Class 1

We know that all Process Industries manufacture products from a variety of starting
materials called as raw materials. In these Industries the raw materials are pre-
treated and conversion takes place in reactor and the separation of products from by-
products is carried out and finally purification of products takes place. The reactor
where the transformation takes place is an important step and all the stapes that are
prior to the main process is called as Upstream processing (raw material preparation)
and all the steps that follows the main process is called as downstream processing(
or product purification) For example let us consider the manufacture of Penicillin the
main process is the fermentor where a medium of corn liquor, yeast and other
substrates are added and made to react for a long period, all the steps preceeding for
preparing the feed materials is called as upstream processing and all the steps
involved in extraction and purification after fermentation is called as downstream
processing. In all the down stream and upstream processes only a physical change
(like changing the concentration, dissolution etc.,) is involved and all these operations
are called as unit operations.
These unit operation accounts for 50-90% of the capital investment
In all Unit operations (Distillation, Absorption, Extraction, Crystallization, Drying,
Mixing and Evaporation Operations) only a physical change occurs and no reactions
are involved
In a process in which transformation or modification inputs occurs is generally
classified as Unit processes and unit Operations. Unit operations are generally used
for separations and purification. Examples of Unit Operations are Evaporation,
Drying, crystallization etc. Unit operations do not involve chemical reactions (does
not involve any chemical changes).

A chemical process consists of a combination of chemical reactions such as synthesis,
calcination, ion exchange, electrolysis, oxidation, hydration and operations based on
physical phenomena such as evaporation, crystallization, distillation and extraction

Bioprocess Principles and Calculations

After completion of the course students must be able to write the material balance
equation for various U O and solve them also. He must also be capable of doing
fundamental calculations for system involving by pass, recycle and passing.
In a process there may be only a physical change or physical change with chemical.
If only physical change- Unit operations
Physical changes and chemical Unit Process
All the fundamental calculations used in these operations is called Material Balance
If it is for U O it is materials balance without reaction and if it is for Unit process it as
materials balance calculations with reactions
For writing material balance equation and solving them we must understand the various
types of operations. Based on variation of the process parameters with time it is
classified as Steady State and unsteady state operation . In a Steady state process
the variables(level, flow rate, concentrations etc.,) does not change with time.
If we take a snapshot at time intervals, all the variables (level, flow rate) will have the
same values as in the first snapshot.
For example if you observe the tank to your left there is an inlet and outlet , if flow rates
in both are of same, under this condition the level of the tank will always remain
constant. This is a study state process,on the other hand if you consider the tank to your
right ,where there is no inflow and If water is allowed to flow, as the time increases the
level comes down and also the flow rate decreases this is an unsteady state process
also called as transient conditions. (If you take a snap short the level varies with time)

Based on the modes of operation continuous batch and semi batch.
In continuous operation materials enter and leave uninterrupted and in a batch
operation materials are fed reacted and discharged. Semibatch operation is a
combination of both
An RO system is usually designed for continuous operation. The operating conditions of
every membrane element in the plant are constant with time. Figure illustrates the
continuous process mode which is designed for continuous operation with constant permeate flow
and pressure (Constant system recovery). Variations in feed water temperature and fouling effects are
compensated for by adjusting the feed pressure.


In certain applications, when relatively small volumes (batches) of special feed waters
occur discontinuously, e.g., wastewater or industrial process solutions, the
subsequently. The permeate is removed and the concentrate is recycled back to the
tank. At the end of the batch process, a small volume of concentrate remains in the feed
tank.
batch operation mode.
The semi-batch mode is a modification of the batch mode. In semi-batch mode of
operation the feed tank is refilled with feed water when already process is in operation.
The batch is terminated with the feed tank full of concentrate. This advantage is a
smaller tank can be e used.

Figure on the left is a continuous distillation column used for distilling large quantities of
feed and to the right is a batch process for small
Most of the industrial processes operate in a steady state wher ,Input = Output . I will
discuss a pre basic problem to understand Degree of freedom Analysis for a state state
non reactive species Degree of freedom Analysis allows us to know before hand or
before going into the calculations ., whether the problem is solvable or not
In this process you have two species A and B
Feed splits into a Top product and a Bottom product In the top stream we have 450
kg/hr of A coming out but we do not know as how much B comes out
Similarly in the bottom stream we have 475 kg/hr of B coming out but we do not know
as how much A comes out
We do a balance for species A and B and evaluate the unknowns
D F = Unknowns number of equations
DF= 0 ( solution is possible)
In the previous examples
Number of unknowns x,y is 2
Number of equations 2 (one for each species A and B)
DF=0
DF<0 (Unknowns are more which means we have to write one more equation)
DF>0 ( no of equations are more which is dangerous then we have to relook before
solving)

This problem is on making of 1% fat Skimmed milk from whole milk of 5% by removing
some of the fat from the whole milk. The composition of various constituent are listed ,
solving this problem makes us to understand the concept of material balance
The law of conservation of mass, which states that mass can neither be created nor
destroyed. Total mass of input is equal to total mass of output. Thus material balance
is an expression of law of conservation of mass in accounting terms
Accumulation is usually the rate of change of holdup of material within the system. If material is
increasing, accumulation is positive; if it is decreasing, it is negative. If the system does not
change with time, it is said to be at steady state, and the net accumulation will be zero.
The generation and consumption of material are the consequences of chemical reactions. If
there is no chemical reaction, the production and consumption terms are typically zero.









Application for Bio process calculation without reaction
Unsteady with no reaction steady state or
Flow in =Flow out + Accumulation
Steady-state process -- no accumulation
Flow in =Flow out


And how the generalized equation are simplified for individual operations.
Development of flow diagrams is important for process calculations. I will briefly explain
them and an introductions to processes missing bypass, single and passing will be
mentioned and I will conclude with a reason

We all know that industrial manufacture products from a variety of starting materials
called as raw materials, in these industries there exists a main process and all the
steps that are prior to the main process is called as upstream processing and all the
steps after the main process is called as down stream processes let me consider the
manufactures of penicillin for example
Material balance calculations serve the following purposes:
1. They help us know the amount and composition of each stream in the process.
2. The calculations obtained form the basis for energy balances which is very
important for design
3. It helps to make technical and economic evaluation of the process and process
units from the knowledge of material and energy consumption and product yield
obtained.
4. We can quantitatively know the environmental emissions of the process.
In mass balance calculations, we begin with two assumptions
There is no transfer of mass to energy
Mass is conserved for each element or compound on either molar or
weight basis
You may write balances on total mass, total moles, mass of a compound, moles of an
atomic species, moles of a compound, mass of a species, etc.
Some chemical processes are quite simple; others such as oil refineries and
petrochemical plants can be very complex. The process description of some processes
could take a lot of text and time to read and still not yield 100% comprehension. Errors
resulting from misunderstanding processes can be extremely costly.
To simplify process description, flow diagrams also known as flow sheets are used. A
flow diagram is a road map of the process, which gives a great deal of
information in a small space. Chemical engineers use it to show the sequence of
equipment and unit operations in the overall process to simplify the visualization of the
manufacturing procedures and to indicate the quantities of material and energy
transferred.
A flow diagram is not a scale drawing but it:
pictorially identifies the chemical process steps in their proper/logical sequence
includes sufficient details in order that a proper mechanical interpretation may be
made
wo types of flow diagrams are in common use, namely, the block diagrams and the
process flow diagrams.
This is a schematic diagram, which shows:
what is to be done rather than how it is to be done. Details of unit
operations/processes are not given
flow by means of lines and arrows
unit operations and processes by figures such as rectangles and circles
raw materials, intermediate and final products




Based on how the process parameters varies with time it is classified as


In a Steady state process the variables(level, flow rate, concentrations etc.,) does not
change with time.
If we take a snapshot at time intervals, all the variables (level, flow rate) will have the
same values as in the first snapshot.
In Un steady-state (Transient) process variables changes with time. Every time we
take a snapshot, the variables have different values than in the first snapshot.
Based on how the process is carried out (mode of operation)it is classified as



Continuous RO proces


RO system for water purification is usually designed for continuous
operation.
The operating conditions of every membrane element in the plant are
constant with time
Batch RO process
When small volumes (batches) feed waters occur discontinuously, eg,
waste water or industrial process solutions the batch operation mode is
preferred.
The permeate is removed and the concentrate is recycled back to the tank.
At the end of the batch process, a small volume of concentrate remains in
the feed tank.


Semi-batch process
Is a process that has some characteristics of continuous and batch
processes
In semi-batch mode of operation the feed tank is refilled with feed water
during operation.
The batch is terminated when the feed tank is full of concentrate.
The advantage is it allows a smaller tank to be used



Degree of Freedom (D F ) analysis
D F for a non reactive species
D F = Unknowns number of equations
DF= 0 ( solution is possible)
In the previous examples
Number of unknowns x,y is 2
Number of equations 2 (one for each species A and B)
DF=0
DF<0
DF>0
Skimmed milk is prepared by removing some of the fat from the whole milk.
The composition of whole milk is
Water 84%
Protein 4%
Carbohydrates 5%
Ash 2%
Fat 5%
If fat is removed and skimmed milk has only 1% of fat find the composition
of the skimmed milk
Basis of 100kg of Whole milk
Let X be the amount of fat removed






The weight of Skimmed milk will be
Water 84 Kg
Protein 4 Kg
Carbohydrates 5 Kg
Ash 2 Kg
Fat 5 - x Kg
------------------------------
Total 100 x Kg





% 1
100
5
is milk skimmed in the present Fat
=

kg
x
x
1 100
100
5
=

x
x



Weight of Fat removed
0.01 (100- )= 5 - x
1-0.01 = 5 - x
x- 0.01 = 5-1
0.99 x = 4


Weight of skimmed milk after fat removal

Water 84 kg 84kg 84kg
Protein 4 kg 4 kg 4kg
Carbohydrates 5 kg 5 kg 5kg
Ash 2 kg 2 kg 2kg
Fat 5-x kg 5-4.04 kg 0.96kg

100-4.04

95.96kg




Weight % of skimmed milk

.01
100
5
=

x
x
kg 04 . 4
99 . 0
4
= = x
0.01
95.96
0.96
Check =
87.5% 100
95.96
84
water = =
% 2 . 4 100
96 . 95
4
Protein = =
% 2 . 5 100
96 . 95
5
tes Carbohydra = =
% 1 . 2 100
96 . 95
2
Ash = =
% 1 100
96 . 95
96 . 0
Fat = =

The law of conservation of mass, which states that mass can neither be
created nor destroyed. Total mass of input is equal to total mass of output.
Thus material balance is an expression of law of conservation of mass in
accounting terms
Application for Bio process calculation without reaction
No reactions -- no generation or consumption of any species
The material balance equation can be written for an unsteady state
process as
Input = Output +Accumulation
Steady-state process -- no accumulation
Input = Output

The general material balances equations are made on a system for
the following

. Total mass
2. Total moles
3. Mass of a chemical compound
4. Mass of an atomic species
5. Moles of a chemical compound
6. Moles of a atomic species
Conversion from mass fraction to moles
An aqueous solution of NaCl is prepared by dissolving 25 kg NaCl in 100
kg H
2
O. Find the composition of solution by wt % and mole %
Basis: 25kg NaCl and 100kg H
2
O
Total wt of solution is 100 + 25 = 125 kg
Wt % on NaCl = (kg NaCl / kg solution) x 100
= (25 / 125) x 100
= 20%
Wt % of H
2
O = (kg H
2
O / kg solution) x 100
= (100/125) x 100 = 80%
Molecular Wt. of NaCl = 58.5
Therefore Moles NaCl = 25 / 58.5 = 0.427 moles
Molecular Wt. of H
2
O = 18
Similarly Moles of H
2
O = 100 / 18 = 5.56 moles

Mole % of NaCl =
0.427
x 100 = 7.13
0.427 + 5.56

Mole % H
2
O =
5.56
x 100 = 92.87
0.427 + 5.56

Common flow diagram symbols


ISO 10628: Flow Diagrams For Process Plants - General Rules
ANSI Y32.11: Graphical Symbols For Process Flow Diagrams
Gas compressor
Combiner and splitter

Avoid crossing streams. If streams must cross, you need to indicate
whether they mix or not.


Methods of drawing a flow diagram
Draw boxes (or other symbols) for all equipment and show arrows
indicating all streams and their directions of flow
Standard practice is that major flows are from left to right
All equipment and all streams should be named and numbered
Choose a basis for calculation(mass or mol)
Indicate the rates rate of each stream which are known
If some are unknown known, assume as(x,y)
Write the basis (Mass or mol)clearly on the flowchart
Write the values of all stream variables (with units)
For example: Flow rates kgmol/hr
Compositions
F
mole fraction
Temperature and pressure (deg centigrade, atm)
Use a common basis (mass or moles )

Development of flow diagram system with recycle, bypass and purging
A mixture of hydrogen and nitrogen is fed to a reactor where some of
the hydrogen and nitrogen is converted to ammonia.
The reactor product is sent to a condenser where all of the ammonia
is condensed.
The condensed ammonia is sent to product storage.
The uncondensed hydrogen and nitrogen are recycled by mixing with
a fresh feed
The resulting mixture is fed to the reactor





























Class 2
Definition of Distillation
Distillation is a process of heating a liquid to form its vapors and condensing the vapors to form a liquid
.It is used to separate two or more substances in a liquid.
Separation is due to differences in volatilities (rate of vaporization) of the components
It consumes enormous amounts of energy, both in terms of cooling and heating requirements
It can contribute to more than 50% of plant operating costs
To reduce operating costs of existing units, a thorough understanding of distillation principles
and how distillation systems operates is essential
Commercial uses of Distillation
It is used to
separate crude oil
Transportation, Power generation and Heating
purify water
-remove impurities, such as salt from seawater.

distilled air by separating its components
Like oxygen, nitrogen, and argon
distilled fermented solutions

- To produce distilled beverages with higher alcohol content.
- Laboratory Scale
- Industrial Distillation
- Herbal Distillate
- Food Processing


- Are almost batch distillation.
- The Still or distillation device
- Consist of a reboiler or pot in which the source material is heated.
- A condenser in which the heated vapour is cooled back to liquid state.
- a receiver in which the concentrated or purified liquid, called the distillate is
- collected











Classification of Distillation


Industrial Distillation
Simple distillation
Fractional distillation
Flash vaporization
Steam distillation
Azetropic distillation
Extractive distillation

- typical performed in a large, vertical cylindrical column know as
distillation towers or columns
- With diameters ranging from 65 cm to 6 meters.
- and heights from 6 to 70 meters
- withdrawal of different fractions when

Process feed has diverse composition is possible

This distillation is not used as a true purification method but to transfer all volatiles from the
source materials.
It is similar to Steam distillation and is commonly used
- Various aromatic herbs and flowers can result in two products.
- An essential oil: often used in perfumery and drug synthesis,
aromatherapy.
- Watery herbal distillate: have many application in drug synthesis, food
processing and skin care

Manufacture of pectin by precipitation with alcohol
Production of hop extract
Production of egg lecithin
Decaffeination of coffee beans
Reprocessing of miscella

In batch operation, the feed to the column is introduced batch-wise. In this operation the
column is charged with a 'batch' and then the distillation process is carried out. When the
desired task is achieved, a next batch of feed is introduced after product removal
Suitable for smaller production
To generate data for design of continuous distillation
For complex or small operations which requires the recovery of the more volatile
component
Continuous Columns
The most common form of distillation used by the chemical, petroleum and petrochemical
industries ethanol distillation.
The feed is constantly charged to the column at a point between the top and bottom
sections. The section above the feed point rectifies the more volatile while the column
section below the feed point strips out the more volatile from the less volatile component
Purpose of distillation is to separate two or more liquid mixtures.
Separation takes place in a distillation column or tower
The liquid mixture is called as feed or charge
The components into which a feed is separated is called as cuts or fractions
The schematic diagram of a plant is represented
In this example a stored feed is pumped to pre heater where it is heated under pressure just
below its boiling point
The pressure in the tower is below the pressure in the pre heater so the liquid boils as it enters
the tower
The vapour from the boiling liquid contains primarily lighter components and raises in the tower
The remaining liquid which primarily contains a heavier components moves down the tower and
collected at the bottom of the tower
Some of the liquid is drawn off as a bottom product and some are sent back to a device called
as reboiler
Reboiler is a heat exchanger and designed to vaporize the lighter component that remains as
liquid in the bottom of the tower
Vapours or mixture of vapours from the Re boiler re enters to the tower and raises
the vapour and the heat they contain are called as boils up
Boil up provide the necessary heat required for the distillation process.
The vapour that raises up are condensed, the purpose of condenser is to cool the vapour to
liquid.
Condenser
The liquid from the condenser flows to the reservoir or accumulator
From the reservoir part of the liquid is returned back to the tower and a part is removed as
distillate or overhead product
All distillation do not have all the operations (re boiling and condensing) but most of them have

Sieve trays distillation column
At the heart of the distillation is a distillation tower- series of distillation stills are stacked
This process is called fractional distillation or fractionators
Fractionation is distillation at different levels of the tower
One type of distillation is illustrated is called as sieve tray used to separate vapours and liquids
Sieve trays - are simply metal plates with holes as in a sieve
Trays are spaced throughout the tower
The openings in the tray allows the vapor to raise
Trays are designed to hold liquid
Dams or weir on each side allow the liquid to build up
Liquid overflowing the weirs flows into down comers
Down comers channels the liquid from tray to tray down the tower
When the upward moving vapor and downward moving liquid come in contact with each other
the vapor transfer some of the heat to the liquid
Two things happen
HEAVIER components of the vapor becomes cooler and condenses to liquid and the LIGHTER component
of the liquid boils
The vapor raises to the next tray this process continues
The raising vapor contains higher concentration of lighter components and lower concentration
of heavier components
All distillation columns are not designed in the same way but every tower can be divided into
three basic sections
In the middle sections the tower the feed enters and part of the liquid vaporizes this
vaporization is commonly known as flashing this section is called as flash zone
The section above the flash zone is rectification in this part of the column the concentration of
the lighter components increases
The section below the flash zone is stripping in this part of the column the concentration of
the heavier components increases by vaporizing or stripping lighter components
Recycling or reflux columns
If the column works perfectly then 100 % separation is possible it never happens
The lighter fraction contains heavier components and heavier fraction contains lighter
components in general
Distillation systems use several methods to improve the purity one of the method is called as
refluxing
The vapors coming from the top of the column is condensed in a the condenser stored in the
reservoir partly removed as distillate and partly returned to the tower and called as external
reflux
Since the external reflux is returned from the reservoir where it is cooler than the vapors in the
top of the column
Vapors made of heavier components condense and liquid of heavier components flows down
the column and called as internal reflux
The top of the column is hot enough to keep the lighter component in vapor form so that it can
be taken to the condenser
Refluxing increases the purity of the overhead product since condensed heavier component is
kept away from the vapors leaving
Another method for improving purification is re boiling
The bottoms that are removed is sent to a reboiler ,in the reboiler part of liquid is removed and
sent to storage tank and part is sent back as vapors or mixture of vapors
The hot vapors entering the column vaporizes the lighter components and flows up the column
to the condenser at the top
This reduces the amount of lighter component in the bottoms
Reboiler provides the additional heat necessary for the distillation process


















Main Components of Distillation Columns

Problems





























Reflux ratio is the number of moles being refluxed (sent back)for one mole of
product.
Reflux ratio (external) = L/D = R





One thousand Kg/h of an ethanol/methanol stream is to be separated in a distillation
column. The feed has 40% ethanol and the distillate has 90% methanol. The flow rate of
the bottoms product is 400kg/h.
a. Draw and completely label the process
b. How many equations can you write?
c. How many unknowns can you see?
d. Determine the %methanol in the bottoms product






Determination of the number of unknowns and % methanol in the bottom product


From Equation (1) D =1000 - 400 = 600
Substituting for D in (2)
600=0.9 x 600+ 400 (x
w
)
600=540+400 (x
w
)
x
w
= (600-540)/400
Therefore 60/400=0.15
Methanol composition in % =15%
From Equation (1) D =1000 - 400 = 600
Substituting for D in (2)
600=0.9 x 600+ 400 (x
w
)
600=540+400 (x
w
)
x
w
= (600-540)/400
Therefore 60/400=0.15
Methanol composition in % =15%


Determination of the number of unknowns and % methanol in the bottom product
Number of unknowns = 2 (D & X
w
)
Materials leaving the top product (D)
and composition of methanol leaving at the bottom (x
w
)
Overall material balance
F= D + W ----- (1)
1000=D + 400
Methanol balance Fx
F
= Dx
D
+ Wx
W
----- (2)
1000 x 0.6= D (0.9)+400(x
w
)
600 = 0.9 D+ 400 ( x
w
)
From (1) D=1000 - 400 = 600
From Equation (1) D =1000 - 400 = 600
Substituting for D in (2)
600=0.9 x 600+ 400 (x
w
)
600=540+400 (x
w
)
x
w
= (600-540)/400
Therefore 60/400=0.15
Methanol composition in % =15%

One thousand Kg/h of an ethanol/methanol stream is to be separated in a distillation column. The
feed has 40% ethanol and the distillate has 90% methanol. Eighty percent of the methanol is to
be recovered as distillate. Determine the % methanol in the bottoms product.












Process Flow diagram and labeling




Number of equations
Total material balance
F= D+ B-------------(1)
Material balance for the distillate
F x
F
= D x
D
+ W x
W
------------ (2)
Determination of the number of unknowns and % methanol in the bottom product

Number of unknowns = 2 (D & X
w
)
Materials leaving the top product (D)
And composition of methanol leaving at the bottom (x
w
)
Overall material balance
F= D + W ----- (1)
1000=D + 400
Methanol balance Fx
F
= Dx
D
+ Wx
W
----- (2)
1000 x 0.6= D (0.9)+400(x
w
)
600 = 0.9 D+ 400 ( x
w
)
From (1) D=1000 - 400 = 600
From Equation (1) D =1000 - 400 = 600
Substituting for D in (2)
600=0.9 x 600+ 400 (x
w
)
600=540+400 (x
w
)
x
w
= (600-540)/400
Therefore 60/400=0.15
Methanol composition in % =15%



Number of equations




Total material balance
F= D+ B-------------(1)
Material balance for the distillate
F x
F
= D x
D
+ W x
W
------------(2)
Eighty percent of the methanol is to be recovered as distillate means
The feed contains X
F
F = 600kg/hr on methanol, of this amount 600, 80% must be
the methanol in stream D. Thus 0.8(600) =480kg/hr
MeoH is in D as a 90% stream. 480=.9(D).D=533 kg/hr
W=1000- 533=467 kg/hr
A solution of ethyl alcohol containing 8.6% alcohol is fed at the rate of 1000 kg/hr
to a continuous distillation column. The product is a solution containing 95.4%
alcohol. The waste solution from the alcohol has 0.1% alcohol. Find the rate of
distillate and residue determine the percentage loss of alcohol


Basis: 1 hr of operation
Overall Balance
F=D + W
D + W=1000 -----(1)
Balance for alcohol
FXF = Dx
d
+ Wx
w
0.086(1000)=0.954D+0.001W ------(2)
Solving (1) & (2)
D + W=1000
0.954D + 0.001W = 86 (3) From Equation 2 0.954D + 0.954W = 954----(4)
(Equation 1 x 0.954)
0.954D + 0.001W = 86------(3)

(4)-(3) 0.953W = 868
W=910.80 Kg/hr
D=89.192 Kg/hr



Percentage con 0.0892
= ------------- x 100
86
=1.037%
Solving problems with recycle streams
A liquid mixture containing 45% Benzene and 55% Toluene by mass is fed to a
distillation column. A product stream leaving the top of the column contains 95% mole of
Benzene and bottom product stream contains 8% of benzene feed the volumetric flow
rate of feed stream is 2000 ltr/hr and specific gravity of the feed mixture is 0.872
.Determine mass flow rate of overhead product stream and the mass flow rate and
composition of the bottom product stream

To draw flow diagram and labeling





To convert from
m

Basis 100 kgmoles of overhead products
Moles of Benzene=95 kgmoles
Moles of Toluene =5 kgmoles
Mass of Benzene=No of moles X molecular weight
=95 X molecular weight
Molecular weight of BenzeneC6H6=(12X6+ 1X6= 78)
=95X78= 7410 kg benzene

Mass of Toluene =No of moles X molecular weight
=5 X molecular weight
Molecular weight of Benzene(C7H8)=(12X7+ 1X8= 92)
= 5X78= 460 kg Toluene
Total mass=7410+460
=7870
Mass fraction of Benzene=mass of benzene/Total mass
7410/7870=0.942
Mass fraction of Benzene=mass of benzene/Total mass
1-0.949=0.058
To find the Unknowns and
to do Degree of freedom analysis
DF For non reacting species
Number of Unknowns 4( They are m1,m2,m3B, m3T)
For solving 4 equations are needed
One equation for Benzene is possible
One equation for over material balance
One equation for converting feed to mass flow from volume flow(specified)
One for the benzene split based on the feed and 8% in the bottom stream
To find mass flow rate in the feed
Volume =2000 lit/hr
Sp gravity=0.0872
Sp gravity=Density of mixture/Density of water =kg/lit
=2000lit/hr x 0.872
m1=1744kg/hr
Mass flow rate of feed=1744kg/hr

To Amount of mass flow rate at bottom based on benzene split
Mass of Benzene in feed = 1744x0.45 =
784.8kg/hr
m3B is 8% of benzene in feed=.08 X 784.8kg/hr =
62.78 Kg/hr
Material balance for Benzene
m1XF = m2Y
B
+ m3B

1744 kg/hr x.45= 0.942Y
B
+62.78kg/hr
m2= 766.5 kg/hr
Overall balance
m 1= m2+m3
1744kg/hr=766.5+m3
m3=977.5kg/hr
Mass fraction of Benzene in bottom stream
= mass of benzene in bottom stream /total mass of
bottom stream
=m3b/m3
Benzene/kg of kg 0.06
973.5
62.78
= =
Mass fraction of Toluene in bottom stream
x
T
=1-x
B
=0.94 Kg of Toluene/Kg


Solving problems of multi component systems




A distillation column separates 10000 kg/hr of a 50% benzene and 50% toluene
mixture. The product D recovered from the condenser at the top contains 95% benzene
and the bottom W contains 96% toluene. The vapor stream entering the condenser from
the top of the column is 8000 kg/hr. A portion of the product from the condenser is
returned to the column as reflux and the rest is withdrawn for use elsewhere. Assume
that the compositions of the streams V, D, L are identical. Draw the flow sheet and find
the ratio of amount refluxed to the product withdrawn.










Basis: 10000 kg of feed
Overall balance: F= D+W ,
10000 = D+W.. (1)
Benzene balance: Fx
F
= Dx
D
+ Wx
W
,
10000x0.5

= D (0.95) + W (0.04),
5000 = 0.95D+0.04W. (2)
From Equation (1) W=10000-D,
Substituting for W in Equation (2) 5000=0.95D + 0.04(1000-D)
5000=0.95D + 400-0.04D, 5000
= 0.91D + 400, 0.91D = 4600,
D=4600/0.91=5054.95 kg / hr
W=10000-5054.95=4945.05 kg / hr
V=8000 kg / hr , D=5054.95 kg / hr
V= L+D
or L=V-D
=8000-5054.95
=2945.05
Reflux ratio R=L/D
= 2945.05/5054.95=0.5826
Solving Problems of multi component systems
P Xylene, styrene, toluene, and benzene are to be separated with the array of
distillation columns as shown. Calculate the molar flow rates of D
1
, D
2
, B
1
, and B
2
and
also D and B













Review
100 kg mole / hr of 40% solution of ethylene dichloride in toluene are fed to
the middle of a distillation column. The distillate stream contains 95 mole %
ethylene dichloride and bottom product contains 90 mole % toluene. What is
the rate of flow of each stream?












Process Flow diagram and labeling

Overall material balance
F = D + W
100 = D + W -------(1)

EDC balance 100 (0.4) = D (0.95) + W (0.9).
40 = 0.95 D + 0.1 W------(2)
Toluene balance 100 (0.6) = D (0.05) + W (0.9)
60 = 0.05 D + 0.9 W----(3)

D = 35.29 kg mol W = 64.71 kg mol
I have explained the following
Principles of Distillation process
Classification of industrial processes
How to write material balance equations for simple binary systems and solve
them
Solving problems for processes involving recycle streams
In the next session I will discuss as how to write material balance equations and
solving them for Drying operations with and without recycle based on the
degree of freedom analysis
Thank you!!!!


















Class 3

In downstream processing, product purification steps requires heating of material
Drying, Evaporation, Distillation, Crystallization, Sterilization and Extraction are
some of the process
In these processes heat transfer where materials with and without phase change
occurs
Definition

Evaporation is a process of phase change from a liquid to gas that takes place on the
surface of liquid
Liquid can change to gas (vapour) at temperatures below the boiling point
It differs from the phenomena of boiling in which the entire mass of liquid is converted to
gas








Differences between evaporation and boiling








Cooling effect of evaporation
On a humid day, the air is full of water vapour and we feel uncomfortable and more hot
Saturated air slows down the evaporation of sweat from the body
Sweat tends to stay on the skin.
No cooling effect occurs
So we fill hot
Cooling effect of evaporation,
If you sit under a fan large volume of air is circulate around your body
Boiling
Occurs at a definite temperature the boiling point
Occurs within liquid
Bubbles appear
Evaporation
Occurs at any temperature
Occurs at surface
No bubbles formed
Sweat comes out of the pores, evaporates thus taking energy away from the skin. So
we feel cool!
If water spills in short time it disappears at room temperature
Evaporation and kinetic theory
Evaporation is the escape of fast-moving particles from the surface of a liquid
Different particles have different velocity
some have higher K.E
Kinetic theory and cooling effect



Fast-moving particles in liquid surface escapes easily and become vapours
While slow-moving particles in vapour stays back in the liquid
The rate of evaporation is a balance between the rate of escape and the rate of
return
Effect of Temperature of water
The rate of evaporation increases with the temperature of the liquid
Molecules have more KE at higher temperatures
Molecules move faster on average and more molecules escapes
larger the surface area, more molecules can escape at the same time
Rate of evaporation is more
Effect of Humidity of air
If the air is humid, it is full of water vapour or saturated no evaporation
Water particles in vapour have greater chance to return to the liquid.
Humidity of the air, lowers the rate of evaporation



Basic calculation
Energy required to heat a substance

If there is no phase change
Apply Q= mcT,
If there is phase change
Apply Q=m
m = mass of the substance kg
c= specific heat J/ kg
o
C
T= Temperature difference
o
C
latent heat of vaporisation J/ kg
A person weighing 60 kg and while doing exercise is covered with sweat. If 1 litre (1 kg) of
sweat is evaporated in 1 hour how much energy is required to evaporate this amount of water?
To find Energy required to evaporate 1 kg of water
Q=m (there is a phase change)
=2260 10
3
J/kg
m=1kg
Q= 1 2.26 10
6
J
If this amount of energy were not removed from the body by sweating by how much would the
body temperature of the person increase
Assume The average specific heat capacity of the human body is 3500 J /kg
o
C
Apply Q= mcT,
T = Q/mc = 2.26 10
6
/ (60 3500)
T = 10.8 C
If the energy were not removed from the body
The body temperature would increase by 10.8 C
Applications in Bio processes

Manufacture of bulk drugs , evaporation process is used in various pharmacy practices
Concentration of milk to produce condensed milk,Concentration of juices
Ether recovery from fat extraction
Manufacture of biological products such as insulin, biochemical products (penicillin) and herbal
extracts
Preparation of blood plasma & serum, Enzymes & antibiotics
Evaporation is a process of vaporizing large quantities of volatile liquid to get a
concentrated product
Evaporation is a surface phenomenon, and mass transfer takes place from the surface
Used for either solutions or suspensions
Liquid must be volatile, while the solute must be non-volatile
Material should be thermo-stable
Liquid is usually water with low solid content
Properties of material to be evaporated should fast-moving and escape
Determine the minimum quantity of air needed to evaporate 6 kg of ethyl alcohol at 20
deg C and 100 kPa.
Vapor pressure of ethanol at 20 deg C and 100 kPa is 5.93 kPa
Ethyl alcohol and air can exist together.
The maximum quantity of ethanol in air corresponds to saturation.
Air corresponding to saturation
is the minimum air needed







Molecular weight of ethanol(C
2
H
5
OH)








air dry of moles
ethanol of moles
06303 . 0 =
mol 33 . 2069 43 . 130
06303 . 0
1
= =
kg g 01 . 60 6 . 60010 29 33 . 2069 = = =
93 . 5 100
93 . 5

=










Strawberries contain about 15 wt % of solids and 85 wt % H
2
O . To make strawberry
jam, crushed strawberries and sugar are mixed in a
45: 55 mass ratios and the mixture is heated to evaporate until the residue contains 1 /
3 water by mass. Calculate how many kg of strawberries are needed to make one kg of
jam.

mol 43 . 130
46
6000
= =




Acetone which is being used as a solvent in an extraction process, is being recovered
by evaporation into a stream ofN
2
. The N
2
enters at 30
o
C containing acetone such that
its dew point is 10
o
C. It leaves at 25
o
C with a dew point of 20
o
C.The barometric
pressure is constant at 760 mm Hg. Calculate
(i) The weight of acetone evaporated per 1000 liters entering
(ii) The volume of the gases leaving the evaporator per 1000 liters entering.
The vapor pressure of acetone:
Temperature,
0
C Vapor pressure,
mm Hg
10 116
20 185
Basis: 1000 litres of gas entering at 30
0
C, 760mm Hg
This contains nitrogen and acetone
Total moles entering





RT
PV
N = 1
) 30 273 ( 082 . 0
) 1000 ( 1
+
=
moles 25 . 40 =

moles of nitrogen=40.25




moles of acetone leaving=0.2434(40.25)
=9.79685
moles of acetone evaporated=9.79685-6.14215
=3.6574moles
Wt of acetone evaporated=3.6574(58)=211.97g
Total moles leaving=40.25+9.79685=50.046
Final volume v
f
=


0.2434
760
185
moles Total
acetone of moles
= =
f
f f
P
RT N
1222.9l
1
25) 82)(273 50.046(0.0
=
+
=


Material and energy balance calculation
The total amount of steam required (Evaporator capacity) can be obtained by drawing a
flow diagram of an evaporator
Writing the fundamental material balance equations
Writing the energy balance equations based on the materials
The enthalpy of each stream is needed
















Evaporator
Vapour out


Material balancing

V Vapour leaving kg/hr
X
v
=0
Feed F kg/hr
mass fraction of feed
X
F
kg of solute /kg solution
Total material entering = Total material leaving


Feed =Product collected + Vapor liberated
F(kg/hr)=L (kg/hr) +V (kg/hr) ..(1)
Writing for material balancing in terms of mass x weight fraction for the solute
FX
F
=LX
L
+ VX
v
............(2)
X
v
= 0
FX
F
= LX
L
An aqueous solution of sodium hydroxide is to be concentrated from 10% to 50% by
weight . The amount of sodium Hydroxide present is 100 kgs .
Material Feed F kg/hr=?
mass fraction of feed
X
F
= 0.1 kg of solute /kg solution
Concentrated product L kg/hr=?
X
L
0.5 kg of solute /kg solution


There are two unknowns in the flow diagram
1 ) Feed rate and 2)Product rate
Feed rate rate can be directly found out since it is specified that the total sodium
hydroxide present is 100 kg
0.1 F=100
F=1000 kg
Component balance for sodium hydroxide
FX
F
=LX
L

1000 x 0.1=0.5 x L
L =200 kgs
Water evaporated is V=F-L=1000-200=800 kgs

Energy balance
Steam is supplied for evaporation.
Let S kg be the steam supplied/hr with an enthalpy of hS J/kg.
Let C kg be the condensate removed having an enthalpy of hC J/kg.
The heat balance can be obtained from total heat entering & total heat leaving
Heat in feed +heat in steam=heat in thick liquor(product) + heat in vapor+ heat in
condensate
Energy balance equation written in terms of enthalpy as FhF+ShS=LhL+VhV+ChC







A temperature difference of 20-30
0
C is sufficient for evaporation of solution.
But in practice, the feed may have the temperature less than boiling point of the
liquid.
The steam may be superheated & the condensate may get cooled.
All these eavaporator Classification
Small Scale Laboratory
Large Scale (Industrial)
Natural Circulation
Evaporation Pan
Short tube evaporation
Forced circulation
Film Evaporation
Long tube
Horizontal Evaporator
Wiped film Evaporator
Rotary film
Improved /Economical
1) Multiple
2) Vapor compressions





Uses:- Concentration of aqueous & thermo liable liquors.
Advantages:- For both large & small scale Simple in construction & easy to operate,
clean & maintain.
Cost of installation & maintenance is low. Construction with wide variety of materials like
copper, aluminum, stainless steel. Stirring & removal of product is easy.
Short tube evaporator



Natural circulation type
Liquid passes through the vertical tubes & the steam is supplied from outside the
tubes.
Heat transfer takes place through the tubes & the liquid inside the tubes gets
heated.
The solvent evaporates & escapes from the top of the evaporator.
The concentrated liquid is collected from the bottom.
Inside the body, Steam chest(calandria )is fitted at the bottom. Calandria consists
of a number of vertical tubes, whose diameter ranges from 0.05 to 0.075 meters
& length of 1-2 meters.
These types of evaporators are used for small installation
Concentrating sugar ,salt and alkali solutions

Body diameter ranges from 1.8 to 2.4 meters diameter & from 2.4 to 3.6 meters height.
Lower part of body consists of a steam compartment with an inlet for steam at one end
& a vent for non condensed gas on the other end
Best suited for non viscous solutions that do not deposit scales or crystals on
evaporation.
E.g. cascara extract.
Advantages :- Cost per square meter of heating surface is usually less.

Forced circulation evaporator
Steam is introduced into the calendria. Pump sends the liquid to the tubes with a positive
velocity.
As the liquid moves up through the tubes, it gets heated & begins to boil.
As a result the vapor & liquid mixture rushes out of the tubes at a high velocity.
This mixture strike the deflector which throws the liquid downward.
This result in an effective separation of liquid & vapor.
The vapor enters the cyclone separator & leaves the equipment.
The concentrated liquid returns to the pump for further evaporation.
Finally the concentrated product is collected.
Uses :- It is operated under reduced pressure, so suitable for thermo labile
substance.
For concentration of insulin & liver extract. Suitable for crystallizing operations
where crystals are to be suspended at all times.
Advantages :- High heat transfer coefficient due to rapid liquid movement.
Salting, scaling & fouling are not possible due to forced circulation.
The heating unit consists of steam jacketed tubes.
The feed inlet is from the top of the steam compartment.
The other provisions are steam inlet, vent & condensate outlet remain same as
other evaporators
Feed enters from the top of the tubes.
The temperature of the boiling liquid is same as that of the vapor head.
The feed flows down the walls of the tubes. The liquid gets heated rapidly.
The liquid boils & become vapor, which forms small bubbles.
These tend to fuse to form large bubbles, which travel down the tubes.
Concentration takes place during this downward journey
Useful the concentration of yeast extract, manufacture of gelatin, extract of tea
& coffee. Used for heat sensitive materials such as fruit juices


Multiple effect evaporator
Advantages :- Suitable for large scale & for continuous operation.
Highly economical when compared to single effect.
Upto 5 evaporators can be attached. Construction in fig is a triple effect evaporator (3
single) effect evaporators
The other aspects of construction remain same as single effect.
The vapor from 1
st
evaporator serves as a heating medium for 2
nd
evaporator. Similarly
for 3
rd
evaporator.
Last evaporator is connected to a vacuum pump.
In this process steam from the 1st effect is utilized by operating the successive
evaporators
They are operated at lesser pressures
The general equation for heat transfer can be expressed as : Q=U A t
Where Q=rate of heat transfer, Watts U=overall heat transfer coefficient, W/m
2
K
A=heating surface area, m
2

t=temperature difference, K
For improving heat transfer coefficient U,Heating surface (A) must be large.
For this purpose more number of tubes are mounted in parallel to form a unit known as
calandria






The overall heat transfer coefficient, U, can be increased regarded as follows.
Improving heat transfer coefficient
Pumping liquid at high velocities (forced circulation) through the tubes has
beneficial effect.
Overall coefficient may be seriously lowered because of deposition of solid
material from the evaporating liquid.















Class 4
Drying




Agenda


Review of previous session
Introduction
Application of drying in Food industries
Classification of Drying processes
Special application
Solving fundamental problems
Solving problems with recycle streams
Summary and Future Session


Definition
Drying is defined as the removal of small amounts of water or other liquid
from a material by the application of heat
Drying is basically mass transfer (diffusion) process consisting of the
removal of water or another solvent by evaporation from a solid, semi-solid
or liquid
In bio process drying is often used in down stream processing before
packaging products

In most of the drying operation, a gas stream usually atmospheric
air, transfers the heat by convection and carries away the vapor

Other possibilities are vacuum drying, where heat is supplied by
conduction or radiation or microwaves while the vapor thus produced
is removed by the vacuum system





To consider for marketing a final product it must be solid, in the form
of a continuous sheet (e.g. paper), long pieces (e.g. wood),
particles (e.g. cereal grains or corn flakes) or powder (e.g. sand, salt,
washing powder, milk powder)
A source of heat, and an agent to remove the vapor produced by the
process are needed
In bio products like food, grains, and pharmaceuticals like vaccines,
the solvent to be removed is usually water
Preservation of Food and drug products
Better characteristics for packing
Preparation of Bulk drugs
Product purification and Improved Handling
How Drying Preserves Food

Removes moisture from food so bacteria, yeasts & molds cant grow
and spoil food
Slows down action of enzymes but doesnt inactivate them
Low humidity of air aids drying
Increasing air current speeds up drying, removes air around food
Smaller pieces dry faster

Principles of Drying

Drying of wet solids is achieved by exposing the solids to a wave of
hot air which removes the moisture by convection from an initial
moisture content. In the process, both the heat transfer and mass
transfer take place. Heat is transferred from hot air to the solids, and
in turn, the moisture diffuses out of the solids and gets transferred
into the stream of relatively dry air. The following are certain terms
which are frequently referred to drying.
Bound , unbound free moisture and equilibrium moisture content with
respect to solid,
Humidity and Relative humidity (RH) with respect to air
Temperatures for Drying in food processing

Optimum temperature for drying food is 60c
If higher temps are used, food cooks instead of drying
Care should be taken , so that food is not dried only in the outer side
and moisture is trapped inside (case hardening )


Terms used in drying phenomena

Moisture content wet basis(x
w
)
The moisture content of a solid is the ratio of moisture present initially
in the solid to the weight of the wet solid




This moisture content is defined on wet basis






Moisture content on dry weight basis (X)
We generally prefer to define the moisture content on dry weight basis
because of its ease in expression. The denominator of it does not change
with the drying process












Total moisture content: the total amount of liquid associated with a wet
solid
In the context of drying, not all of it can be easily removed by the
simple evaporative processes employed by most pharmaceutical
driers
wetsolid of kg
moisture of kg
X
W
=
solids dry the of kg moisture of kg
moisture of kg
+
=
W
W
X 1
X
solid dry of kg
moisture of kg
X

= =
1 X
X
X
W
+
=
The easily removable water is known as the free moisture content
(unbound water)

Bound moisture : part of the moisture present in a wet solid may be
adsorbed on surfaces of the solid or be adsorbed within its structure
prevent it from developing its full vapor pressure
and from being easily removed by evaporation
Such moisture is described as 'bound' and is more
Difficult to remove than unbound water







Equilibrium moisture content
Evaporative drying processes will not remove all the possible
moisture present in a wet product since the solid equilibrates with the
moisture present in the air
The amount of water present in the solid under this condition exerts a
vapour pressure equal to the vapour pressure of the atmosphere
surrounding it
This value depends on temperature, humidity and the nature of the
solid.






















Air entering has some relative humidity If we have to dry the material, we
cannot do it below this relative humidity as drying is an equilibrium process
The portion of water in the wet solid that cannot be removed by inlet air
because of humidity of the latter is called as equilibrium moisture



Principles of Drying








RH of air
CD: un bound moisture: CF: Bound moisture
EB: Equilibrium moisture content:
BG: Free moisture




PSYCHROMETRIC RELATIONSHIPS



HUMIDITY




H=humidity kgs of water per kg of dry air
P is total pressure
P
A
= Partial pressure of air
P
T
= Total pressure
M
A
= Molecular weight of air
M
B
= Molecular weight of water




SATURATION HUMIDITY
P
A
= Partial pressure of air
P
w
= vapour pressure of water
M
A
= Molecular weight of air
M
B
= Molecular weight of water
PERCENT RELATIVE HUMIDTY







PERCENT HUMIDITY




Tray dryer
) (
A T B
A A
p P M
p M
H

=
) (
W T B
W A
s
p P M
p M
H

=
S
P
H
H
H 100 =
Working Principle
In tray dryers, hot air is continuously circulated.
To remove moisture from the solids placed in trays air is forced into the
dryer by a fan
The moist air is removed partially.
This is also called as shelf, cabinet or compartment dryer.
Construction
It consist of rectangular chamber whose walls are insulated.
Trays are placed inside the Drying chamber in racks.




Rack contain shallow trays: 750 mm square and 50-150 mm deep, Air
velocity: 2-5 m/s by fan, Baffles to distribute air
Advantages:
Handling of materials can be done without losses
It can be operated batch wise
Equipment is readily adjusted for use in drying of variety of materials
Valuable products can be handled efficiently
Disadvantage :It requires more labor to load & unload, Time consuming
4-48hrs
Application:Sticky materials Plastic substances, Precipitates , Chemicals
,Tablet ,granules & powders



FLASH OR SPRAY DRYERS

CONTACT FLOW WITH COCURRENT FLOW OF HOT AIR
SOLIDS MAY BE ENTRAINED
SOLIDS MAY FALL THROUGH AIR
MAY INCORPORATE CYCLONE
MAY INCORPORATE SPRAYER TO PRODUCE SLURRY
DROPLETS
MAY BE INCLUDED ON TALL TOWER (PRILLING)
OPERATION
Slurry or liquid solution dispersed
into a stream of hot gas in the form of mist of fine droplets
Moisture rapidly vaporizes from droplets leaving residual particles of dry
solid
Droplets formed by pressure nozzles
To prevent droplets or wet particles of solid from striking solid surface,
diameter is made large (2.5-9 m)










Specification:
Spray disk = 300 mm, rotates at 5000-10000 r/min
Cylindrical chamber with conical bottom to collect the solids, Gas leaving is
passed to cyclone for removal of entrained solid
Advantages:
Continuous process drying completes within 3 to 300 S
Labor cost is low.
Product of uniform & controllable size can be obtained.
Application: Citric acid, Gelatin ,Barium sulphate Detergents , Pepsin
,Vaccines, Penicillin , Acacia Borax, Fruit juices , Blood, Pancreatin
Hormones , Chloramphenicol , Extracts ,Milk Lactose Plasma , Vitamins
,Serum ,Starch

DRUM DRYER

In drum dryer, a heated hallow metal drum rotates on its longitudinal axis,
which is partially dipped in the solution to be dried.
The solution is carried as a film on the surface of the dryer and dried to
form a layer.
A suitable knife scraps the dried material, while the drum is rotating.


Specifications: It consist of a horizontally mounted hollow steel drum of 0.6
3.0 meters diameter 0.6 4 meters in length
Working: Drum is rotated at a rate of 1- 10 revolutions per minute.
The liquid material present in the feed pan adheres as a thin layer to the
external surface of drum during its rotation
Material is completely dried during its journey in slightly less than one
rotation
The dried material is scrapped by knife, which then falls into a
storage bin
The time of contact of the material with the hot metal is 6-15 seconds
Uses ( Heat sensitive ) Milk product Starch product, Antibiotics Yeast
& pigments ,Malt & glandular extracts, Insecticides


FLUIDIZED BED DRYER


In fluidized bed dryer, hot air (Gas) is passed at high pressure
through a Perforated bottom of the container containing granules to
be dried.
The granules are lifted from the bottom and suspended in the stream
of air. The condition is called fluidized state.
The hot gas is surrounding every granule to completely dry them.
Thus, materials or granules are uniformly dried.


The wet granules to be dried are placed in the detachable bowl & it is
pushed into dryer.
Fresh Hot air is allowed to pass through the bottom of the bowl.
The air velocity is gradually increased. When the velocity of the air is
greater than settling velocity of granules.
The granules remain partially suspended in the gas stream.
The granules rise in the container because of high velocity gas & later fall
back in a random boiling motion.
This condition said to be Fluidized State. The gas surrounds every granule
to completely dry them. The air leaves the dryer by passing through bag
filters


FREEZE DRYER

Freeze drying is also known as lyophilization.
Principle:
In freeze drying, water is removed from the frozen state by
sublimation, i.e., direct change of water from solid into vapour without
conversion to a liquid phase
Solid-liquid- vapour equilibrium phase diagram of water is useful to decide
the experimental conditions. The drying is achieved by subjecting material
to temperature & pressure below the triple point. Under this conditions, any
heat transferred is used as latent heat & ice sublimes directly into vapour
state. The water vapour is removed from the system
by condensation in a cold tra p
maintained at a temperature lower than rozen material.

DIELECTRIC OR MICROWAVE DRYING

It is the method of drying in which electromagnetic radiation (radio
frequency from 3-150 MHz or microwave frequency at 915 or 2450
MHz) is applied to material dried.
If polar solvent molecules are present, the electromagnetic field
induce orientation of the dipoles in molecules
As the field oscillates, the polar solvent molecules oscillate with the
field, resulting in increased kinetic energy from dipolar molecules and
their collisions with others
This manifested in thermal or heat energy
The rate of heating is proportional to the dielectric constant of
materials placed in the field
Water has dielectric constant 70 and the granule around 10, then
water will be heated more rapidly than other components in granule
Selection


The different drying equipments are available, but the suitable dryer
is selected based on the Nature of material, cost, time and nature of
the product required.
When considering how to dry a material, the following points should
be considered:
Heat sensitivity of the material being dried
Nature of the liquid to be removed
The scale of the operation
The general principles for efficient drying
Large surface area for heat transfer
Efficient heat transfer to supply sufficient latent heat of
vaporization or heat of sublimation
Efficient mass transfer of evaporated water through any
surrounding boundary layers
Efficient vapor removal, i.e. low relative
humidity air


Wet solid containing 10% moisture is sent into the drier where it is dried to
a moisture content of 3%. If the flow rate of entering wet solid is 50 kg/hr,
determine the rate of evaporation in the drier and the product rate




Bone dry solid: solid which does not contain any water. Such components
whose constitution does not change is called by component or tie
substances.
Basis : 1 hr
Bore dry solid balance:
0.9 (WS) = 0.97 (P)
0.9 (50) = 0.97 (P)
There fore P = 46.4 kg/hr
There fore W=WS-P
= 50-46.4
= 3.6082 kg/hr
Therefore rate of evaporation in the drier is 3.6082 kg/hr
A batch of leather after drying weighs 500 kg and contains 6 % moisture.
During the process of drying, leather lost 60 % of its original weight.
Calculate
a) moisture content in the leather originally present expressed as kg of
water / kg of bone dry leather
b) kg of water removed per kg of bone dry leather
c) Water removed as percentage of water originally present

BASIS 500 KG Dried leather











Wet solids contain 20 % moisture and are to be dried to water content of 1
% by circulating hot air over them. Fresh air contains 0.018 kg of water
vapor per kg of dry air and exhaust air contains 0.095 kg water vapor per
kg dry air. Calculate the volumetric flow rate of fresh air used for drying
1000 kg / h of wet solids if the air is supplied at 27
o
C and 101.325 kPa.
Basis: 1000 kg / h of wet solids fedLet W be the amount of moisture
removed from F to the air stream. F = D + W
D + W = 1000



Milk powder is produced in a spray dryer, which evaporates all liquid water.
The operation is shown in the figure. Assuming inlet air contains no water,
calculate the production rate of milk powder and molar flow rate of inlet air.





Air at temperature of 60 C, pressure of 745 mm Hg and a percentage
humidity of 10.0, is supplied to a drier at a rate of 1500 m/hr. water is
evaporated in the drier at a rate of 25kg/hr. the air leaves at 35 C and 742
mm Hg.
Calculate
a) Percentage humidity of air leaving the drier
b) Volume of wet air leaving the drier per hour



Percentage humidity=





Molal humidity = (0.1) (0.25)
= 0.025 k mol / k mol dry air







air dry mol k
water mol k
P P
P
H
W r
W
S
25 . 0
38 . 149 745
38 . 49
=

=
S
H
H
= 1 . 0
hr kmol / 78 . 53
273
333
745
760
414 . 22
1500
=
(

Mol fraction




Entry stream






Leaving stream



1-0.058=-.942


k mol of dry air entering = 53.78(0.8) =43 k mol


Water evaporated =








Molal humidity of outgoing air= 0.025 + 0.035=0.0573








yair O yH
P
P
r
W
/ 2 =
2 . 0
745
38 . 149
=
058 . 0
742
43
=
mol k 389 . 1
18
25
=
032 . 0
00 . 43
389 . 1
= =
air dry of mol k
evaporated water of mol k
% 17 . 93 100
43 742
43
0573 . 0
100 % =
(
(
(
(

= =
S
H
H
RH


Volume of air leaving=43 (1+0.0573) (22.414)










Basis : 1 g dry solid.

Let x g dry air be recycled

Water removed by drying = (1.562-0.099)=1.463 g

water removed/g of dry air = 0.0525-0.0152=0.0373
Dry air needed = 1.463/0.0373=39.22 g
Dry air passing through drier (e) = 52.5 g
(between B and C)
There fore Dry air recycled (x)
=52.5-39.22=13.28 g
hr m / 56 . 1177
742
760
273
308
3
=
|

\
|
|

\
|
There fore fraction recycled
= x/e= 13.28/52.5=0.253



CONCLUSION

I. The water activity, which is a measure of the moisture content, when
reduced below certain levels, will make the biological materials free
from the survival and growth of microorganisms, and hence will help
in increasing the shelf-life of the material
II. Drying will reduce both the weight and volume of the product, which
will facilitate easy packaging and transportation
III. The shelf-life of dry products will increase considerably


iv. Freeze drying is process in which the moisture in the product is frozen
by reducing temperature and pressure below the triple-point of water, and
subsequently the moisture is removed by raising the temperature and
keeping the vacuum constant, so that the moisture in the form of ice
sublimes to vapour without going through the liquid phase.

V. Microwave heating is altogether a different heat transfer method, in
which heat is generated in the wet solids by molecular friction by
continuously changing the polarity of the water molecules by applying
electromagnetic waves.








Class 5


Review of previous session
Introduction and Definition
Methods of Crystallization
Mechanism of crystal growth
Writing material balance equations and solving them
Solving fundamental problems of binary systems
Crystallization is the process of formation of solid crystals precipitating from a solution
In this process the atoms, molecules or ions arrange themselves in a repeating pattern

Crystallization is also a solidliquid separation technique, in which mass transfer of a solute from
the liquid solution to a pure solid crystalline phase occurs
The crystallization process consists of two major events, nucleation and crystal growth
Nucleation is the step where the solute molecules dispersed in the solvent start to gather into
clusters, that become stable under the operating conditions (temperature, supersaturation,
etc.)

These stable clusters constitute the nuclei.
The clusters need to reach a critical size in order to become stable nuclei
It is at the stage of nucleation that the atoms arrange in a defined and periodic manner that
defines the crystal structure
Used to recover pure solids from solution
Highly desirable end product because of:
Exceptional purity
Ease of handling
Long shelf life
One of the final treatment steps in the purification and concentration of drugs
Methods of Crystallization
Super saturation: liquid (solvent) contains more dissolved solids (solute) than can ordinarily be
accommodated at that temperature
Can be achieved by several methods:
Cooling
Evaporation
Solvent addition
There are numerous methods to obtain crystals
For small molecules, crystals are grown by reducing the solubility of the sample
The solubility of most compounds decreases as the temperature is lowered thus the cooling of a
saturated solution will often produce crystals.
Since rapid cooling may cause the precipitation of amorphous solid or microscopic crystals, flask
is insulated to slow the rate of cooling
The solubility of most solid substances increases with temperature, so decreasing the
temperature will cause the solubility of both the impurities and the substance to be purified to
decrease.
However, since it is likely that much more of the pure substance is present than impurities, the
pure substance will crystallize out long before the impurities will.
Therefore, as long as the temperature is not lowered too quickly, the pure substance will
crystallize out from mixtureHigh purity downstream
Disadvantages:
Temperature change does not always have a positive effect on super saturation in proteins
Protein stability may be at risk
Solubility can be relatively insensitive to temperature at high salt concentrations
Cooling will only help reach super saturation in systems where solubility and temperature are
directly The slow concentration of dissolved samples is one of the most general ways of
obtaining crystals when the concentration exceeds the solubility, nucleation and
crystallization/precipitation may follow. This can be done a variety of different ways such as
evaporation of the solvent (in open or closed systems). For insoluble samples, Soxhlet
extraction is often a particularly effective method of concentration.
Solute is dissolved in solution by heating to a certain temperature (75C)
Slowly cooled until crystals precipitate
Shell and tube heat exchanger is used to heat and cool solution
Advantages:
high purity levels downstream
Disadvantages:
Vaporization chamber requires high pressures
Protein viability very sensitive to high temperatures
Solvents are generally good protein precipitants
Their low dielectric constants lower the solvating power of their aqueous solutions
Requires acidic solvent
For crystallization, an insulin protein falls out of solution at isoelectric point
pH 5.4-5.7
Advantages:
Proteins viability not at risk due to temperature change
Disadvantages:
Possible protein contamination due to insufficient downstream solvent recovery
Benefits of Continuous
Can maintain solution in supersaturated state
Large fluidized bed for crystallization
Minimizes operation costs
Minimize down time (startup and shutdown)
Benefits of Batch
Good when have low concentration of product, high viscosity or many impurities
Can produce high quality crystal
Crystal Size and Growth Rate
Crystal size distribution is important for the production process; affects:
downstream processing
solids transport
caking and storage properties of the material
Correct crystal size vital for economic production
Crystals produced in commercial crystallization processes are usually small
30 to 100 um in diameter
Crystals produced in commercial crystallization processes are usually small
30 to 100 um in diameter
Crystal size distribution is important for the production process; affects:
downstream processing
solids transport
caking and storage properties of the material
Correct crystal size vital for economic production
Crystals produced in commercial crystallization processes are usually small
30 to 100 um in diameter

In process industries products are produced with impurities in the reactors.
To get pure products different unit operations such as distillation, evaporation, crystallization
etc. are used.
Crystallization is carried out when a solid product is to be recovered from its solution with other
component. This is done by super saturating the solution by one or more of the three methods
namely cooling, evaporation and adiabatic cooling.
If the solubility of the solute increases to larger extent with increase in temperature (strong
function of temperature) a saturated solution becomes super saturated by simply cooling and
temperature reduction.
If the solubility is relatively independent of temperature as in the case of NaCl solution, super
saturation is obtained by evaporating a portion of the solvent.
To increase the capacity of crystallization, adiabatic cooling is normally carried out (evaporation
and cooling simultaneously carried out with out the addition of heat).
Some times a solid has to be removed from solid mixture. The purification of the mixture
(separation of one component) is carried out by treating the solid mixture with a suitable
solvent so as to dissolve only the desired component and then crystallizing it. The solubility of
solute plays an important role in the crystallization operation.
It is the maximum amount of solute that can be dissolved in a solvent at a particular
temperature. Solubility in general increases with temperature.
The solubility of a solute is expressed in different ways
1.gms solute/ 100 gm solvent
2. gm moles solute/ 1000 gms solvent
3.% solute in solution
Solubility: It is the maximum amount of solute that can be dissolved in a solvent at a particular
temperature :
g solute/ 100 g solvent ; and g mol solute / 100 g mol solvent
A solution of CaCl
2
in water contains 62 kg of CaCl
2
per 100 kg water. Calculate the weight of this
solution necessary to dissolve 250 kg of CaCl
2
.6H
2
O at 25
0
C.
Solubility at 25
0
C = 7.38 kg mol CaCl
2
per 1000 kg H
2
O
Molecular weight of

CaCl2

= 111 and CaCl
2
.6H
2
O = 219
A solution of CaCl
2
in water contains 62 kg of CaCl
2
per 100 kg water. Calculate the weight of this
solution necessary to dissolve 250 kg of CaCl
2
.6H
2
O at 25
0
C.
Solubility at 25
0
C = 7.38 kg mol CaCl
2
per 1000 kg H
2
O
Molecular weight of

CaCl2

= 111 and CaCl
2
.6H
2
O = 219
A solution of CaCl
2
in water contains 62 kg of CaCl
2
per 100 kg water. Calculate the weight of this
solution necessary to dissolve 250 kg of CaCl
2
.6H
2
O at 25
0
C.
Solubility at 25
0
C = 7.38 kg mol CaCl
2
per 1000 kg H
2
O
Molecular weight of

CaCl2

= 111 and CaCl
2
.6H
2
O = 219





A solution of NaCl in water is saturated at 15
0
C . Calculate the amount of NaCl that can be dissolved by
100 kg of this solution if heated to a temperature of 65
0
C.
Data : Solubility of NaCl at 15
0
C = 385 kg / 1000 kg of water and at 65
0
C = 372.65 kg / 1000 kg of
water.


F + C = L ,
FX
F
+ CX
C
= LX
L
; (100 X.278 C=(100+C)X0.2715
C = - 1.12 kg at 65
0
C
- ve value shows that solution crystallizes out

Material Balance for Crystallization
processes
Crystallization is the formation of solid particles
from liquid on super saturation. It is a unit
operation, where separation of a desired
component and the phase change simultaneously
takes place. The driving force for crystallization is
the super saturation, which discharges as crystals
to the solid phase or by evaporation. Super
saturation is mainly accomplished by cooling the
liquid in bulk crystallizers.
1
During the crystallization processes some
solutes takes water molecule into the crystal
structure and gets converted in to crystals. Such
crystals are known as hydrated crystals. The
most important targets in crystallization are to
get pure crystals with a desired product crystal
size distribution in the chemical, medical and in
food industries
32
Crystallization
Crystallization is the removal of solute
from solution by super saturating the
solution.
Vapor V, Xv =0
Mother liquor
L, XL
Crystal C, Xc
Feed solution
F kg, XF
33

F,V,C,L are the quantities of Feed, Vapor
produced, Crystals formed and mother liquor
obtained.
x
F
, x
V
, x
C
, x
L
are the weight fraction of solute in the
feed , vapor ,crystal and mother liquor.
The value of x
V
will always be zero because vapor
does not contain solids.
The value of x
C
is 1 for anhydrous crystal and is
less than 1 for hydrated crystal.
For hydrated crystal x
C
is calculated as the ratio of
wt of anhydrous crystal to the wt of hydrated
crystal
% yield: Percentage yield is the percentage ratio
of crystals obtained to the solute entering the
crystallizer
34

Definitions
% Saturation =
(Weight of solute / Weight of
solvent)actual
.100
Weight of solute / Weight of solvent) at
saturation
% Yield =
kg solute crystals obtained
.100
kg solute in feed
35

An aqueous solution of Na
2
SO
4
is saturated
at 35
0
C. Calculate the percentage of
solute crystallized as Na
2
SO
4
.10H
2
O if it
is cooled to 27
0
C. Solubility at 27
0
C is 23.3
% Na
2
SO
4
by weight and at 35
0
C is 32.5
% by weight.
F
xF=0.325
27C
L, x
L
=0.233
Crystals
Na
2
SO
4
.10H
2
O
36
Basis : 100kg Na
2
SO
4
.H
2
O solution
Overall balance F = C + L
Na
2
SO
4
balance F (0.325) = C (0.441) + L (0.233)
32.5 = C (0.441) + (100 C) (0.233)
C = 44.23 kg
441 . 0
322
142
10
2 . 4 2
4 2
= = =
O H SO Na
SO Na
x
C
Yield =
(44.23) (0.441)
100=60%
100 (0.325)
37
A crystallizer is charged with 7500 kg of an
aqueous solution at 104
0
C, 29.6 % by
weight of which is anhydrous sodium
sulphate. The solution is cooled. During
cooling operation 5 % of water originally
present was lost, as a result, crystals of
Na
2
SO
4
.10H
2
O crystallize out. The mother
liquor is found to contain 18.3% by weight
of anhydrous salt. Calculate the yield of
crystals and quantity of mother liquor.
38

F=7500 kg
xF=0.296
xH20=0.704
V
C
L
xL=0.183
xC=0.441
Basis : 7500 kg of feed
Water in the feed = 7500 (0.704) =5280 kg
Amount of water lost = 5280(0.05) = 264 kg
39

Overall balance: F = V + C + L
7500 = 264 + C + L
C + L =7236
Na
2
SO
4
balance:
7500 (0.296) = C (0.441) + L (0.183)
But L = (7236 C) ; C = 3472.13 kg
Mother liquor L = 3763.86 kg
% Yield =
(3472.13) (0.441)
.100=68.97%
7500 (0.296)
40

150 kg of saturated solution of AgNO
3
at 100
0
C is
cooled to 20
0
C. The crystals are filtered out. The
wet filter cake contains 80% solid crystals and 20%
saturated solution by mass, is sent to the drier.
Calculate the amount of water that must be
removed to get moisture free product. Also
calculate the weight of dry AgNO
3
obtained
Solubility of AgNO
3
@100
0
C = 952g / 100g water and
@20
0
C = 222g /100g water
41

C
F 150 kg
wet, Xc=0.8
Sat.soln.=0.2
XF= 0.9051
689 . 0
222 100
222
=
+
=
L
X L
952 100
952
+
=
F
X
Dry crystals
Drier
water
42

Basis : 150 kg AgNO
3
solution at 100
0
C
Overall balance F =L + C or L = 150 - C
Solute balance F (0.9051) = L (0.689) + C (0.8) + [C
(0.2)] 0.689
C = 130.226 kg
Dry crystals = 130.226 x 0.8 = 104.181 kg
With salt solution = 130.226 104.181 = 26.045 kg
Amount of salt solution = C (0.2) =130.226(0.2) =26.052
kg
Amount of water in this = 26.052 (1- 0.689) = 8.102 kg
Solute in salt solution = 26.052 (0.689) = 17.945 kg
Total dry crystals (dry, x
c
= 1) = (17.945 + 104.181 ) kg
43

Overall balance: F=L+C, 1000=L+C
L=1000-C
NaNO
3
balance: Fx
F
= Lx
L
+ Cx
C
,
1000x0.49= (1000-C) 0.445+C,
490=445-0.445C+C
Therefore C=81.08 %
Yield=(crystal obtained/solute entering)X 100
= (81.08/1000x0.49)x100=16.55%
44
45
1000 kg of 25% by weight solution of sodium nitrate is
concentrated to saturation by evaporation. The solution
is cooled to 20C. The crystals of sodium nitrate are
removed by filtration. The wet crystals carry 10% by
weight mother liquor. This is dried. The solubility of
sodium nitrate is 1.76kg per kg of water at 100C and
0.88 kg per kg water at 20C. Calculate the amount of
water to be evaporated to get a saturated solution at
100C.and the total weight of sodium nitrate obtained.
Crystallization
V=607.966,x
V
=0
20 C,L,x
L
=0.88/1.88=0.468
F=1000 kg ,
x
F
=0.25
C,x
C
= 0.9
Water
48
Dry crystal from crystallizer Cx
C
=138.95 x 0.9=125.055 kg
Mother liquor adhering to crystal= 138.95x0.1 = 13.895 Kg
Solute in mother liquor adhering = 13.895 x0.468 = 6.503 Kg
Water in mother liquor adhering = 13.895 x(1-0.468)=7.395Kg
Water to be removed in drier = 7.395 Kg
Total dry crystal obtained after drying= 125.055 + 6.503=
131.558 Kg
Water to be evaporated to get saturated solution at 100
0
C=
607.966 Kg
Total weight of dry crystal obtained = 131.558 Kg
50

n= .9302 n=67.3 moles
Over all balance for K
0.21 m =1000
m = 4762 kg/hr
Material balance around crystallizer
m=m+m+m
m=3671
m=.95 (m + m)
2073 kg/hr
62

n= .9302 n=67.3 moles
Over all balance for K
0.21 m =1000
m = 4762 kg/hr
Material balance around crystallizer
m=m+m+m
m=3671
m=.95 (m + m)
2073 kg/hr
63



























Introduction to Extraction Processes
Equilibrium relations in Extraction using Triangular chart
Single- Stage Equilibrium Extraction
Equipment for Liquid-Liquid Extraction
Application of Extraction in Bio process
Solving fundamental material balance on single stage and multi stage Extraction
When separation by distillation is very difficult e.g. close-boiling mixture, liquid
extraction is one of the main alternative to consider.
Extraction depends on the partitioning of the biomolecules between liquid phases
-Miscibility of two liquid phases
-Rate of equilibration of biomolecules between two phases
Liquid-liquid extraction (or solvent extraction)
Liquid-Liquid extraction is a mass transfer operation in which a liquid solution (feed) is
contacted with an immiscible or nearly immiscible liquid (solvent) that exhibits
preferential affinity or selectivity towards one or more of the components in the feed.
Two streams result from this contact(feed and Solvent):
a) Extract is the solvent rich solution containing the desired extracted solute.
b) Raffinate is the residual feed solution containing little solute.
Introduction to Extraction Processes
Liquid-liquid extraction principle

When Liquid-liquid extraction is carried out in a test tube or flask the two immiscible
phases are shaken together to allow molecules to partition (dissolve) into the preferred
solvent phase.



One feed stream contacts one extraction solvent
Mixture divides into equilibrium extract and raffinate phases
Distribution of solute at equilibrium is defined as the partition coefficient
K = y/x
K depends on many factors
-Size of molecule being extracted
-pH
-Types of solvent
-Temp.
-Concentration and MW of polymers or salt in phase







Each of the three corners represents a pure component A, B, or C.
Line sloping to the right represents various amounts of component B
Point M represents a mixture of A, B, and C.
The perpendicular distance from the point M to the base AB represents the mass
fraction x
C
. The distance to the base CB represents x
A
, and the distance to base AC
represents x
B
.

Liquid C dissolves completely in A or in B.
Liquid A is only slightly soluble in B and B slightly soluble in A.
The two-phase region is included in the curved envelope.
Original mixture of composition M will separate into two phases a and b which are on
the equilibrium tie line through point M.
The two phases are identical at point P, the Plait point.

Define the composition of point A, B, C, M, E, R, P in the ternary-mixture

Point A = 100% Water
Point B = 100% Ethylene Glycol
Point C = 100% Furfural
Point M = 30% glycol, 40% water, 30% furfural
Point E = 41.8% glycol, 10% water, 48.2% furfural
Point R = 11.5% glycol, 81.5% water, 7% furfural


The miscibility limits for the furfural-water binary system are at point D and G.
Point P (Plait point), the two liquid phases have identical compositions.
DEPRG is saturation curve; for example, if feed 50% solution of furfural and glycol, the
second phase occurs when mixture composition is 10% water, 45% furfural, 45% glycol
or on the saturation curve.


The system acetic acid (A) water (B) isopropyl ether solvent (C). The solvent pair B
and C are partially miscible.


An original mixture weighing 100 kg and containing 30 kg of isopropyl ether (C), 10 kg of acetic
acid (A), and 60 kg water (B) is equilibrated and the equilibrium phases separated. What are the
compositions of the two equilibrium phases?
Solution:
Composition of original mixture is
x
c
= 0.3, x
A
= 0.10, and x
B
= 0.60.
The two phases in liquid-liquid extraction must be brought into intimate contact with a
high degree of turbulence in order to obtain high mass-transfer rates.
Liquid extraction: Density difference between the two phases is not large and separation
is more difficult.
Liquid extraction equipment
Mixing by mechanical agitation
Mixing by fluid flow themselves
Mixer-Settles for Extraction




Extraction of valuable products from fermentation broth.
Purification of heat sensitive materials
- Such as pharmaceuticals, flavors, fragrances and food products.
-Extraction of caffeine from coffee beans
-ProExtraction is the removal of solute (active constituent) from a liquid mixture using a
solvent

This method is used to separate miscible liquid mixtures and is preferred over distillation
when the mixture forms azeotrope, when the mixture is sensitive to heat and also when
the relative volatility of the mixture is near to one

Feed is a mixture of diluent (A) and solute(C).To this mixture a solvent (B) is added and
the mixture is agitated for better contacting. tein extraction using polymer or
polymer/salt mixtures



The solute distributes into B.
After sufficient time of contact the agitation is stopped and the mixture is allowed to
settle to get two layers separated.
The solvent rich layer which overflows is called extract and the diluents rich layer which
settles down is called the raffinate.
The diluent and solvent are immiscible in each other.
In such cases the extract and raffinate will contain only two components namely B and
C & A and C.
In practice getting a solvent which is perfectly immiscible with diluents may not be
possible and solvents with partial miscibility are used. When partially miscible solvents
are used the extract and raffinate will contain three components namely A, B and C.
Single Stage Calculations


Overall balance: F+S= E+R
Solute balance: Fx
F
+ Sx
S
= Ex
E
+ Rx
R


Ethylene tetrachloride C
2
Cl
4
, water H
2
O and isopropyl alcohol C
3
H
7
OH separate in to
two phases in composition ranges.
The equilibrium data are given below
C
2
Cl
4
rich layer: C
2
Cl
4
-94%, C
3
H
7
OH-5.2%, H
2
O-0.8%
H
2
O rich layer: C
2
Cl
4
-0.9%, C
3
H
7
OH-28.1%,H
2
O-71%
To a 100 kg mixture containing 30% C
3
H
7
OH and 70% H
2
O, 50kg of C
2
Cl
4
is added,

thoroughly mixed and allowed to settle. Calculate the amount
of phases formed.

Basis: 100 kg feed and 50 kg solvent
Let x be the weight of C
2
Cl
4
layer,
y be the weight of H
2
O layer
Overall balance: x+y=150 (1)
C
3
H
7
OH balance: 100x0.3=x(0.052)+y(0.281),
30=0.052x+0.281y (2)
From (1) y=150-x
Substituting for y in (2), 30=0.052x+0.281(150-x), 30= 0.052 x+42.15-0.281x
0.229x=12.15 therefore x=12.15/0.229=53.057
Y=150-x=150-53.057=96.943
Weight of C
2
Cl
4
layer=96.943 kg
Weight of water layer=53.057 kg
A mixture of water and phenol constitutes a mutually soluble two phase system. At 30C
the phenol rich layer contains 70 weight % phenol and water rich layer contains 91
weight % water. A mixture is made up of 50 kg phenol and 50 kg water at
30C.Calculate the weight of phenol rich layer and water rich layer after the system
attains equilibrium







Basis: 50 kg phenol and 50kg water
Let x be the phenol layer and y be the water layer
Overall balance: x+y=100 (1)
Phenol balance: 50=0.7x+0.09y (2)
From (1) y=100-x, substituting for y in (2)
50 = 0.7x+0.09(100-x)
50=0.7x+9-0.09x,
0.61 x=50-9=41,
therefore x=41/0.61=67.21,
y=100-67.21=32.79
Weight of phenol layer=67.21kg,
Weight of water layer=32.79 kg
A 100 kg mixture consisting of 27.8 % acetone A, 72.2 % chloroform B, by weight is to
be batch extracted with a mixed solvent at 25
0
C . This mixed solvent of unknown
composition is known to contain water S
1
and acetic acid S
2
. The mixture of the original
mixture and the mixed solvent is shaken well, allowed to attain equilibrium and
separated in to two layers. The composition of two layers is given below.
Layer A B
S
1
S
2

Upper layer 7.5 3.5 57.4 31.6
Lower layer 20.3 67.3 2.8 9.6
Find 1) the quantities of two layers
2) weight ratio of mixed solvent to original mixture
3) composition of mixed solvent
Basis : 100 kg of original mixture

Balance for A 100 (0.278) = x (0.075) + y (0.203)

Balance for B 100(0.722) = x (0.035) + y (0.673)

Solving x = 93.5 kg y = 102.4 kg x + y = 195.9 kg

Mixed solvent = 195.9 100 = 95.9 kg
= 0.959
Balance of S
1
: 95.9 (S
1
) = 93.5 (0.574) + 102.4 (0.028) S
1
= 56.48 kg

Balance of S
2
: 95.9 (S
2
) = 93.5 (0.3136) + 102.4 (0.096) S
2
= 39.34 kg
Solvent Weight Weight %
S1 56.48 58.94
S2 39.34 41.06
95.82 100.00
Soya bean seeds are extracted with hexane in batch extractors. The flaked seeds
contain 18.6% oil, 69.6% solids and 12.4% moisture. At the end of the process, cake
(meal) is separated from hexane oil mixture. The cake analysis yields 0.8% oil, 87.7%
solids, and 11.5% moisture. Find the percentage recovery of oil. All percentages are by
weight.
100
9 . 95
=
ture Orginalmix
nt Mixedsolve


% 61 . 96 100 .
6 . 18
97 . 17
=
A aqueous solution of pyridine containing 27 weight % pyridine and 73 weight % water is to be
extracted with chloro benzene. The feed and the solvent are mixed well and allowed to stand for
phase separation. The extract phase contains 11 % pyridine , 88.1 % chloro benzene and 0.9
% water by weight . The raffinate phase contains 5 % pyridine and 95 % water by weight.
Calculate a) the quantities of two layers(phases)
b) the weight ratio of solvent to feed based on 100 kg of feed.

Basis: 100 kg feed
Overall material balance F + Z = X + Y
100 + Z = X + Y Pyridine material balance 27
= X (0.11) + Y (0.05)
Water material balance 73 = X (0.009) + Y (0.95)

4 kg, y = 74.87 kg, z = 186.24 k




Oil is extracted from cod livers in a multiple counter current extractor using ethyl ether as a
solvent. The fresh livers are charged in to the extractor at the rate of 1000 kg / hr and contain
25.7 % oil. Pure ether enters from the bottom of the extractor and the overflow from the
extractor contains 70 % oil. The underflow contains 0.23 kg solution per kg oil free solid and is
known to contain 12.8% oil. Find the flow rate of ether and percentage recovery of oil.


8624 . 1
100
24 . 186
= =
Feed
Solvent
Basis : 1000 kg / hr fresh lever

All solids will be in underflow only.
Inert solids in feed = 743 kg = inert solids in raffinate
Quantity of soln retained by inert solids in raffinate
= (743)(0.23) = 170.89 kg
Raffinate Oil = (170.89) (0.128) = 21.87 kg

Ether = (170.89) (0.872) = 149.016 kg
Oil=(oil entering-oil in raffinate)
Extract Oil = 257 21.87 = 235.13 kg
Ether = 235.13 (30/70) = 100.77 kg
Extract oil=235.13 which contributes to 70%
ie 235.13= E (0.7) or E = 335.9 kg
Solvent = 100.77 kg
Total solvent ether entering = 100.77 + 149.016 = 249.786 kg
F = 1000 kg E = 335.9
S = 249.786 kg R, solids = 743.00
Oil + solvent = 170.886
1249.786 kg 1249.786 kg

It is desired to extract acetone from a feed containing acetone and H
2
O using
chloroform as the solvent, in two cross current extraction as shown in figure.
Assume that H
2
O and chloroform are immiscible. The following data are given for the
process.
The feed is equimolar mixture of acetone and H
2
O
The quantities of chloroform used in the two stages are equal.
60 mol% of the acetone in the feed is extracted in the stage

The extract and raffinate phases exiting from each stage are in equilibrium. The
equilibrium relation for the distribution of acetone is given by.
Moles of acetone in H
2
O
rich phase
=
2
Moles of acetone in chloroform rich
phase
Moles of H
2
O in H
2
O rich
phase
Moles of chloroform in chloroform
rich phase
1. Determine the quantity of chloroform used in each stage per mole
of feed.
2. Determine the mole fraction of acetone in the final product stream.
Basis: 1.0 mol of feed
Acetone, A
1
= 0.5 mol
H
2
O, W
1
= 0.5 mol because of equimolar feed
In stage I, 60% acetone is extracted,
Acetone in stream 5 = A
5
= (0.5)(0.6) = 0.3 moles
Acetone in stream 2 = A
2
= 0.5 0.3 = 0.2 moles
If S moles of chloroform are used, then we have




Moles of acetone in
H
2
O rich phase
=
2
Moles of acetone in
chloroform rich phase
Moles of H
2
O in Moles of chloroform in
H
2
O rich phase chloroform rich phase






S=0.667 moles

Quantity of chloroform used in each stage per mole of feed=0.667 moles
To determine the mole fraction of acetone in the final product stream.
A
2
= 0.2 = sum of acetone in stream 3 & 7 = A
3
+ A
7

A
7
= 0.2 - A
3,
W
3
= 0.5 moles, S
6
= 0.667 moles = S
7

Moles fraction of acetone in the final product stream( 7),
= (0.12) / (0.12 + 0.5) = 0.1935
Quantity of chloroform used in each stage per mole of feed=0.667 moles
Or A
3
= 0.12 mol


3 . 0
2
5 . 0
2 . 0
s
=
0.667
A
2
5 . 0
A
7 3
=
0.667
) A - (0.2
2
5 . 0
A
3 3
=