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Separation processes
Anam Saeed

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Synopsis of this lecture:


Separation processes Importance of mass transfer in Chemical Engineering What is Mass Transfer? What are mass transfer operations? Different mass transfer operations Course outline

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Separation process:
Is used to transform a mixture of substances into two or

more distinct products. The separated products could differ in chemical properties or some physical property, such as size, or crystal modification or other separation into different components. Separation processes can essentially be termed as mass transfer processes. The mixture at hand could exist as a combination of any two or more states: solid-solid, solid-liquid, solid-gas, liquid-liquid, liquid-gas, gas-gas, solid-liquid-gas mixture, etc.
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Mass Transfer:
Mass Transfer is the transport of material from one point to another in a single phase or from one phase to another generally in the presence of difference of conc., vapour pressure, in activity that provides the driving force. The mass transfer operations include such techniques as Distillation, gas absorption, adsorption, liquid extraction, leaching etc.

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Importance of Mass Transfer in Chemical Engineering:


Key part of unit operations Unit Operations; is the systematic study of the operations that

are helpful in the manufacturing of final product. Depending on the raw mixture, various processes can be employed to separate the mixtures. Many times two or more of these processes have to be used in combination to obtain the desired separation. Mass transfer operations are widely used in refinery, fertilizer, food industries etc.

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Different Mass Transfer Operations:


1. Distillation:

Is a unit operation or a physical separation process whereby two or more miscible liquids are separated using their volatility differences( differences in boiling points). Application: Water is distilled to remove impurities, such as salt from seawater.
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Distillation of water
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Absorption:
Unit operation and is mass transfer phenomena where the solute of a gas are removed by being placed in contact with a nonvolatile liquid solvent that removes the components from the gas.

Application:
The washing of ammonia from the mixture of ammonia and air by means of liquid water.

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Removal of SO2 gas


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Liquid Liquid Extraction:


This is the separation of a substance from a mixture by preferentially dissolving that substance in a suitable solvent. By this process a soluble compound is usually separated from an insoluble compound.

Application:
Acetic acid can be separated from water by using MIBK solvent.

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Leaching:
Leaching is concerned with the extraction of a soluble constituent from a solid by means of a solvent. Application: The process may be used either for the production of a concentrated solution of a valuable solid material, or in order to remove an insoluble solid, such as a pigment, from a soluble material with which it is contaminated.

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Soil leaching
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Different Mass Transfer Operations


Separation process Distillation Feed Liquid Separating Agent Heat Product Liquid + vapor Principle of separation Practical example

Difference in Fractionation relative of crude oil volatility Different Recovery of solubilities acetic acid of different species in the two liquid phases

Liquid liquid extraction

Liquid

Immiscible liquid

Two liquids

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Cont
Separation process Absorption Feed Separating Agent Liquid absorbent Product Principle of separation Practical example Mixture of gases Rich Difference in Good for liquid concentration recovery of and pure soluble gas gases Concent- Concentratio rated n difference solid Extraction of metals from ores

Leaching

solid

Liquid solvent

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Course outline:
Introduction to mass transfer operations; selection criteria among different separation processes; complete design calculations for equilibrium stage processes; distillation; Absorption; Leaching; liquid liquid extraction: design calculations for differential contractors; applications of mass transfer fundamentals, calculations of rate of mass transfer: limiting processes; case study taking environmental, manufacturing and economic effects
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Books:
Text books:
1. Coulson and Richardsons CHEMICAL ENGINEERING Volume 2 Fifth Edition 2. Unit operations of chemical Engineering by julian C. Smith. Warren L. McCabe Peter Harriott Fifth Edition 3. Mass transfer operations by Robert E. Treybal; 3rd edition

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Distillation
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Introduction:
The separation of liquid mixtures into their various components is one of the major operations in the process industries, and distillation, the most widely used method of achieving this end, is the key operation in any oil refinery. In this chapter consideration is given to the theory of the process, methods of distillation and calculation of the number of stages required for binary system.

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Distillation:
Is a unit operation or a physical separation process whereby two or more miscible liquids are separated using their volatility differences( differences in boiling points). Is simply defined as a process in which a liquid or vapour mixture of two or more substances are separated into its component fractions of desired purity by the application and removal of heat.

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Vapourliquid equilibrium:
The composition of the vapour in equilibrium with a liquid of given composition is determined experimentally using an equilibrium still. The results are conveniently shown on a temperaturecomposition diagram.

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For distillation purposes it is more convenient to plot y against x at a constant pressure, since the majority of industrial distillations take place at substantially constant pressure. This is shown in Figure 11.4

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Partial vaporization and partial condensation:


If a mixture of benzene and toluene is heated in a vessel, closed in such a way that the pressure remains atmospheric and no material can escape and the mole fraction of the more volatile component in the liquid, that is benzene, is plotted as abscissa, and the temperature at which the mixture boils as ordinate.

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Continue..
Partial vaporisation of the liquid gives a vapour richer in the more volatile component than the liquid If the vapour initially formed, as for instance at point E, is at once removed by condensation, then a liquid of composition x3 is obtained, represented by point C. The step BEC may be regarded as representing an ideal stage, since the liquid passes from composition x2 to a liquid of composition x3. Thus, partial condensation brings about enrichment of the vapour in the more volatile component in the same manner as partial vaporisation.
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Daltons law:

By Daltons law of partial pressures, P = PA, that is the total pressure is equal to the summation of the partial pressures. Since in an ideal gas or vapour the partial pressure is proportional to the mole fraction of the constituent, then: PA = yAP

Raoults law:
For an ideal mixture, the partial pressure is related to the concentration in the liquid phase by Raoults law which may be written as: PA = PAxA
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Example 11.1
The vapour pressures of n-heptane and toluene at 373 K are 106 and 73.7 kN/m2 respectively. What are the mole fractions of n-heptane in the vapour and in the liquid phase at 373 K if the total pressure is 101.3 kN/m2?

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Methods of distillation:
There are three main methods used in distillation practice. (a) Differential distillation. (b) Flash or equilibrium distillation, and (c) Rectification.

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Differential distillation:
The simplest example of batch distillation is a single stage, differential distillation, starting with a still pot, initially full, heated at a constant rate. In this process the vapour formed on boiling the liquid is removed at once from the system. Since this vapour is richer in the more volatile component than the liquid. it follows that the liquid remaining becomes steadily weaker in this component, with the result that the composition of the product progressively alters. Thus, whilst the vapour formed over a short period is in equilibrium with the liquid, the total vapour formed is not in equilibrium with the residual liquid.
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Cont.
At the end of the process the liquid which has not been vaporised is removed as the bottom product. As this process consists of only a single stage, a complete separation is impossible unless the relative volatility is infinite.

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Flash or equilibrium distillation:


Flash or equilibrium distillation, frequently carried out as a continuous process, consists of vaporising a definite fraction of the liquid feed in such a way that the vapour evolved is in equilibrium with the residual liquid. The feed is usually pumped through a fired heater and enters the still through a valve where the pressure is reduced. The still is essentially a separator in which the liquid and vapour produced by the reduction in pressure have sufficient time to reach equilibrium. The vapour is removed from the top of the separatorand is then usually condensed, while the liquid leaves from the bottom.
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Example 11.6:
An equimolar mixture of benzene and toluene is subjected to flash distillation at 100 kN/m2 in the separator. Using the equilibrium data given in Figure 11.9, determine the composition of the liquid and vapour leaving the separator when the feed is 25 per cent vaporised. For this condition, the boiling point diagram in Figure 11.10 may be used to determine the temperature of the exit liquid stream.

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Rectification:
In the two processes considered, the vapour leaving the still at any time is in equilibrium with the liquid remaining, and normally there will be only a small increase in concentration of the more volatile component. The essential merit of rectification is that it enables a vapour to be obtained that is substantially richer in the more volatile component than is the liquid left in the still. This is achieved by an arrangement known as a fractionating column which enables successive vaporisation and condensation.

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Fractionating Column:
Is a series of stills placed one on top of the other. As vaporization occurs, the lighter components of the mixture moves up to the tower and are distributed on the various trays. Heavier components goes down lighter components goes up. The feed is introduced at the middle section of the column at intermediate tray where the liquid has the same composition as that of feed.

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Types of section:
Rectifying section:
The part of column above the feed point is known as rectifying section.

Stripping section:
The part of the column below the feed point is known as stripping section.

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Major components of a typical distillation are:


Vertical Shell Column internals Reboiler Condenser Reflux Drum
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Distillation Equipments

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Distillation Equipments

Continuous distillation:
liquid mixture is continuously (without interruption) fed

into the process and separated fractions are removed continuously as output stream. The liquid in the base of column heated, and the vapour rises to the bottom try. where it is partially condensed and partially vaporized. The operation of partial condensation of raising vapour and partial vaporization of the reflux liquid is repeated on each try.
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Vapours are moving upward while the liquid is flowing downward in the distillation column and mixing of vapour and liquid take place on each tray.

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Continue.
Vapour of composition yt (MVC) from the top try is

condensed to give top product D and the reflux R, both of same composition yt. The vapour rising from an ideal tray will be in equilibrium with the liquid leaving, although in practice smaller degree of enrichment occur.

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The system tends to reach equilibrium on each tray:


Some of the less volatile component condenses from the

rising vapour into the liquid thus increasing the concentration of the more volatile component in the vapour. Some of the MVC is vaporized from the liquid on the tray thus decreasing the concentration of the MVC in the liquid.

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Equimolar counter diffusion:


The number of molecules passing in each direction from vapour to liquid and in reverse is approximately the same since the heat given out by one mole of the vapour on condensing is approximately equal to the heat required to vapourize one mole of the liquid.this is called Equimolar counter diffusion.

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Constant molar overflow:


If the molar heat of vaporisation are approximately constant, the flow of liquid and vapour in each part of the column will not vary from tray to tray. This concept is called constant molar overflow.

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Number of plates required in a distillation column:


In order to develop a method for the design of distillation units to give the desired fractionation, it is necessary, in the first instance, to develop an analytical approach which enables the necessary number of trays to be calculated. First the heat and material flows over the trays, the condenser, and the reboiler must be established. Thermodynamic data are required to establish how much mass transfer is needed to establish equilibrium between the streams leaving each tray. The required diameter of the column will be dictated by the necessity to accommodate the desired flowrates, to operate within the available drop in pressure, while at the same time effecting the desired degree of mixing of the streams on each tray.
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Heat balance over a plate:

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Assumptions:
The heat losses will be small and may be neglected, and

for an ideal system the heat of mixing is zero. For such mixtures, the molar heat of vaporization may be taken as constant and independent of the composition. V =VN so that the molar vapour flow is constant up the column unless material enters or is withdrawn from the section. The temperature change from one plate to the next will be small, and HLn may be taken as equal to H n+1.
N-1

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Cont.
Ln = Ln+1,so that the moles of liquid reflux are also constant

in this section of the column. Thus Vn and Ln are constant over the rectifying section, and Vm and Lm are constant over the stripping section. on the basis of these assumptions there are two methods to find out the number of plates 1. LewisSorel method 2. The method of McCabe and Thiele

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Calculation of number of plates using the LewisSorel method


A binary feed F is distilled to give a top product D and a bottom product W, with xf , xd, and xw as the corresponding mole fractions of the more volatile component, and the vapour Vt rising from the top plate is condensed, and part is run back as liquid at its boiling point to the column as reflux, the remainder being withdrawn as product, then a material balance above plate n.

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The method of McCabe and Thiele

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Thank you

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