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Evaporation

(Dr.) Mirza Salman Baig


Assistant Professor (Pharmaceutics)
AIKTC, School of Pharmacy,New Panvel
Affiliated to University of Mumbai (INDIA)

CONTENT
EVAPORATION

Defination
Mechanism
Factors affecting Evaporation
EVAPORATION UNDER REDUCED
PRESSURE
EQUIPMENT USED FOR EVAPORATION
APPLICATION OF EVAPORATION
REFERENCES

EVAPORATION
Defination:Theoretically,
Evaporation means simply
formation of vapors from the surface
of a liquid,below its boiling point.
Thus, no boiling occurs and the rate
of vaporization depends on the
diffusion of vapour through the
boundary layers above the liquid.

Thus a practical definition of evaporation


is The removal of solvent from a solution
by boiling the liquor (solution) in a suitable
vessel and withdrawing the vapour,
leaving a concentrated liquid residue.
This means that heat will be necessary to
provide the latent heat of vaporization
and, in general the rate of evaporation is
controlled by the rate of heat transfer.
Evaporators are designed, therefore, to
give maximum heat transfer to the
liquid, with the largest possible area, a
suitable temperature gradient.

Mechanism
When heat applied to the solution,
motion of molecules increase and
molecules present in the surface
overcome the surface tension and
get escape from the surface.

Factors affecting Evaporation


1.
2.
3.
4.
5.

Temperature
Surface area
Agitation
Vapour pressure
Atmospheric pressure on the liquid
under evaporation
6. Type of product required
7. Economic factors

M=KS/p (b-b')
M= mass of vapour
S= surfacee area of liquid
p= atmospheric pressure
b= max vap. pressure
b'= pressure due to vapour in air
K= constant

1) Temperature: The rate of evaporation is


directly proportional to the temperature.
2) Surface area: The rate of evaporation is
directly proportional to the surface area of
the vessel exposed to evaporation.
3) Agitation: is necessary for evaporation.
4) Atmospheric aqueous vapour
pressure: The rate of evaporation is
inversely proportional to the atmospheric
aqueous vapour pressure.

5) Atmospheric pressure on the liquid


under evaporation: The rate of
evaporation is inversely proportional to the
atmospheric pressure on the liquid under
evaporation.
6) Vapour pressure: evaporation is paster in
dry air as b' is less
7) Type of product required: The selection
of the method and apparatus to be used for
evaporation depends upon type of product
required.
8) Economic factors: When selecting the
method and apparatus the economic factors
are important

EVAPORATION UNDER REDUCED


PRESSURE
At reduced pressure evaporation increases.
Advantage:
1. Evaporation occurs at low temperature,
with less risk of damage to heat sensitive
materials.
2. A lower operating temperature gives
higher temperature gradients, without
the need of excessive steam pressures.
3. The lower the operating temperature,
lower the steam pressure that can be
used.

EQUIPMENTS USED FOR


EVAPORATION
Types of Evaporator:
Evaporators are divided mainly into three groups.
1. Natural circulation evaporator
Types:
i) Evaporating pans (Open)
ii) Evaporating stills (Close)
iii) Short tube evaporator.
a) Vertical tube
b) Horizantal Tube

Contd...
2) Forced circulation evaporator
3) Film evaporator
Types:
i) Wiped Film evaporator
ii)Long Tube Evaporator
a) Climbing film evaporator
b) Falling film evaporator

1) NATURAL CIRCULATION
EVAPORATORS
Working principle:
The movement of the liquid results
from convection currents set up by
the heating process.
Convection currents: The process
in which heat moves through a gas
or liquid as the hotter parts rises and
the cooler part sinks. VID

(Open) Pan Evaporator


On a manufacturing scale, liquid extracts containing
water are evaporated in open pans called evaporating
pans.
Construction:
The evaporating pan consists of
Hemispherical shallow made of
Copper
Stainless steel
Alluminium
Enameled iron
Steam jacket

The hemispherical shape gives the best


surface\volume ratio for heating and the largest area
for the disengagement of vapour.

Working:
The dilute solution is taken
in the pan. Steam is
introduced through the
steam inlet into the jacket
to heat the pan.
In these evaporators the
movement of the liquid
results from convection
currents set up by the
heating process.
The concentrated liquid is
collected through the outlet
placed at the bottom of the
pan.

Advantages
1) They are simple, easy and cheap to
construct.
2) They are easy to use and clean.
3) Stirring of the evaporating liquids
can be done easily.

Disadvantage
1) The whole of the liquid is heated all the time
which may lead to decomposition of the
components.
2) On the evaporating surface foam is rapidly
formed which decreases evaporation.
3) Solids may be deposited at the bottom which
make the stirring necessary.
4) This pan can only be used for evaporating
aqueous and thermostable liquid extracts.
5) They can not be used for evaporating extracts
containing organic solvents like alcohol etc.

ii) (Close) Pan Evaporator


Construction
It consists of a jacketed-evaporating
pan with a cylindrical coverthat
connects it to a condenser.
The over all assembly is calledstill.
The cover is clamped with the
evaporating pan.

Working :
The dilute liquid is fed
into the still, the cover
is clamped.
Steam is introduced
into the jacket.
The liquid is
evaporated and
condensed in the
condenser and
collected.
The product (i.e.
concentrated liquid) is
collected through the
product outlet.

Contd...
Advantages:
Easy to clean and maintain.
Allow the equipment to be used for
slovents other than water E.g. ethanol.
Disadvantages:
All the liquor is heated all the time.
The heating surface is limited.

iii) Short tube evaporator


Construction:
The evaporator is a cylindrical vessel. The lower
portion of the vessel consists of a nest of tubes with
the liquor inside and steam outside this
assembly is calledcalendria.
The specifications of calendria are as follows:

Tube length: 1 2 m
Tube diameter: 40 80 mm
Diameter of evaporator: 2.5 m
Number of tubes:1000

The feed inlet is at the top of the calendra.


The product outlet is placed at the bottom of the
evaporator. Steam inlet and outlet is placed from
the side of the calendria.

Vertical Tube (Short Tube)


Working:
Steam Passes through
jacket.
The liquor in the Vertical
tubes is heated by the
steam and begins to boil.
When the mixture of
liquid and vapor shoot up
the tubes (Like the, liquid
that is allowed to boil to
vigorously in a test-tube).
The product is collected
through the product
outlet.

Multiple effect evaporator

Working
Steam enters calendria of evaporator-1 and air is
replaced by steam, after transfering heat to feed
inside evaporator-1 it get condensed, and
condensate released through C1.
Remaining steam from calendria of Evaporator -1
passes through Vent (V-1) and enters steam inlet
S-2 of evaporator-2.
Processes continues until steam reaches
evaporator 3.
Feed in Evap. 2&3 is not heated by steam rather it
is heated by vapours comming out of seperator
from evap 1&2 respectively.

Horizantal Tube (Short Tube)


Steam Passes
through horizantal
tubes.
Solvent escape
from the top of
evaporator.
Concentrated
liquor collected
from bottom.

Advantages
1.Use of tubular calendria increases the heating
area.
2.
Increasing the rate of heat transfer.
3.Condenser and receiver can be attached to run
the evaporation under vacuum with nonaqueous
solvents.
Disadvantages
1. Since the evaporator is filled to a point above
the level of the calendria, a considerable amount of
liquid is heated for a long time. (The effect of
this continual heating can be reduced to some
extent by removing concentrated liquor slowly from
the outlet at the bottom of the vessel)
2.Complicated design, difficult for cleaning and
maintenance.

2) Forced circulation
evaporators

Construction:
The evaporator consists of a short tube calendria 2.5
meter and a large cylindrical vessel (body of the
evaporator) for separation of vapor and liquid takes
place.
The liquor inlet is provided at the side of the
cylindrical vessel.
A pump is fitted in between the calendria and
the body of the evaporator.
A tangential inlet for liquid under high pressure is
placed at neck of the body of the evaporator.
The vapor outlet is placed at the top of the
evaporator body, it may be passed through a
condenser to collect the condensed liquid.

Working principle:
Feed is introduced
through the liquor inlet.
Pump will force the
liquid through the
calendria.
Steam heats the liquid
inside the calendria.
As it is under
pressure in the
tubes the boiling
point is elevated and
no boiling takes place.

Contd...
As the liquor leaves the tubes and
enters the body of the evaporator
through the tangential inlet there is a
drop in pressure and vapor flashes
off from the superheated liquor.
The concentrated liquid is pumped
out through the product outlet and
the vapor is collected through the
vapor outlet.

Advantages
1) It is useful for rapid liquid movement
improves heat transfer, especially for
viscous liquids or materials that deposit
solids or foam readily.
2) The equipment is suitable for operation
under reduced pressure
3) These evaporators possess rapid
evaporation rate.

4) These evaporators are mainly used


for thermolabile materials.
5) These can also be used in practice
for the concentration of insulin
and liver extracts.
Disadvantage:
Corrosion-erosion can occur, due to
high circulation velocities.
Salt deposits detach and
accumulate at the bottom.

3) FILM EVAPORATORS
Film evaporators spread the
material as a film over the heated
surface, and the vapor escapes the
film.
Following are the types of film
evaporators
(Long Tube Evaporator)
a) Climbing film evaporator
b) Falling film evaporator

i) Long tube evaporators


(Climbing film evaporators)
Construction:
The heating unit consists of steamjacketed tubes, having a length to
diameter ratio of about 140 to 1, so
that a large evaporator may have
tubes 50 mm in diameter and about
7 m in length.

The liquor to be
evaporated is
introduced into
the bottom of the
tube
The film of liquid
forms on the walls
and rises up the
tubes, hence it is
calledclimbing
film evaporator

Working
At the upper end, the mixture of vapor and
concentrated liquor enters a separator, the
vapor passes to a condenser, and the
concentrated liquid to a receiver.
Cold or pre heated liquor is introduced into
the tube.
As more vapor is formed, the slug of liquid
is blown up the tube, the tube is filled with
vapor, while the liquid continues to
vaporize rapidly, the vapor escaping up
the tube
Because of friction between the vapor and
liquid, the film also is dragged up the
tube upto a distance of 5 to 6 metres.

ii) Long tube evaporators


(Falling film evaporators)
Construction:
The heating unit consists of steamjacketed tubes, having a length to
diameter ratio of about 140 to 1, so
that a large evaporator may have
tubes 50 mm in diameter and about
7 m in length.
Vid

Working principle
The liquor to be
evaporated is
introduced at the top
of the evaporator
tubes and the liquor
comes down due to
gravity.
The concentrate and
vapor leaves the
bottom.
They are separated in
a chamber where the
concentrate is taken
out through product
outlet and vapor from
vapor outlet.

Advantages:
Because of obtaining good heat
transfer the method being
especially useful with liquids that are
too viscous.
Disadvantages:
A major disadvantageof fallingfilm
evaporatorsis the potential
instability of the falling film
Expense to manufacture and install
the instrument is high.
Difficult to clean and maintain.

4) Wiped film evaporator


Construction:
The wiped film evaporator or rotary film
evaporator, contains of a single, short tube of
wide diameter or a narrow cylindrical
vessel,1 or 2 meters in length.
A section across the evaporator is
surrounded by a heated jacked.
Through the vessel is a bladed rotor, with a
clearance of the order of 1mm between the
tips of the rotor blades and the wall of the
vessel.

Working:

The liquor is introduced at the top


of the vessel and spread as a film
over the heated wall by the
action of the rotor.
Evaporation occurs as the liquor
passes down the wall, vapour is
taken to a condenser and the
concentrated liquor withdrawn at
the bottom of the vessel.
The evaporator is therefore a
form of single tube,
It is like falling film evaporator in
which the film is formed and
agitated mechanically.......Vid

Centrifugal rotary evaporator


Centrifugal
concentrators induce
solvent boiling under
vacuum
Samples are cold but,
but not frozen.
Rotary evaporation
explained

Contd...
Advantage
Centrifugation ensures that solvent
boils from the sample surface
Thereby minimising boiling over and
solvent bumping(rapid boiling will
expel the liquid from the container)
Hence, preventing sample loss &
Cross-contamination

Contd...
The vortex created
generates a large
sample surface area
for evaporation,
making the process
relatively fast
Vid

Factors Affecting the Speed of


Evaporation
Heat supply
Vapour removal and
Solvent surface area available for
evaporation

Evaporator Accessories
Condensers,
expansion and bucket traps,
entrainment separators, Vacuum pump

Condensor
If evaporater is used with vacuum then
condensor is used with it.
Surface Condensor
In surcface condensor, liquid to be condensed
and cooling liquid is seperated by thin metal
wall.

Contact Condensor
In this type Vapour and cooling liquid are
mixed directly.
Parallel/ Counter current
Wet/Dry condensor
Barometric/ Low Level

Surface Condensor
It is like tubular heater (exchanger)
Vapours outside tube and water inside the
tube.
"Heat transfer coefficient" or "Capicity to
cool" can be increase by increasing water
(cold) velocity (by making it multipass)
Vapour pressure is lower than atmospheric
pressure hence vacuum pump needed to
remove air.
It is used when vapours are other than
water vapour.

Surface Condensor

Contact condensor
If vapour to be condensed is water
then contact type condensor is
always used.
There is direct contact between
vapours and cooling liquid.

Parallel current wet contact


Wet contact
because outlet for
un-condensed
vapour and water
is same
Parallel current
because direction
of flow of water
and vapour is same.

Counter current dry contact


Dry contact
because outlet for
un-condensed
vapour and hot
liquid is different.
Counter current
because direction
of flow of cold
water and hot
vapour (Air) is
different.

Steam Traps
Condensate can be removed by
using pump/ trap
Steam trap is a device who's function
is to allow condensate to drain but to
prevent steam from blowing out of
the space drained.
Types
Expansion trap
Bucket trap
Tilt trap

Expansion Trap

A-Cartrige
B-corrugated tube
C-valve

Contd...
Space between cartrige and
corrugated tube is filled with oil
When cool condensate enter valve it
get drain out.
when steam enters valve, heat of
steam causes cartige to expand and
valve get closed.

Bucket Trap

Contd...
The inverted bucket steam trap consists of a
chamber containing an inverted bucket which
actuates a discharge valve through a linkage.
The valve is open when the bucket rests (at
the bottom) of the trap. This allows air to escape.
When condensate start accumulating bottom
inside, outside and above the inverted bucket,
then the bucket get sealed from its bottom side
by rising condensate.
The valve remains open as long as condensate
is flowing, and trapped air bleeds out through a
small vent in the top of the bucket.

Contd..
When steam enters the trap, it fills the
bucket, causing the bucket to float so it rises
and closes the valve.
The steam radiate heat and get condenses, thus
allowing the bucket to sink and reopen the valve
for condensate to flow.
Small amounts of non-condensible gases (or
air) that enter the trap during normal operation
are also vented through the small opening in the
top of the bucket. Vid

Entrainment seperator
Principle If liquid
droplet can be
made to impinge
on solid surface
they coalesce into
a sheet, and not
readily picked even
by high vapour
velocities.
Vid

Vacuum pump
(steam-jet ejector)
The pump use
to remove hot
water and non
condensed gas
with the help of
parallel
current wet
condensor.

Components
Motive Chest
Nozzel (converging-diverging)
Suction Chember
Diffuser

Vacuum pump

Contd...

It consists of a motive fluid inlet nozzle


and a converging-diverging outlet nozzle.
Water, air, steam, or any other fluid at
high pressure provides the motive force at
the inlet.
The Venturi effect is principle behind its
working.
Fluid under high pressure is converted into
a high-velocity jet at the throat of the
convergent-divergent nozzle which creates
a low pressure at that point.

Contd...
The low pressure draws the suction
fluid into the convergent-divergent
nozzle where it mixes with the
motive fluid. Vid
Steam get condence by water jet at
bottom B.
Air passes to second nozzel C

APPLICATION OF EVAPORATION
Evaporation is one of the most
important processes in the
manufacture of pharmaceuticals.
It is used in the preparation of
Liquid extracts, soft extracts & dry
extracts.
In the concentration of blood
plasma & serum.
It is also used in the manufacture of
drugs containing, antibiotics,
enzymes, hormones & many other
substances.
64

Contd...

Used in purification of vitamins.


Concentration of proteins.
Concentration of biological products.
Stripping of solvents from vegetable
& plant or herbal extracts.
Removal of water & solvents from
fermentation broths.
Concentration of penicillin & related
products
65

Reference
Intro. to chem engg. Badger
Pharmaceutical engg by CVS
Subrahmanyam
Intro to pharm engg Paradkar

Syllabus for periodic test


1.
2.
3.
5.
6.
7.
9.

Fluid flow
Fluid and pressure measurements
Pumps
Conveying of solids
Crystallization
Evaporation
Refrigeration

Evaporator Accessories
Condensers,
expansion and bucket traps,
entrainment separators, Vacuum pump

Condensor
Surface Condensor
In surcface condensor, liquid to be
condensed and cooling liquid is
seperated by thin metal wall.

Contact Condensor
In this type Vapour and cooling liquid
are mixed directly.
Parallel/ Counter current
Wet/Dry condensor
Barometric/ Low Level

Surface Condensor
It is like tubular heater (exchanger)
Vapours outside tube and water inside the
tube.
"Heat transfer coefficient" or "Capicity to
cool" can be increase by increasing water
(cold) velocity (by making it multipass)
Vapour pressure is lower than atmospheric
pressure hence vacuum pump needed to
remove air.
It is used when vapours are other than
water vapour.

Surface Condensor

Contact condensor
If vapour to be condensed is water
then contact type condensor is
always used.
There is direct contact between
vapours and cooling liquid.

Parallel current wet contact


Wet contact
because outlet for
unn condensed
vapour and water
is same
Parallel current
because direction
of flow of water
and vapour is same.

Counter current dry contact


Dry contact
because outlet for
uncondensed
vapour and hot
liquid is different.
Counter current
because direction
of flow of cold
water and hot
vapour (Air) is
different.

Steam Traps
Condensate can be removed by
using pump/ trap
Steam trap is a device who's function
is to allow condensate to drain but to
prevent steam from blowing out of
the space drained.
Types
Expansion trap
Bucket trap
Tilt trap

Expansion Trap

A-Cartrige
B-corrugated tube
C-valve

Contd...
Space between cartrige and
corrugated tube is filled with oil
When cool condensate enter walve it
get drain out.
when steam enters valve, heat of
steam causes cartige to expand and
valve get closed.

Bucket Trap

Contd...
The inverted bucket steam trap consists of a
chamber containing an inverted bucket (the
opening at the bottom) which actuates a
discharge valve through a linkage.
The valve is open when the bucket rests at
the bottom of the trap. This allows air to escape
during warm-up
When condensate start accumulating bottom
inside and outside the inverted bucket, then
the bucket get sealed from its bottom side by
rising condensate.
The valve remains open as long as condensate
is flowing, and trapped air bleeds out through a
small vent in the top of the bucket.

Contd...
When steam enters the trap, it fills the
bucket, causing the bucket to float so it
rises and closes the valve.
The steam slowly escapes through the bucket
vent and condenses, thus allowing the bucket
to sink and reopen the valve for condensate
flow.
Small amounts of air and non-condensible
gases (such as carbon dioxide) that enter the
trap during normal operation are also vented
through the small opening in the top of the
bucket, which prevents the trap from
becoming air-bound.

Entrainment seperator
Principle If liquid
droplet can be
made to impinge
on solid surface
they coalesce into
a sheet, and not
readily picked even
by high vapour
velocities.

Vacuum pump
(steam-jet
ejector)
The pump use
to remove hot
water and non
condensed
gas from
parallel
current wet
condensor.

Vacuum pump Contd...


It consists of a motive fluid inlet nozzle and
a converging-diverging outlet nozzle.
Water, air, steam, or any other fluid at high
pressure provides the motive force at the
inlet.
The Venturi effect is a particular case of
Bernoulli's principle.
Fluid under high pressure is converted into a
high-velocity jet at the throat of the
convergent-divergent nozzle which creates
a low pressure at that point.
The low pressure draws the suction fluid into
the convergent-divergent nozzle where it
mixes with the motive fluid.

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