A Project report on

DESIGNING OF DISTILLATION COLUMN FOR THE

EFFECTIVE RECOVERY OF IPA(ISOPROPYL
ALCOHOL)FROM IPA-WATER SYSTEM
BACHELOR OF TECHNOLOGY
IN
CHEMICAL ENGINEERING
Submitted By
P.ANUSHA(N110063)
G.LAKSHMI(N110057)
G.PALLAVI(N110101)
CH.MANSURUNNISA(N110639)
Under the Guidance of
P.SRINIVAS REDDY
Sr.manager
process engineering department

RGUKT-APIIIT,NUZVID
MYLAVARAM ROAD, KRISHNA DISTRICT,ANDHRA PRADESH-521201

ACKNOWLEDGEMENT
We would like to express our sincere gratitude to our guide Mr. SRINIVAS
REDDY&Mr.NAGARJUNA, AUROBINDO PHARMA LIMITED, for their faithful support
and encouragement in spite of their busy and tiring schedule and aiding us in an
valuable insight and practical knowledge in the Chemical industry.

We would also like to take this opportunity to thank MR.K.GAURISHANKAR

(HR) for giving permission and allowing us to undergo our training and for their
cooperation in endowing us the necessary details about the plant. We would like to
extend our sincere thanks to all of them.

We would like to express our special gratitude and thanks to the Head of
The Department, Mr.P.BANGARAIAH for giving me such attention and time.

We are highly indebted to our project guide Sr.manager P.SRINIVAS

REDDY for his guidance and constant supervision as well as for providing necessary
information regarding the project & also for their support in completing the project.
P.ANUSHA(N110063
G.LAKSHMI(N110057)
G.PALLAVI(N110101)
CH.MANSURUNNISA(N110639)

INDEX
1. COMPANY PROFILE
2. OPERATIONS INVOLVED
2.1 DISTILLATION
2.2 MAIN COMPONENTS OF DISTILLATION COLUMN
2.3 BASIC OPERATIONS AND TERMINOLOGY
2.4 TYPES OF DISTILLATION
2.5 APPLICATION OF DISTILLATION
2.6 TYPES OF DISTILLATION COLUMNS
3. EQUIPMENTS USED
3.1 HEAT EXCHANGERS AND ITS PRINCIPLES
3.2 PREHEATER
3.3 PUMPS
3.4 COOLING TOWERS
4. ACTIVE PHARMACETICAL INGREDIENT-API
5. SOLVENT RECOVERY PROCESS
5.1 PROCESS DESCRIPTION
6. DESIGNING OF DISTILLATION COLUMN FOR IPA-WATER SYSTEM
6.1 CALCULATION OF NUMBER OF STAGES
6.2 TOWER SPECIFICATIONS
6.3 REBOILER AND CONDENSER CALCULATION
7. ALTERNATIVE SOLVENT RECOVERY METHODOLOGY FOR IPA WATER
SYSTEM
7.1 BATCH DISTILLATION PROCESSES
7.2 EXPERIMENTAL METHOD
8. USES OF ISO PROPYL ALCOHOL
9. SAFETY ASPECTS
10. CONCLUSION
11. REFERENCES

1.COMPANY PROFILE
Aurobindo Pharma was born of a vision. Founded in 1986 by Mr.
P.V.Ramaprasad Reddy, Mr. K.Nityananda Reddy and a small, highly committed group
of professionals, the company became a public venture in 1992. It commenced
operations in 1988-89 with a single unit manufacturing semi synthetic penicillins (SSPs)
at Pondicherry. Aurobindo Pharma had gone public in 1995 by listing its shares in
various stock exchanges in the country. The company is the market leader in semisynthetic penicillin drugs. It has a presence in key therapeutic segments like SSPs,
cephalosporins, antivirals, CNS, cardio-vascular, gastroenterology, etc. Over the years,
the Aurobindo Pharma has evolved into a knowledge driven company. It is R&D
focused, has a multi-product portfolio with multi-country manufacturing facilities, and
is becoming a marketing conglomerate across the world.
Aurobindo Pharma created a name for itself in the manufacture of bulk actives,
its area of core competence. After ensuring a firm foundation of cost effective
production capabilities and a clutch of loyal customers, the company has entered the
high margin speciality generic formulations segment, with a global marketing network.
The formulation business is systematically organised with a divisional structure, and
has a focused team for each key international market. Aurobindo believes in gaining
volume and market share in every business/segment it enters
Aurobindo has invested significant resources in building a mega infrastructure
for APIs and formulations to emerge as a vertically integrated pharmaceutical
company. Aurobindo has five units for APIs and four units for formulations are
designed for the regulated markets.
Aim / Vision / Mission:

Vision
"To become Asia's leading and one among the top 15 generic Pharma companies in
the world, by 2015
Mission
Aurobindo's mission is to become the most valued Pharma partner for the World
Pharma fraternity by continuously researching, developing and manufacturing a wide
range of pharmaceutical products complying to the highest regulatory standards.

Team / Manpower
Mr.P.V.Ramaprasad Reddy- Chairman
Mr.K.Nityananda Reddy-

Managing Director

Mr. M. Madan Mohan Reddy- Whole-time Director

Dr.M.Sivakumaran Dr.P.L.Sanjeev Reddy-

Whole-time Director
Non-Executive Director

Dr. D. Rajagopala Reddy - Non-Executive Director

Mr.K.Ragunathan-

Non-Executive Director

AWARDS AND ACHIEVEMENTS (OVER RECENT PERIOD OF YEARS)

2010- Aurobindo Pharma has received final approval from the United States Food and
Drug Administration for its product Ceftazideme injection in different dosages.

2011-Aurobindo Pharma receives USFDA tentative approval for Famciclovir Tablets

Aurobindo Pharma Announced Strategic Divestment of Aurobindo (Datong)
Bio Pharma,

China.

Aurobindo Pharma received USFDA tentative approval for Levofloxacin

Tablets.

 Aurobindo Pharma received USFDA tentative approval for Venlafaxine

Extended Release Capsules.
Aurobindo Pharma received USFDA tentative approval for Famclclovir Tablets.
Aurobindo Pharma received Platinum Certificate of Outstanding Exports Award
from Pharmexcil.
Company has splits its Face value of Shares from Rs 5 to Re 1.

2012-Aurobindo Pharma received final approvals for QuetiapineFumarate Tablets.

Aurobindo Pharma received final approval for Olanzapine Tablets".
Aurobindo Pharma got USFDA nod for anti-HIV drugs Lamivudine and
Zidovudine
Aurobindo Pharma got USFDA nod to launch Clopidogrel tablets.
Aurobindo Pharma received final approval for Metformin Hydrochloride
Extended Release Tablet.
OUR VALUES

BUSINESS CARE:
Operational Excellence is a continuous journey of excellence wherein every
employee can see the flow of value to the customer and fix that flow when it
fails to deliver.
Stakeholder Orientation means being responsive to a group or
individual who are/is interested in the achievement of the firm's
objectives.
Quality is a measure of excellence or a state of being free from defects
and innovision is discovering present and future business opportunities.
PEOPLE CARE:
It deals with the core philosophy of the management of human
resources such as Talent Development, Talent Recognition, and Talent
Welfare.
Fairness, humility and respect for individuals Appreciating each other's
talent, ideas and treating all individuals in a consistently humble
Business care is the continuous monitoring and improvement of
performance indicators.
fair and equal manner.
Teamwork is the capability of people within and among groups to
continuously improve the performance.
Applied Learning Emphasis on Learn-by-Doing that empowers and
upgrades skills of employees.
ORGANIZATION CARE: It deals with the action and words of employees that
lead to building a Greater Aurobindo.

 Accountability is to own up responsibility for outcome, leading to

actualizing the commitment at work.
Integrity:Steadfastness to honesty in our business transactions and
interfaces .It involves conscience and consistent action by choice.
Achievement: A strong desire and drive to focus on performance and
desired business results.

2.OPERATIONS INVOLVED
2.1 DISTILLATION
Distillation is a process in which miscible liquids are separated based on their
physical

properties, specifically, relative volatilities. A liquid can be classified as

volatile when it is readily vaporized at a relatively low temperature. The boiling of the
more volatile components of the mixture drives the distillation process. When the
vapor is cooled, the more volatile material condenses in a greater proportion than the
less volatile material. It is a unit operation in which constituents of liquid mixture are
separated by using thermal energy depends upon the relative volatility of constituents
by partial vaporization and condensation. Distillation with rectification or Fractional
distillation gives almost pure product. The product removed from top is called the
distillate or overhead product and that removed from the bottom is called the bottom
product. This unit operation is also termed as fractional distillation or fractionation.
Distillation is a widely used operation in the petroleum, chemical,
petrochemical, beverage and pharmaceutical industries. It is important not only for
the development of new products, but also for the recovery and reuse of volatile
liquids. For example, pharmaceutical manufacturers use large quantities of solvents,
most of which can be recovered by distillation with substantial savings in cost and
pollution reduction. While distillation is one of the most important unit operations, it is
also one of the most energy intensive operations. It is easily the largest consumer of
energy in petroleum and petrochemical processing, and so, must be approached with
conservation in mind. Distillation is a specialized technology, and the correct design of
equipment is not always a simple task.
There are many types of distillations based on separation technique used. Here
we follow the simple distillation. Distillation is the combination of two unit operations,

evaporation and condensation. Evaporation takes place in the column and

condensation occurs in condenser.
2.2 MAIN COMPONENTS OF DISTILLATION COLUMNS
Distillation columns are made up of several components, each of which is used
either to transfer heat energy or enhance material transfer.

A typical distillation contains several major components

1. A vertical shell where the separation of liquid components is carried out Column
internals such as trays/plates and/or packings which are used to enhance component
separations.
2. A reboiler provide the necessary vaporization for the distillation process
3. A condenser to cool and condense the vapour leaving the top of the column.
4. A reflux drum to hold the condensed vapour from the top of the column so that
liquid (reflux) can be recycled back to the column.
5. The vertical shell houses the column internals and together with the condenser and
reboiler, constitutes a distillation column.

Fig -1 A schematic of a typical distillation unit with a single feed and two product
streams

2.3 BASIC OPERATION AND TERMINOLOGY

The liquid mixture that is to be processed is known as the feed and this is
introduced usually somewhere near the middle of the column to a tray known as the
feed tray. The feed tray divides the column into a top (enriching or rectification)
section and a bottom (stripping) section. The feed flows down the column where it is
collected at the bottom in the reboiler.
Heat is supplied to the reboiler to generate vapour. The source of heat input
can be any suitable fluid, although in most chemical plants this is normally steam. In
refineries, the heating source may be the output streams of other columns. The
vapour raised in the reboiler is re-introduced into the unit at the bottom of the
column. The liquid removed from the reboiler is known as the bottoms product or
simply, bottoms

Fig-2 schematic diagram of column

The vapour moves up the column, and as it exits the top of the unit, it is
cooled by a condenser. The condensed liquid is stored in a holding vessel known as
the reflux drum. Some of this liquid is recycled back to the top of the column.

This is called the reflux. The condensed liquid that is removed from the system is
known as the distillate or top product.

Thus, there are internal flows of vapour and liquid within the column as well as
external flows of feeds and product streams, into and out of the column.

Formulae Used and Definitions:

1. Solvent Added: it is the solvent input to the reactor for a particular process. Its unit is
kg (for batch processes) or kg/s (continuous processes).

2. Solvent Recovered: it is the solvent recovered after the distillation. Solvent must have
the permissible purity percentage for reusing the solvent. Units are same as above.

3. Solvent Consumed: it is the difference between the input solvent and recovered
solvent. Mostly it goes in the waste. Ideally, solvent should not be consumed because
it only provides the medium for reaction b/w constituents.

4. Consumption Coefficient (CC): the ratio of solvent consumed to the product produced
for same reference of time (for the continuous process) or for the same batch (for
batch process).

CC=solvent consumed/product produced

5. Percentage Recovery: it is the percentage of recovered solvent to the solvent input in

the process.
% recovery =
6. Total Consumption of solvent over a year: it is the solvent consumed in a financial
year. We calculate it by given formula
= CC total product produced in financial year
7. Total solvent consumption in a year in rupees:
= total consumption budgeted price
2.4 Types of Distillation:
Batch Distillation
Continuous Distillation
Simple Distillation
Fractional Distillation
Steam Distillation

Vacuum Distillation
Extractive Distillation

Batch Distillation
Batch distillation is a technique used for separating two or more miscible liquid or
vapor mixtures that are separated into their component fractions of desired purity.
This is accomplished by the application and removal of heat. The separation is
based on the boiling points of the mixture components. You will operate this column at
total reflux, Periodically taking small distillate samples, and determines the number of
theoretical trays. In the column.
Distillation is the most common separation technique, however it does suffer
from Some disadvantages (Refer to Table 1 for applications). It usually takes a large
amount of Heat, both in terms of heating and cooling, to run a distillation apparatus. This
heat requirement can contribute to more than 50% of plant operating cost. The best way

to cut Down on operating costs is to improve the distillation units efficiency and
operation via Process control and optimization.
Batch distillation is desirable when small quantities of high valued chemicals need
to be Separated. The biggest advantage to using a batch column is its flexibility. This
allows one to deal with unknowns in the feed or product specifications. In a batch system,
the column can handle different mixtures by simply changing its operating conditions. The
main disadvantage to using a batch system is that the longer the components are
exposed to high temperatures, the better the chances that the components are broken
down via thermal degradation. Along with this, the energy requirements are usually
higher for a batch system. A column is built for separating a specific mixture in continuous
distillation. Therefore, the distillation column apparatus needs to be modified for each
new mixture that is to be separated.
In order to provide the highest contact area, a column is filled with packing that
has a large volumetric area and that has high porosity. The liquid trickles down the
column and through the packing as small droplets. The gas is sent through the column in
the upward direction. This countercurrent flow of liquid and vapor exists only in a packed
column. Ideally, the porosity of the packing should not hinder the gas flow through the
column. In this lab, the packing in the column is glass sand. The distillation column also
contains a condenser, which cools and condenses the vapor leaving the top of the
column. A reboiler is connected to the bottom of the distillation apparatus and it provides
the reboil heat that is necessary for distillation.
Continuous Distillation
Continuous distillation is an ongoing distillation in which a liquid mixture is
continuously (without interruption)

fed into the process and separated fractions are

removed continuously as output streams as time passes during the operation. Continuous
distillation produces at least two output fractions, including at least one volatile distillate
fraction, which has boiled and been separately captured as a vapor condensed to a liquid.
There is always a bottoms (or residue) fraction, which is the least volatile residue that has
not been separately captured as a condensed vapor.

Continuous distillation differs from batch distillation in the respect that

concentrations should not change over time. Continuous distillation can be run at
a steady state for an arbitrary amount of time. For any source material of specific
composition, the main variables that affect the purity of products in continuous distillation
are the reflux ratio and the number of theoretical equilibrium stages (practically, the
number of trays or the height of packing). Reflux is a flow from the condenser back to the
column, which generates a recycle that allows a better separation with a given number of
trays. Equilibrium stages are ideal steps where compositions achieve vapor-liquid
equilibrium, repeating the separation process and allowing better separation given a
reflux ratio. A column with a high reflux ratio may have fewer stages, but it refluxes a large
amount of liquid, giving a wide column with a large holdup. Conversely, a column with a
low reflux ratio must have a large number of stages, thus requiring a taller column.

Separation operations achieve their objective by the creation of two or more

coexisting zones which differ in temperature, pressure, composition, and phase state.
Each molecular species in the mixture to be separated reacts in a unique way to differing
environments offered by these zones. Consequently, as the system moves toward
equilibrium, each species establishes a different concentration in each zone, and this
result in a separation between the species. The separation operation called continuous
distillation utilizes vapour and liquid phases at essentially the same temperature and
pressure for the co-existing zones.
General improvements
Both batch and continuous distillations can be improved by making use of
a fractionating column on top of the distillation flask. The column improves separation by
providing a larger surface area for the vapor and condensate to come into contact. This
helps it remain at equilibrium for as long as possible. The column can even consist of
small subsystems ('trays' or 'dishes') which all contain an enriched, boiling liquid mixture,
all with their own vapor-liquid equilibrium.

Simple Distillation
In simple distillation, all the hot vapors produced are immediately channeled into a
condenser that cools and condenses the vapors. Therefore, the distillate will not be pure its composition will be identical to the composition of the vapors at the given temperature
and pressure, and can be computed from Raoult's law.
As a result, simple distillation is usually used only to separate liquids whose boiling
points differ greatly (rule of thumb is 25 C), or to separate liquids from in volatile solids
or oils. For these cases, the vapor pressures of the components are usually sufficiently
different that Raoult's law may be neglected due to the insignificant contribution of the
less volatile component. In this case, the distillate may be sufficiently pure for its intended
purpose.

Fractional distillation
For many cases, the boiling points of the components in the mixture will be
sufficiently close that Raoult's law must be taken into consideration. Therefore, fractional
distillation must be used in order to separate the components well by repeated
vaporization-condensation cycles within a packed fractionating column. This separation,
by successive distillations, is also referred to as rectification.
As the solution to be purified is heated, its vapors rise to the fractionating
column. As it rises, it cools, condensing on the condenser walls and the surfaces of the
packing material. Here, the condensate continues to be heated by the rising hot vapors; it
vaporizes once more. However, the composition of the fresh vapors is determined once
again by Raoult's law. Each vaporization-condensation cycle (called a theoretical plate) will
yield a purer solution of the more volatile component. In reality, each cycle at a given
temperature does not occur at exactly the same position in the fractionating
column; theoretical plate is thus a concept rather than an accurate description. More
theoretical plates lead to better separations.
Steam distillation
Steam distillation is a special type of distillation (a separation process) for
temperature sensitive materials like natural aromatic compounds. Many organic
compounds tend to decompose at high sustained temperatures. Separation by normal
distillation would then not be an option, so water or steam is introduced into the
distillation apparatus. By adding water or steam, the boiling points of the compounds are
depressed, allowing them to evaporate at lower temperatures, preferably below the
temperatures at which the deterioration of the material becomes appreciable. If the
substances to be distilled are very sensitive to heat, steam distillation can also be
combined with vacuum distillation. After distillation the vapors are condensed as usual,
usually yielding a two-phase system of water and the organic compounds, allowing for
simple separation.

Vacuum distillation
At atmospheric pressure, di methyl sulfoxide boils at 189C. Under a vacuum, it
distils off into the connected receiver at only 70C.Vacuum distillation is a method of
distillation whereby the pressure above the liquid mixture to be distilled is reduced to less
than its vapor pressure (usually less than atmospheric pressure) causing evaporation of
the most volatile liquid(s) (those with the lowest boiling points). This distillation method
works on the principle that boiling occurs when the vapor pressure of a liquid exceeds the
ambient pressure. Vacuum distillation is used with or without heating the mixture.
This technique is also very useful for compounds which boil beyond
their decomposition temperature at atmospheric pressure and which would therefore be
decomposed by any attempt to boil them under atmospheric pressure.
Extractive distillation
It is defined as distillation in the presence of a miscible, high boiling, relatively
non-volatile component, the solvent, that forms no azeotrope with the other components
in the mixture. The method is used for mixtures having a low value of relative volatility,
nearing unity. Such mixtures cannot be separated by simple distillation, because the
volatility of the two components in the mixture is nearly the same, causing them to
evaporate at nearly the same temperature at a similar rate, making normal distillation
impractical.
The method of extractive distillation uses a separation solvent, which is generally
non-volatile, has a high boiling point and is miscible with the mixture, but doesn't form an
azeotropic mixture. The solvent interacts differently with the components of the mixture
thereby causing their relative volatilities to change. This enables the new three-part
mixture to be separated by normal distillation. The original component with the greatest
volatility separates out as the top product. The bottom product consists of a mixture of
the solvent and the other component, which can again be separated easily because the
solvent doesn't form an azeotrope with it. The bottom product can be separated by any
of the methods available.

2.5 APPLICATIONS OF DISTILLATION

The

application

of

distillation

can

roughly

be

divided

in

four

groups: laboratory scale, industrial distillation, distillation of herbs for perfumery and
medicinal (herbal distillate), and food processing. The latter two are distinctively different
from the former two in that in the processing of beverages, the distillation is not used as a
true purification method but more to transfer all volatiles from the source materials to the
distillate.
The main difference between laboratory scale distillation and industrial distillation
is that laboratory scale distillation is often performed batch-wise, whereas industrial
distillation often occurs continuously. In batch distillation, the composition of the source
material, the vapors of the distilling compounds and the distillate change during the
distillation.
In batch distillation, a still is charged (supplied) with a batch of feed mixture, which
is then separated into its component fractions which are collected sequentially from most
volatile to less volatile, with the bottoms (remaining least or non-volatile fraction)
removed at the end. The still can then be recharged and the process repeated.
In continuous distillation , the source materials, vapors, and distillate are kept at a
constant composition by carefully replenishing the source material and removing fractions
from both vapor and liquid in the system. This results in a better control of the separation
process.

2.6 TYPES OF DISTILLATION COLUMNS

Packed Columns
In a packed column, liquid-vapour mixing is promoted through a packed bed.
Packed beds provide true counter-current flow as vapour flows up and liquid flows down
the bed simultaneously. Distribution of the liquid and vapour flows is key to good
operation of these types of columns.

The packing itself comes in a variety of forms either as loose packing or as a preassembled grid. A number of different designs are available including Raschig Rings, Pall
Rings, Lessing Rings and Berl Saddles - as well as a number of proprietary designs. They
all aim to maximise the surface area per unit volume to maintain good vapour-liquid
contact and to minimize pressure drop.
Packing can be made in a range of material including ceramics, metal, glass and
plastic. Selection of materials of construction is based on the need for corrosion
resistance and weight limitations.

Fig-4.Different types of packing material

Fig-5.Structured packing

Fig-6.Super-Raschig rings
There are no hard and fast rules, the choice coming down to balance between
cost and performance. In general, plate columns are better at accommodating a wider
range of liquid and vapor flow rates. Packed columns rely on a good distribution of liquid
across the bed, performing poorly at low liquid flows. Packed columns are better at
handling corrosive or foaming liquids. A packed column has lower pressure drops than
plate column for the same duty. This makes them a better choice for low pressure drop
applications, such as in vacuum distillation. For column diameters less than 0.6 metres,
packing is normally cheaper than using plates. Large distillation columns are invariably
equipped with plates.
Advanced packings:
1.MELLAPAK PLUS):

Tray column
Trays are a series of plates arranged vertically up the column. The liquid
flows along each plate, over a weir and then under gravity flows down a downcomer to
the tray below. The height of the weir determines the quantity of liquid held on each
tray. The downcomer is taken beneath the liquid surface on the tray below to create a
vapour seal. The vapour flows upwards through perforations in the plate (the upward flow

is achieved by maintaining a pressure drop between the bottom and top of the column).
The vapour passes through the liquid on the tray and then travels up to the tray above.
The distance between each tray is important. If the tray spacing is too large, the column
becomes very high, increasing the capital cost. If the spacing is too low, there is a risk of
liquid becoming entrained with the vapour, reducing the column effectiveness. Spacing
between trays is typically around 60 cm.

Fig-7.Section of an industrial distillation tower showing detail of trays with bubble

caps
Detailed design is a specialist subject and will depend on conditions in the column
- in particular the relative rates of the vapour and liquid flows. If the vapour flow is too
low, the operation of the column becomes unstable. If the vapour flow is too high, liquid
entrainment reduces column performance. Excessive liquid flow will flood the column.
There are several styles of tray. The simplest is the sieve tray where vapour simply
flows through holes in the plate. More complicated designs (valve and bubble caps) have
a wider operating range as they reduce leakage of liquid through the hole at low vapour
flows.
The types of tray used in distillation columns are as follows:
THE SIEVE TRAY is simply a metal plate containing drilled holes through which the rising
vapor can pass into the liquid flowing across the tray.

THE VALVE TRAY is similar to the sieve type but, each hole is fitted with a flapper valve
which opens as vapor passes through the hole. This type is used where vapour velocity is
not constant and the valves prevent liquid from dumping through the holes at times of
low gas velocity.
THE BUBBLE-CAP TRAY is the most efficient separation device but, is also the most costly.
It consists of a number of 'Chimneys' or 'Risers' (small, short pipes set into the tray),
through which the vapor can pass. Fitted over the riser is a 'Cap' which causes the rising
vapor to turn through 180 . This forces the gas to 'Bubble' through the liquid flowing
across the tray. The liquid level on the tray is maintained below the top of the riser to
prevent dumping of liquid down the tower.
3 EQUIPMENTS USED
3.1 HEAT EXCHANGERS
A heat exchanger is a piece of equipment built for efficient heat transfer from one
medium to another. The media may be separated by a solid wall, so that they never mix,
or they may be in direct contact. They are widely used in space heating, refrigeration, air
conditioning, power

plants, chemical

plants,

petrochemical

plants, petroleum

refineries, natural gas processing, and sewage treatment. The classic example of a heat
exchanger is found in an internal combustion engine in which a circulating fluid known
as engine coolant flows through radiator coils and air flows past the coils, which cools the
coolant and heats the incoming air.

1. Shell and tube exchangers: used for all applications.

2. Double-pipe exchanger: the simplest type, used for cooling and heating.
3. Plate and frame exchangers (plate heat exchangers): used for heating and cooling.
4. Plate-fin exchangers.
5. Spiral heat exchangers.

The word exchanger really applies to all types of equipment in which heat is
exchanged but is often used specifically to denote equipment in which heat is exchanged
between two process streams. Exchangers in which a process fluid is heated or cooled by
a plant service stream are referred to as heaters and coolers. If the process stream is
vaporised the exchanger is called a vaporizer if the stream is essentially completely
vaporised, and when the process stream is completely condensed; a reboiler if associated
with a distillation column; and an evaporator if used to concentrate a solution. The term
fired exchanger is used for exchangers heated by combustion gases, such as boilers; other
exchangers are referred to as unfired exchangers.
There are two primary classifications of heat exchangers according to their flow
arrangement. In parallel-flow heat exchangers, the two fluids enter the exchanger at the
same end, and travel in parallel to one another to the other side. In counter-flow heat
exchangers the fluids enter the exchanger from opposite ends. The counter current
design is most efficient, in that it can transfer the most heat from the heat (transfer)
medium.See countercurrent exchange. In a cross-flow heat exchanger, the fluids travel
roughly perpendicular to one another through the exchanger.

PRINCIPLES OF HEAT EXCHANGERS:

Simplified heat exchanger concepts heat exchangers work because heat naturally
flows from higher temperature to lower temperatures. Therefore if a hot fluid and a cold
fluid are separated by a heat conducting surface heat can be transferred from the hot
fluid to the cold fluid.
The rate of heat flow at any point (kW/m2 of transfer surface) depends on:
Heat transfer coefficient (U), itself a function of the properties of the fluids involved,
fluid velocity, materials of construction, geometry and cleanliness of the exchanger
Temperature difference between hot and cold streams
Total heat transferred (Q) depends on:

Heat transfer surface area (A)

Heat transfer coefficient

Average temperature difference between the streams, strictly the log mean (DTLM)

Thus total heat transferred Q = UADTLM

But the larger the area the greater the cost of the exchanger

Therefore there is a trade-off between the amount of heat transferred and the exchanger
cost.
3.2 PRE-HEATER
Due to the combustion of coal in the furnace fuel gasses evolve form the coal. The
fuel gasses at a temperature are sucked from the top and leaves through the bottom. Any
heavy particles that are smoke or fuel fall down and are collected in the plastic bags. The
pre-heater have metallic pipes as in a heat exchanger the boiler feed water circulates
around the tubes and gets heated up. The fuel gases through tubes and for cyclone
separator and large steam systems, or in any process requiring high temperatures, the
input fluid is usually preheated in stages, instead of trying to heat it in one step from
ambient to the final temperature. Preheating in stages increases efficiency and minimizes
thermal shock stress to components, as compared to injecting ambient temperature liquid
into a boiler or other device that operates at high temperatures.
In the case of a steam system, a portion of the process steam is tapped off and
used as a heat source to reheat the feed water in preheated stages. Figure 8 is an
example of the construction and internals of a U-tube feed water heat exchanger found in
a large power generation facility in a preheated stage. As the steam enters the heat
exchanger and flows over and around the tubes, it transfers its thermal energy and is
condensed. Note that the steam enters from the top into the shell side of the heat
exchanger, where it not only transfers sensible heat (temperature change) but also gives
up its latent heat of vaporization (condenses steam into water). The condensed steam
then exits as a liquid at the bottom of the heat exchanger. The feed water enters the heat

exchanger on the bottom right end and flows into the tubes. Note that most of these
tubes will be below the fluid level on the shell side.
This means the feed water is exposed to the condensed steam first and then
travels through the tubes and back around to the top right end of the heat exchanger.
After making the 180 bend, the partially heated feed water is then subjected to the hotter
steam entering the shell side.
The feed water is further heated by the hot steam and then exits the heat
exchanger. In this type of heat exchanger, the shell side fluid level is very important in
determining the efficiency of the heat exchanger, as the shell side fluid level determines
the number of tubes exposed to the hot steam.

3.3 PUMPS
For the pumping of liquids or gases from one vessel to another or through long
pipes, some form of mechanical pump is usually employed. The energy required by the
pump will depend on the height through which the fluid is raised, the pressure required at
delivery point, the length and diameter of the pipe, the rate of flow, together with the
physical properties of the fluid, particularly its viscosity and density. The fluid may be a gas
or liquid of low viscosity, or it may be a highly viscous liquid, possibly with non-Newtonian
characteristics. It may be clean, or it may contain suspended particles and be very
corrosive. All these factors influence the choice of pump. Because of the wide variety of
requirements, many different types are in use including centrifugal, piston, gear, screw,
and peristaltic pumps; though in the chemical and petroleum industries the centrifugal
type is by far the most important. In general, pumps used for circulating gases work at
higher speeds than those used for liquids, and lighter valves are used. Moreover, the
clearances between moving parts are smaller on gas pumps because of the much lower
viscosity of gases, giving rise to an increased tendency for leakage to occur.

3.4 COOLING TOWERS

A cooling tower is a device designed to reject heat absorbed through a cooling
system to the atmosphere. A cooling tower is a series of systems that are use to cool large
structure or process. This cooling system utilizes a series of baffles inside a tower in order
to permit a heat transfer between the atmospheric air and the water been cooled. A draft
inducted system is one common configuration for rapid cooling effects using an air fan as
the driving mechanism. The cooling tower experimental activity consisted in obtaining
different parameters for the analysis of the systems performance. Such parameters as
the speed of the fans and voltage were used to determine the power require for them.
Apart from the fans, the temperatures of the water and air entering and exciting were
used to calculate the thermodynamic balance in order to obtain the effectiveness of the
system.
Water cooling in towers operates on the evaporative principles, which are a
combination of several heat and mass transfer processes. The most important of these is
the transfer of liquid into a vapour air mixture, as, for example, the surface area of a
droplet of water. Convective transfer occurs as a result of the difference in temperature
between the water and the surrounding air. Both these processes take place at the
interface of the water surface and the air. Thus it is considered to behave as a film of
saturated air at the same temperature as the bulk of the water droplet.
Finally, there is the transfer of sensible heat from the bulk of the water to the surface
area. Thus the two main processes are evaporation of water and convective cooling. The
first is based on the difference in partial vapor pressure and the second upon the
temperature difference.

4.ACTIVE PHARMACEUTICAL INGREDIENT -API

An active ingredient (AI) is the substance in a pharmaceutical drug or a pesticide that
is biologically active. The similar terms active pharmaceutical ingredient (API) and bulk
active are also used in medicine, and the term active substance may be used for pesticide
formulations. Some medications and pesticide products may contain more than one
active ingredient. The traditional word for the API is pharmacon or pharmakon (from
Greek:), adapted from pharmacos) which originally denoted a magical substance or drug.
A dosage form : the API, which is the drug itself; and an excipient, which is the substance
of the tablet, or the liquid the API is suspended in, or other material that is
pharmaceutically inert. Drugs are chosen primarily for their active ingredients.
Because homeopathic products no longer have any biologically active ingredients, their
list of ingredients refers to the original ingredients used in their preparation and the
finished product no longer contains any active ingredients.
Active Pharmaceutical Ingredients are made in several locations around the world. In
the United Kingdom there is a significant number of members of the Northeast of
England Process Industry Cluster (NEPIC) that manufacture, formulate and package API's
for consumer use. Aesica Pharmaceuticals, Shasun Pharmaceuticals, Piramal
Enterprises are based in Northumberland and Epax Pharmaceuticals on Teesside are
companies that perform primary manufacture of active pharmaceutical ingredients(APIs)
to cGMP standards. While Aesica, Piramal, MSD(Northumberland),Sanofi(Tyne & Wear)
and GlaxoSmithKline (County Durham) are all secondary pharmaceutical manufacturers
who formulate and package API's for consumer use
.

5.BATCH PROCESS CONTROL RECORD

A BPCR is nothing but the sequential flow of the Process or the Operation which is
prescribed for the safe operation in the Pharmaceutical Industry.In this record the
prescribed amount materials or the raw materials are being mentioned for the production
of the API.
At Aurobindo BPCR are being followed convientionally which is prescribed by the R&D
Department.
General BPCR includes
1.Procurement of Raw Materials from the Warehouse Department.

2.Transporting of Raw Materials from the Warehouse Section to the

Production Block.

3.At the Production Block the prescribed Temperature and the Operating Pressure
are beingmaintained so as to obtain the required product.
4.The obtained product is furthur being processed into various stages like
Blending,Shiftingetc depending upon the type of product.
5.Finally,the obtained product is being Packed and Dispatched.
In the Production Process various Solvents are being used and these solvents are to
recovered so as to avoid wastage which would be loss to the company.So the Spent
solvents are being treated at the Solvent Recovery Plant(SRP) where solvents are being
treated and recovered with high purity.
In the due process of production some of the solid effluent are being generated and
these are sent to Effluent Treatment plant where the effluents are treated and are being
disposed which are not harmful to environment(less toxicity).

SOLVENT
RECOVERY
PLANT( FOR
THE
RECYCLING OF
SOLVENTS )

RAW MATERIALS
FROM
WAREHOUSE

PRODUCTION
BLOCK

EFFLUENT
TREATMENT
PLANT

BLENDING

SHIFTING

PACKING/DISPATC
HING

5.1 GENERAL PRODUCTION BLOCK OVERVIEW

REACTION
REACTOR

EXTRACTION
REACTOR

CARBON
TREATMENT
REACTOR

FILTERATION(S
PARKLER
FILTER)

DISTILLATION(
FOR
PRECIPITATION
OF PRODUCT)

CENTRIFUGAL
SEPERATION

DRYER(MOSTL
Y VACCUM
AND TRAY
DRYER)

SHIFTING AND
BLENDING

For an API likeAurobindo,Production Blocks are the heart as they produce the required
products like Gabapentin,Cephroxamineetc.So the Production Block procedure is being
described in the following steps: In the first reactor ,Raw materials from the warehouse and with the help of suitable
solvents are being fed into the reactor where the reaction between them takes
place.
In the second Reactor ,Extraction takes place where the solvents are being
extracted with the help of another suitable solvent. For example to remove ethyl
acetate from the reaction mixture water is being used so as to extract ethyl acetate
effectively. Here mainly the extraction is done through propellers and is being left
out for 15 minutes so as to settle the layers.
In the next step the reaction mixture is being treated with the Carbon (Activated
Carbon Treatment) so as to remove the the colour content that has been formed
in the reaction mixture while in the process of the Extraction.
In the fourth Reactor the filteration process is being carried and majorily the
Aurobindo unit handles Sparkler Filter where the suspended particles are being
removed.
The Distillation Process is being carried out where the separation is being done
basing upon the volataility of the components.Aurobindo unit utilizes Vaccum
Distillation.
After Distillation,the separated residue is being sent to the Centrifugal Seperator
where the moisture content is being removed.
In the Seventh stage of the process the product from the Centrifugal separator is
now being loaded in to the Vaccum Dryer where the final moisture content in the
product is being removed.This process of drying is being done nearly for 22-24
hours for effective and good quality of the product.
After drying the product, foreveness among the particles of the product, blending
and shifting operation is being done where the product is being charged in to the
Tumbler which is being rotated at certain speed.
Finally the batch is being packed and then the lot is being sent to the QC
Department for checking the Quality and then to the QA Department for Assuring
the lot or the batch which is produced is according to the BPCR.
After producing the batch,all the reactors are being washed so as to use these
reactors for the next sort of product preparation.Here mainly with the help of
water and other solvents,the reactor vessels are being cleaned and the solvents
and the water are being sent to the Effluent Treatment Plant and to the Solvent
Recovery Plant(as followed in Aurobindo Unit).

The fraction collection is being carried and the unconverted vapors are pumped back to the
column by Reflux Line.
At the Reboiler the desired product is being seperated(IPA).The formed IPA is being cooled
and is collected in the reciever .
The unconverted IPA is being pumped back to the kettle so as to repeat the
process.Industrially(At Aurobindo) this process is being carried out for an operating time of
24hrs with

Feeding-1/2 hrs

Heating-1/2 hr

Reflux-2hrs

Fraction-1hrs

Collection-19hrs

Cooling and Cleaning-1hrs

6.DESIGNING OF DISTILLATION COLUMN FOR IPA WATER SYSTEM

6.1 CALCULATION OF NUMBER OF STAGES

Basis-1000kg/hr of feed mixture pumped in to the column.
Analysis Composition
IPA-96%
Water-4%

Final Composition
IPA-99.5%
Water-0.5%

(in weight percentage)

Now to initiate the design procedure, the material balance is important one. So on applying
Material balance to the current system we get
Water-1000*0.04=40Kg

IPA-1000*0.96=960kg
FEED

AMOUNT

MOLECULAR WEIGHT

BOILING POINT

WATER

40 Kg

18

100

IPA

960 Kg

60

82.6

Now mole fraction of Feed(Xf),mole fraction of Distillate(Xd),mole fraction of Residue(Xw).

Xf=(96/60)/[(96/60)+(4/18)]=0.87
Xd=(99.5/60)/[(99.5/60)+(0.5/18)]=0.98
Xw=(0.5/60)/[(0.5/60)+(99.5/18)]=0.0015
From Component Balance we have
Fxf=Dxd+Wxw and F=D+W W=F-D
1000(0.87)=0.98D+0.0015W
D=887.5Kg/hr
W=112.4Kg/hr

Sample calculations for T-xy data:

Antoine equation:

P=vapour pressure in mmHg

A,B,C are constants
T in degree Celsius

IPA constants

WATER constants

A=20.4463

A=18.5882

B=4628.95

B=3984.92

C=252.64

C=233.43

Total pressure=1atm=760mmHg
At T=82^c

A=Isopropanol, B=Water

lnPa^v=20.4463-[4628.95/(252.64+82)]

lnPb^v=18.5882-[3984.92/(233.43+82)]

lnPa^v=6.6136

lnPb^v=5.954

Pa^v=744.649 mm Hg

Pb^v=385.402mm Hg
P=x *Pa^v+(1-x)*Pb^v
Y=(x*Pa^v)/p

X=1.04
Y=1.01

Developing T-x-y Data for IPA-Water System :

TEMPERATURE(

100

98

0.073

0.135

96

0.157

0.268

94

0.25

0.395

92

0.319

0.466

90

0.464

0.627

88

0.588

0.736

86

0.725

0.836

84

0.876

0.931

83

0.9558

0.97668

82

1.04

1.01

The Typical plot of IPA-Water will be

By plotting the above data ,now we have

For finding min reflux ratio:From graph

Xd/(Rmin+1) =0.545

Here lets take feed enters at the saturation level. So the q line drawn from Xf will be parallel
to y-axis.
Rmin=0.79816
Now,R=1.5*Rmin R=1.5*0.79816
R=1.19724

On plotting the operating lines for stripping and rectifying section, the number stages
obtained are17stages.
Let the tray efficiency be50%
So, the required number of Actual Stages will be Number of Ideal stages/stage efficiency
= (17-1)/0.5
= 32stages
Height of the Column = (n-1+2)*p

where

n= Number of Actual Stages

p=Plate Spacing
Height of the Column=(32-1+2)*0.45 = 14.85m
HETP= (column height) / (No of theoretical plates within the column)
=14.85/32
`

=0.464m
6.2 TOWER SPECIFICATIONS
Height of the Column=14.85m
Tray Spacing=0.45m
Tower diameter=500mm=0.5m
Type of packing=structured packing, Mellapak plus 752.Y
No of segments in the column=3, each segment having 4.95m
Total Packingheight=3*4=12m

Number of theoretical stages( graphically)=16 stages(excluding reboiler)

Number of Actual stages(by considering 50% Tray Efficiency)= 32stages.

6.3 REBOILER AND CONDENSER CALCULATIONS

96% IPA

4% WATER

IPA density: 0.786g/cc

water density=1000kg/m3

Specific heat=0.62 Kcal 0c

Specific heat 4.187kJ/kgK

Latent heat: 159kcal/kg

Vaparization rate:

Latent heat: 539.92 kcal /kg

V=2000Kg/Hr

Condenser calculation:
Condensing load Qc=V+VCp(Tb-Ta)+VCp(Ta-Tc)
Tb=boiling temp, Tc=Actual temp, Tc=condensing temp
Qc=2000(159)+2000*0.62(81-79)+2000*0.62(79-60)
=318000+2480+23560
Qc =344,040 kcal/hr
810c
320c

Qc=UA Tm

Tm= (T - T)/ ln (T/T)

= 49-32/ln(49/32)
=39.80c
U=150w/m^2 K
Area of condenser:

A= Q /U Tm
=344,040/150*39.8

600c
280c

=57.6m^2

Reboiler calculation :
1280c

Steam applying at 3 kg/cm2,

810c

At 3 kg/cm2 steam temperature: 127

U=600w/m^2k
Q=UA Tm

Tm= (T - T)/ ln (T/T)

= 47-63/ln(47/63)
=54.60c
Area of reboiler: A= Q /U Tm
=344040/(600*54.6)
=10.5m^2
Steam Calculations:
Steam consumption:
Q=mcpdt+m
m=3440404/(1*35)+510
m=631 Kg/hr

Domestic coal calorific value=3800kcal/kg

540 kcal coal produce 1kg steam
1kg coal produce 7.03kgs steam
Steam consumption=631kg/hr

Cp=1, =510 KCal/Kg

930c
300c

For 1 hour 631kgs of steam producing 89.7kgs of coal required

Cooling tower capacity

= Q / 3024
= 3440404/3024
=113.76 TR

1TR=3024Kcal.
7.ALTERNATIVE SOLVENT RECOVERY METHODOLOGY FOR IPA-WATER SYSTEM
7.1 BATCH DISTILLATION PROCESSES.
At atmospheric condition, a binary mixture of IPA and water forms a homogeneous
minimum-boiling azeotrope at 87.487.7 mass% (68.167.5 mole%) and 80.380.4C.
Therefore, conventional distillation of a binary mixture Water IPA will distillate the binary
azeotrope.
There are two kinds of approaches to obtain a nearly pure IPA using advanced
continuous distillation processes. One is to utilize an azeotropic distillation process using
benzene or cyclohexane as an entrainer and the other is an extractive distillation process
using ethylene glycol as a solvent.
In azeotropic distillation, by forming a ternary heterogeneous azeotrope
lower than any other binary azeotropic temperatures, a nearly pure IPA can be obtained
as a bottom product of the azeotropic distillation column. In extractive distillation, by
adding a solvent exclusively familiar with water like ethylene glycol, IPA can be obtained
as a top product of the extractive distillation column.
In this study the recovery of IPA from an industrial waste stream (IPA/water mixture) was
studied by heterogeneous azeotropic batch distillation with cyclohexane. This technique is
compared with conventional distillation and salting out methods.
7.2 EXPERIMENTAL METHOD
An An industrial IPA/Water mixture with an IPA content > 97 mass% was used. The IPA
was previously dewatered by sodium hydroxide. The goal is to purify it with less than 0.1%
water. Cyclohexane with a purity 99% was used.
The water content of the samples was measured with an automatic Karl Fisher titration.
The cyclohexane and IPA content were measured by gas chromatography using pentane
as an internal standard.
CONVENTIONAL DISTILLATION

780 g of an IPA/water mixture, which contained 2.00 mass% water was distilled with the
conventional distillation column. The reflux ratio was until steady state conditions were
reached at the top of the column (boiling temperature of binary IPA/water azeotrope).
The IPA/water azeotrope was distilled with a reflux ratio of 30:2.
SALTED-OUT DISTILLATION
In a second experiment MgSO4 was added as a drying agent to a known amount of
IPA/Water mixture (2.47 mass% water). This mixture was mixed during 0.5h. A small
amount of the salt dissolved in the mixture. The mixture was distilled with the
conventional distillation method,with a reflux ration of 20:2, when equilibrium conditions
were reached. In a third experiment the added MgSO4 was filtered off prior to distillation.
The water content of the initial IPA/water mixture was 1.75 mass%.
HETEROAZEOTROPIC DISTILLATION
50L of an IPA/water mixture, which contained 0.83 mass% water and 2.5L of cyclohexane
were added to the reboiler. This cyclohexane amount is slightly larger than the total
holdup of the column (2250 mL). Preliminary test showed that this was the optimal
entrainer volume. The vapor flow rate was set at 0.23 kmol/h.
The reflux ratio was until steady state conditions were reached at the top of the column
where the recorded temperature was that of the boiling ternary IPA/water/cyclohexane
azeotrope. Then the reflux ratio of the column was set at 30:1. In a second step, the
ternaryIPA/water/cyclohexane heteroazeotrope was collected, cooled with ice and
transferred to aseperatory funnel. The water phase was collected and the organic phase
was completelyrefluxed at the top of the column. This was continued until separation of
the two phasebecame difficult because of the water removal. Then homogeneous
distillation proceeded.

8.USES OF ISO PROPYL ALCOHOL

Iso propyl alcohol can be used as an industrial cleaner for machinery and plants. It is used
in the manufacture imaging photo developers. Largest use of IPA is as solvent, and
usually as a cleaner. It is used in electroplating-cold-cleaning solvents and heat
transferring agents secondary coolants. Used as printing solvents for flexography and also
for gravure printing, lithography.
It is found in many everyday products such as paint thinner, inks, general purpose
cleaners, disinfectants and windshield thawing agents. 99% of IPA is used to clean
surfaces and to prevent infection from minor surface wounds like scrapes and cuts.
IPA frequently used is tattoo shops to clean bacteria off of the skin before a tattoo
or piercing. IPA 99% is used in heavily in the nail industry. The chemical is great for
cleaning the surface of clients nails and producing maximum nails shine.

9.SAFETY ASPECTS
INTRODUCTION
Technical advancement and the risk factor both move almost in the same proportion.The
risk factor if not eliminated, can be controlled to a great extent and can be kept in the
safety zone if we adhere to the certain safety measures.Right from the time the raw
materials enters the factory, it involves unloading, storage, transporting and the
participates in the reaction. Different types of hazards are hidden at different operation, if
in general instructions of safety are followed strictly we can achieve accident free work
environment which is the preamble of safety policy.
Some of the safety measures which we should strictly follow
While charging the reactants through the manhole one should always wear
goggles, face shield to avoid any splashing in the eyes.
After charging the materials are must to taken to be to see that all the bolts of
manhole are tightened fully to avoid any flying of the manhole cover in the case of
some pressure which might built in the reactor.
Most of the values used in the industry are ball valves, so care is to be taken to see
that all these are closed slowly. Abrupt closing of these values causing the danger
of line getting damaged or burst at any point due to liquid hammer which may go
up to abnormally high pressure.
Abrupt heating and closing of the glass-lined reactor should always be avoid
otherwise it may get a crack in lining due to thermal shock.
Whenever temperature scans are fixed and maintain, temperature in the reactor is
important, it should checked locally by mercury thermometer.
While discharging solvent in drums check that earthen wire is connected properly.
Activated carbon or any other fine dust material should not be charged free
through the man hole to avoid the dust explosion. It should always be kept wet
with water or with media in which the carbon treatment is given and charged.
Mostly heating is done by steam and the auto ignition temperature is quite high

for almost all the solvents but whenever the other source of heating is utilized.

10.CONCLUSION
The recovery of solvent Iso propyl alcohol is recovered from Iso propyl alcohol-water
mixture. Solvent is recovered by distillation and also taking care and precaution and also
safety devices are used while product manufacturing in plant.
The waste effluent which is coming out from the industry is also well treated and
disposed effectively and gases coming out from the condensate is also treates well and
converted into byproduct.
The above project is also feasible when compared to the Economics involved in it and by
using Heteroazeotropic Distillation Process maximum separation could be done by using
Cyclohexane as an entrainner.
But, since the process is being developed in laboratory scale, the scope for future study
has more priority in this Solvent Recovery Field.

11. REFERENCES
Coulson & Richardson's CHEMICAL ENGINEERING volume 1, Sixth edition- Fluid
Flow,Heat Transfer and Mass Transfer
Chemical Engineering, Volume 6, Third edition Chemical Engineering Design R.
K.Sinnott
Mass transfer operations by Robert e treybal MGH publications.
Principles of Mass Transfer and Separation Processes BY Binay K.Dutta.
www.sulzer structured packing.com
Chemical process calculationsby KA Ghavane, Nirali publications.