liquid extraction is a mass transfer process betweentwo phases. One liquid phase is the
feed consisting of a solute and a carrier. The other phase is the solvent. The extraction is
understood to be a transfer of the solute from the feed to the solvent. During and at the end of the
extraction process, the feed deprived of solute becomes a raffinate and the solvent turns into
extract. Depending on the phases following types of extraction, exist:
Solid-liquid extraction (leaching)
Liquid-liquid extraction
Gas-liquid extraction also called absorption.

The main area of extraction is for hydro metallic processes, for pharmaceutical industry
(producing active agent), for petroleum industry (production of monomers and aromatic) and for
cleaning of wastewater to separate solved compounds.
Objectives:
It is aiming to purify the feed or to recover one or more compounds from it.
For separation of the constituents of a liquid solution by contact with another
insoluble liquid.

15

3.1 Definition of Extraction

Extraction a separation of the constituents of a liquid solution by contact with another insoluble
liquid.The solution which is to be extracted is called the feed. The solvent-richen product of the
operation is called the extract and the residual liquid from which the solute is separated is called
the raffinate.
The following are some examples techniques of extraction.
The separation of aromatics from kerosene based fuel oils,
The production of fuels in the nuclear industry and
The separation of penicillin from fermentation mixtures

3.2 Selection of the solvent

The solvent for extraction has to withdraw the active agent from a mixture. Any solvent can be
select based on the following points;
Selectivity: only the active agent has to be extract and no further substances, which
means that a high selectivity is required.
Capacity: To reduce the amount of necessary solvent the capacity of the solvent has to
be high.
Difference in density: After extraction, the two phases have to be separate in a separator
and for this, a high difference in density is positive.
Low price and no or low toxicity

16

Conclusion
Extraction is the withdrawing of active agent or a waste substance from a solid or liquid mixture
with a liquid solvent. The solvent is not or only partial miscible with the solid or the liquid.
Extraction types depend on phases are Solid-liquid extraction, Liquid-liquid extraction and gasliquid extraction. Extractions are classifies in to two steps, which are single step extraction and
multi-step extraction

17

Reference
Drying of solids ,Oldrich Holecek, Martin Kohout
Extraction, lecturer, Dr.Gamse
NONHEBEL,G. and MOSS,A.A.H.:Drying of Solids in the Chemical Industry(Butterworth,
London, 1971).
Psychrometry, Ray A. Bucklin and Dorota Z. Haman2
SHERWOOD,T.K. and PIGFORD,R.L.: Absorption and Extraction, 2nd ed. (mcgraw-Hill, New
York,1952).
TREYBAL, R.E.: Liquid Extraction.2nd ed. (mcgraw-Hill, New York, 1963).

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