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SEPARATION PROCESSES
LAB MANUAL
_______________________________________________________
List of equipment
1. Batch Distillation Column
2. Continuous Distillation Column
3. Liquid Liquid Extraction Unit
List Of Experiments
1. To determine the pressure drop of the distillation column as function of boil-up rate in
batch distillation for batch distillation column.
2. To determine plate-to-plate temperature profiles along the column as a function of boil-up
rate for batch distillation column.
3. To observe the degree of formation of flooding on trays for each power increment for batch
distillation column.
4. To determine column efficiency as a function of boil-up rate, at total reflux for batch
distillation column.
5. To construct McCabe-Thiele diagram of operating line for batch distillation column.
6. To determine variation of top product composition with time at constant reflux ratio for
batch distillation column.
7. To determine the pressure drop of the distillation column as function of boil-up rate in
batch distillation for continuous distillation column.
8. To determine plate-to-plate temperature profiles along the column as a function of boil-up
rate for continuous distillation column.
9. To observe the degree of formation of flooding on trays for each power increment for
continuous distillation column.
10. To determine column efficiency as a function of boil-up rate, at total reflux for continuous
distillation column.
11. To construct McCabe-Thiele diagram of operating line for continuous distillation column.
12. To determine variation of top product composition with time at constant reflux ratio for
continuous distillation column.
Program Learning
Course Learning
Outcome (CLO): Upon successful completion of this course, students will be able to:
CLO-2: Analyze and Interpret the experimental data and verify the different
behaviours and trends on the empirical relations relations to above mentioned
phenomena also contemplate through experimentation.
4 Injury from sharp glass objects First aid kit is recommended for lab
Fire
5 1. ATU, diphenyl carbazone, Calmagite and EDTA CO2 type Fire extinguisher
can cause chemical fire at high temperature. is recommended
2. Electrical short circuiting (class C fire)
S. No. Chemicals
1 Methanol
Cleanliness
The Chemical Reaction Engineering Laboratory contains equipment that uses water
or chemicals as the fluid. There are “housekeeping” rules that students are required to clean up
their area at the conclusion of the performance of an experiment. Cleanup will include
Removal of spilled water (or any liquid) or chemicals
Wiping the table top on which the equipment is mounted
The lab should always be as clean as or cleaner than it was when you entered.
Cleaning the lab is your responsibility as a user of the equipment.
Safety
This is to serve as a guide and not as a comprehensive manual on safety. Every
staff/student has, at all time, a duty to care for Health and Safety of himself/herself and
of all people who may be affected by his/her action.
Lab coat or Jackets MUST is worn all times.
Rubber gloves should be worn when handling corrosive materials,
Any appropriate instruction sheets should be studied before starting the experiment.
Particular attention should be given to the recommended precautions, startup procedure
and sequence of operation.
There should be NO Eating, No Smoking is strictly prohibited in all laboratories
The objectives of this experiment, which involves batch distillation to separate alcohol from a
mixture of alcohol and water, are:
To determine the pressure drop of the distillation column as function of boil-up rate in
batch distillation.
To determine plate-to-plate temperature profiles along the column as a function of boil-
up rate
To observe the degree of formation of flooding on trays for each power increment
To determine column efficiency as a function of boil-up rate, at total reflux
To construct McCabe-Thiele diagram of operating line
To determine variation of top product composition with time at constant reflux ratio
To compare performance parameters (e.g. pressure drop, plate efficiency etc.) between
packed column and sieve plate column.
Introduction
Distillation is defined as a process in which liquid or vapor mixture of two or more substances is
separated into its component fractions of desired purity, by the application and removal of heat.
Distillation is based on the fact that the vapor of a boiling mixture will be richer in the
components that have lower boiling points, therefore when this vapor is cooled and condensed
the condensate will contain more volatile components. At the same time, the original mixture
will contain more of the less volatile material.
Distillation is in fact the most common separation technique used in industry, it consumes
enormous amounts of energy (both in terms of cooling and heating requirements), and it can
contribute to more than 50% of plant operating costs. The best way to reduce operating costs of
existing units is to improve their efficiency and operation via process optimisation and control.
To achieve this improvement, a thorough understanding of distillation principles and how
distillation systems are designed is essential. An example of a common distillation unit operation
is the separation of a solution containing water and alcohol. The alcohol is normally present in
greater quantities in the vapour. In most cases the component that is in the vapour in the greatest
quantities is the component with the lowest boiling point, although there are some cases when
this is not true. The fact that one component 'prefers' to be in the vapour is used to design
distillation columns which separate two or more substances based on differences in their
volatility.
There are many types of distillation column, each designed to perform specific types of
separation, and each differs in terms of complexity;
I. Batch column: In batch operation, the feed to the column is introduced batch-wise.
That is, the column is charge with a `batch` and then the distillation process is carried
out. When the desired task is achieved, a next batch of feed is introduced.
II. Continuous column: In contrast, continuous columns process a continuous feed
stream. No interruptions occur unless there is a problem with the column or
surrounding process unit.
They are capable of handling high throughputs and are the most common of the two types, trays
column and packed column;
a. Tray column(internal) – where trays (e.g. bubble cap, sieve tray etc.) of various design are
used to hold up the liquid to provide better contract between vapor and liquid
b. Packed column – where instead of trays `packings` (e.g. rasching rings) are used to
enhance contact between vapor and liquid.
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 (figure 1) contains several major
components:
I. A vertical shell (or column) where the separation of fluid components is carried out.
II. Column internals such as trays/plates or packings which are used to enhance components
separations.
III. A reboiler to provide the necessary vaporization for the distillation process.
IV. A condenser to cool and condensed the vapor leaving the top of the column
V. A reflux drums to hold the condensed vapor from the top of the column so
that liquid (reflux) can be recycled back to the column.
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) section and bottom
(stripping) section. This applies to the continuous distillation, whereas for batch distillation the
feed is poured direct to the reboiler. Heat is supplied to the reboiler to generate vapor. The source
of heat input can be any suitable fluid, although in most chemical plants this is normally stream.
In vapor 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 bottom product.
The vapor 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 and 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 vapor and liquid within the column as well as external flows of
feeds and product streams, into and out of the column.
Theory
One of the most common calculation methods used for distillation columns is McCabe-Thiele
method. It involves finding compositions and flows for the top (rectifying) and bottom
(stripping) sections of the column, and graphically determining the proper number of stages as
well as the appropriate feed stage. This graphical method is performed on a y-x (composition in
vapour phase vs. composition in liquid phases) equilibrium plot. The compositions of the
distillate, xD, and bottoms, xB, are plotted on the graph, and operating lines for the rectifying and
stripping sections are derived from these conditions. The McCabe-Thiele method can also be
used when side-withdrawal or multiple feeds are in use.
This experiment deals with a slightly different method, as it involves a batch distillation process.
While it is not commonly found in industry, it is still a very useful learning tool as it operates on
most of the same principles as continuous distillation columns. The column in the laboratory also
operates using total reflux. At total reflux, the mass balance over the column is:
… (1)
At steady state (temperatures are constant), the molar liquid flow rate is equal to the molar
vapour flow rate everywhere in the column, so yn=xn+1. This should result in an operating line
that is straight; co-incident with the y = x line. Therefore, determining the theoretical number of
plates is done by measuring the steady-state compositions at the top and bottom of the column.
The initial batch (liquid) composition is not directly involved, so it should be excluded from
calculations.
A useful quantity when studying distillation columns is the Murphree Efficiency (ηM). It is
measure of the efficiency of each individual tray. The Murphree Efficiency assumes that
complete mixing takes place between the liquid on the tray is of constant composition and is of
the same composition as the liquid entering the next tray below [2]. It can be calculated
numerically by using the following equation:
… (2)
where yn ≡ vapour mole fraction for vapour leaving plate n-1
yn-1 ≡ vapour mole fraction for vapour leaving plate n-1
yn* ≡ vapour in equilibrium with liquid leaving plate n
The overall plate efficiency for the column is found using the following formula:
… (3)
where Nt = number of theoretical (ideal) plates which can be calculated by different methods, i.e.
McCabe-Thiele graphical analysis, Fenske equation etc.
Na = number of actual plates.
Overall and Murphree efficiencies can be related by a simple expression assuming linear
selection involving phase equilibria and uniform Murphree efficiency across the column [4].
… (4)
Where: m = slope of equilibrium line
The operation of a batch column can be analyzed using a McCabe-Thiele diagram, with the same
operating-line equation that was used for the rectifying section of a continuous distillation
expressed as,
𝑅𝐷 𝑥𝐷
𝑦𝑛+1 = 𝑥𝑛 + … (5)
𝑅𝐷 +1 𝑅𝐷 +1
Equipment
A schematic layout of the batch distillation rig is shown in figure 2. The core equipment is a 75
mm diameter plate distillation column containing 8 sieve plates and downcomers. Every plate
includes a temperature sensor positioned to measure accurately the temperature of the liquid on
An overhead condenser is used to condense vapors by pumping in with measured and adjusted
cooling water. A condensate collecting vessel, equipped with overflow weirs and exit pipes
allows separation of immiscible liquids. A reflux return valve, solenoid operated, to provide for
0%-100% reflux, is adjustable by electrical signal.
A U tube differential manometer connected to the top and bottom of the column, serves purpose
of monitoring column pressure drop. Sampling points throughout the system are provided for
composition analysis.
The materials of construction for surfaces in contact with the process fluids are; glass, stainless
steel, PTFE or similar solvent resistant materials. Lagging is provided to prevent heat loss from
column and the condenser.
Sieve Plate Column Details:
o Column length = 1000mm
o Column dia = 80mm & inner dia=74mm
o No of plates = 08
o Each plate thickness = 12mm
o Plate to plate distance = 95mm
o Hole size = 3mm (Triangular)
o Plate to temperature sensor distance = 60mm
o Down comer glass tube dia = 10mm
o Weir height = 5mm
Packed Column Details:
o Wall thickness = 3mm
o Inner ɸ = 59mm
o Outer ɸ = 65mm
o Column length = 1000mm
o Vapour pressure point from bottom = 230mm
Thermocouple Display:
Operating Procedure
1. Check that all vent lines are open and all drain valves are closed.
2. Turn on the overhead condenser cooling water supply.
3. Charge the Reboiler (spherical vessel) up to the equator with a methanol/water mixture of
known concentration.
4. Find the composition of the initial charge by gravimetric analysis.
5. Turn on the switch of the heating source.
6. Wait for the column to settle down to uniform operation under total reflux (check the
thermometer readings under total reflux)
7. Set the reflux timer to the desired reflux ratio and switch on the timer.
8. At regular time interval (say after 15 minutes) , carry out the following steps:
o Record the thermometer readings of the Reboiler and the plates.
o Take samples from the top product sampling valve and analyze their compositions. (Find
the composition of the Reboiler from its temperature using the equilibrium data for
methanol/water system).
9. Continue the distillation until uniform operation has been reached.
10. Turn off the heating mantle and the reflux timer.
11. Find the average comopstion of the total distillate collected.
12. Turn off the condenser cooling water supply when boiling has stopped.
Treatment of Results:
The student should produce plots of column position against temperature and methanol
concentration against column position as a function of time, for each reflux ratio used. These
plots will be obtained as a function of boil up rate. Sketch the graphs are shown below:
The objectives of this experiment, which involves batch distillation to separate alcohol from a
mixture of alcohol and water, are:
To determine the pressure drop of the distillation column as function of boil-up rate in
batch distillation.
To determine plate-to-plate temperature profiles along the column as a function of boil-
up rate
To observe the degree of formation of flooding on trays for each power increment
To determine column efficiency as a function of boil-up rate, at total reflux
To construct McCabe-Thiele diagram of operating line
To determine variation of top product composition with time at constant reflux ratio
To compare performance parameters (e.g. pressure drop, plate efficiency etc.) between
packed column and sieve plate column.
Introduction
Distillation is defined as a process in which liquid or vapor mixture of two or more substances is
separated into its component fractions of desired purity, by the application and removal of heat.
Distillation is based on the fact that the vapor of a boiling mixture will be richer in the
components that have lower boiling points, therefore when this vapor is cooled and condensed
the condensate will contain more volatile components. At the same time, the original mixture
will contain more of the less volatile material.
Distillation is in fact the most common separation technique used in industry, it consumes
enormous amounts of energy (both in terms of cooling and heating requirements), and it can
contribute to more than 50% of plant operating costs. The best way to reduce operating costs of
existing units is to improve their efficiency and operation via process optimisation and control.
To achieve this improvement, a thorough understanding of distillation principles and how
distillation systems are designed is essential. An example of a common distillation unit operation
is the separation of a solution containing water and alcohol. The alcohol is normally present in
greater quantities in the vapour. In most cases the component that is in the vapour in the greatest
quantities is the component with the lowest boiling point, although there are some cases when
this is not true. The fact that one component 'prefers' to be in the vapour is used to design
distillation columns which separate two or more substances based on differences in their
volatility.
There are many types of distillation column, each designed to perform specific types of
separation, and each differs in terms of complexity;
III. Batch column: In batch operation, the feed to the column is introduced batch-wise.
That is, the column is charge with a `batch` and then the distillation process is carried
out. When the desired task is achieved, a next batch of feed is introduced.
IV. Continuous column: In contrast, continuous columns process a continuous feed
stream. No interruptions occur unless there is a problem with the column or
surrounding process unit.
They are capable of handling high throughputs and are the most common of the two types, trays
column and packed column;
a. Tray column(internal) – where trays (e.g. bubble cap, sieve tray etc.) of various design are
used to hold up the liquid to provide better contract between vapor and liquid
b. Packed column – where instead of trays `packings` (e.g. rasching rings) are used to
enhance contact between vapor and liquid.
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 (figure 1) contains several major
components:
I. A vertical shell (or column) where the separation of fluid components is carried out.
II. Column internals such as trays/plates or packings which are used to enhance components
separations.
III. A reboiler to provide the necessary vaporization for the distillation process.
IV. A condenser to cool and condensed the vapor leaving the top of the column
V. A reflux drums to hold the condensed vapor from the top of the column so
that liquid (reflux) can be recycled back to the column.
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) section and bottom
(stripping) section. This applies to the continuous distillation, whereas for batch distillation the
feed is poured direct to the reboiler. Heat is supplied to the reboiler to generate vapor. The source
of heat input can be any suitable fluid, although in most chemical plants this is normally stream.
In vapor 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 bottom product.
The vapor 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 and 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 vapor and liquid within the column as well as external flows of
feeds and product streams, into and out of the column.
Theory
One of the most common calculation methods used for distillation columns is McCabe-Thiele
method. It involves finding compositions and flows for the top (rectifying) and bottom
(stripping) sections of the column, and graphically determining the proper number of stages as
well as the appropriate feed stage. This graphical method is performed on a y-x (composition in
vapour phase vs. composition in liquid phases) equilibrium plot. The compositions of the
distillate, xD, and bottoms, xB, are plotted on the graph, and operating lines for the rectifying and
stripping sections are derived from these conditions. The McCabe-Thiele method can also be
used when side-withdrawal or multiple feeds are in use.
This experiment deals with a slightly different method, as it involves a batch distillation process.
While it is not commonly found in industry, it is still a very useful learning tool as it operates on
most of the same principles as continuous distillation columns. The column in the laboratory also
operates using total reflux. At total reflux, the mass balance over the column is:
… (1)
At steady state (temperatures are constant), the molar liquid flow rate is equal to the molar
vapour flow rate everywhere in the column, so yn=xn+1. This should result in an operating line
that is straight; co-incident with the y = x line. Therefore, determining the theoretical number of
plates is done by measuring the steady-state compositions at the top and bottom of the column.
The initial batch (liquid) composition is not directly involved, so it should be excluded from
calculations.
A useful quantity when studying distillation columns is the Murphree Efficiency (ηM). It is
measure of the efficiency of each individual tray. The Murphree Efficiency assumes that
complete mixing takes place between the liquid on the tray is of constant composition and is of
the same composition as the liquid entering the next tray below [2]. It can be calculated
numerically by using the following equation:
… (2)
where yn ≡ vapour mole fraction for vapour leaving plate n-1
yn-1 ≡ vapour mole fraction for vapour leaving plate n-1
yn* ≡ vapour in equilibrium with liquid leaving plate n
The overall plate efficiency for the column is found using the following formula:
… (3)
where Nt = number of theoretical (ideal) plates which can be calculated by different methods, i.e.
McCabe-Thiele graphical analysis, Fenske equation etc.
Na = number of actual plates.
Overall and Murphree efficiencies can be related by a simple expression assuming linear
selection involving phase equilibria and uniform Murphree efficiency across the column [4].
… (4)
Where: m = slope of equilibrium line
The operation of a batch column can be analyzed using a McCabe-Thiele diagram, with the same
operating-line equation that was used for the rectifying section of a continuous distillation
expressed as,
𝑅𝐷 𝑥𝐷
𝑦𝑛+1 = 𝑥𝑛 + … (5)
𝑅𝐷 +1 𝑅𝐷 +1
Equipment
A schematic layout of the batch distillation rig is shown in figure 2. The core equipment is a 75
mm diameter plate distillation column containing 8 sieve plates and downcomers. Every plate
includes a temperature sensor positioned to measure accurately the temperature of the liquid on
An overhead condenser is used to condense vapors by pumping in with measured and adjusted
cooling water. A condensate collecting vessel, equipped with overflow weirs and exit pipes
allows separation of immiscible liquids. A reflux return valve, solenoid operated, to provide for
0%-100% reflux, is adjustable by electrical signal.
A U tube differential manometer connected to the top and bottom of the column, serves purpose
of monitoring column pressure drop. Sampling points throughout the system are provided for
composition analysis.
The materials of construction for surfaces in contact with the process fluids are; glass, stainless
steel, PTFE or similar solvent resistant materials. Lagging is provided to prevent heat loss from
column and the condenser.
Sieve Plate Column Details:
o Column length = 1000mm
o Column dia = 80mm & inner dia=74mm
o No of plates = 08
o Each plate thickness = 12mm
o Plate to plate distance = 95mm
o Hole size = 3mm (Triangular)
o Plate to temperature sensor distance = 60mm
o Down comer glass tube dia = 10mm
o Weir height = 5mm
Packed Column Details:
o Wall thickness = 3mm
o Inner ɸ = 59mm
o Outer ɸ = 65mm
o Column length = 1000mm
o Vapour pressure point from bottom = 230mm
Thermocouple Display:
Operating Procedure
13. Check that all vent lines are open and all drain valves are closed.
14. Turn on the overhead condenser cooling water supply.
15. Charge the Reboiler (spherical vessel) up to the equator with a methanol/water mixture of
known concentration.
16. Find the composition of the initial charge by gravimetric analysis.
17. Turn on the switch of the heating source.
18. Wait for the column to settle down to uniform operation under total reflux (check the
thermometer readings under total reflux)
19. Set the reflux timer to the desired reflux ratio and switch on the timer.
20. At regular time interval (say after 15 minutes) , carry out the following steps:
o Record the thermometer readings of the Reboiler and the plates.
o Take samples from the top product sampling valve and analyze their compositions. (Find
the composition of the Reboiler from its temperature using the equilibrium data for
methanol/water system).
21. Continue the distillation until uniform operation has been reached.
22. Turn off the heating mantle and the reflux timer.
23. Find the average comopstion of the total distillate collected.
24. Turn off the condenser cooling water supply when boiling has stopped.
Treatment of Results:
The student should produce plots of column position against temperature and methanol
concentration against column position as a function of time, for each reflux ratio used. These
plots will be obtained as a function of boil up rate. Sketch the graphs are shown below:
ICATION EQUIPMENT
The most obvious form of humidification equipment is the spray chamber. Here, the contacting
liquid is sprayed as a mist into the gas stream. Gas velocity is kept low so that the contact time is
high so that there will be only small amount of liquid physically entrained in the gas stream. These
units are usually restricted to the small-scale operations and are frequently used in humidity control
of a room or plant where either humidification or dehumidification of the inlet air is required.
Types of cooling towers
Cooling towers are generally used for humidification operations. Cooling towers fall into two main
sub-divisions: natural draft and mechanical draft. Natural draft designs use very large concrete
chimneys to introduce air through the media. Due to the tremendous size of these towers (500 ft high
and 400 ft in diameter at the base) they are generally used for water flow rates above 200,000
gal/min. Usually these types of towers are only used by utility power stations. Mechanical draft
cooling towers are much more widely used. These towers utilize large fans to force air through
circulated water. The water falls downward over fill surfaces that help increase the contact time
between the water and the air. This helps maximize heat transfer between the two. The experimental
setup for UG lab uses mechanical draft cooling tower, which is shown in Fig.1.
The physical arrangement is shown in Fig.2. The subscripts 1 and 2 refer to the bottom and top of the
column.
On the basis, for a tower of constant cross section, an overall material balance gives
Most commonly, the column will operate nearly adiabatically with q→0. The approach to adiabatic
operation will be closer the larger the column diameter. For this situation, similar balances for the
differential height (dz) will be written. The condensable component balance becomes
If the rate of solute transfer between phases is small compared to the total flow stream, an average
value of L may be used, and the change in enthalpy of the liquid phase may be expressed as if it
resulted solely from the change in temperature at constant specific heat. Thus,
where
For the change in gas–phase enthalpy, the expression in terms of temperature is rigorous if c is
h
constant.
Rate equations for heat and mass transfer can also be written. Here, however,
complications arise because of the fact that heat is transferred from the bulk of the liquid
phase to the liquid-gas interface entirely as a result of the temperature potential, but from
the interface to the bulk of the gas phase, heat is transferred as the result by two
mechanisms. On the gas-phase side of the interface, heat is transferred as the result of a
temperature potential, and the latent heat associated with the mass transfer is transferred by
these two mechanisms are separated as the two terms on the right side of the equation (8).
With these ideas, equations for the heat- transfer processes indicated in equations (6) and (8) can be
written separately. For the liquid phase transfer
for the gas phase. Separating k a from the right side of the equation and designating h /k c as r, the
y c y h
psychrometric ratio, give
In putting r into this equation for h a/ k ac , the assumption is made that a, the area per unit
c y h
volume of tower, is the same for heat transfer as it is for mass transfer. This will be true only at such
high liquid rates that the tower packing is completely wet. If r is equal to 1, as it is for the air-water
system under normal conditions, the terms within parentheses in equation (13) are enthalpies as
defined by equation (13a).
Equation (15) is a design equation; the driving force is expressed as an enthalpy difference. Enthalpy
is an extensive thermodynamic property. As such, it cannot be a driving force for any transfer
operation. Thus, the mathematical treatment that leads to equation (15) should be examined. First,
in the energy balances, the total flow per unit time is fixed. The enthalpy terms are then “specific
enthalpy”, based upon a fixed mass of material. Second, in the basic design equation, Equation (13),
the driving force is a function of T and Y, the quantities that would be expected to control rates of
heat and of mass transfer. Only in the fortuitous case that r=1 can H be substituted for these T and
Y functions. In all other cases, Equation (15)would be written as
Equation (18) applies at any point in an air-water contacting device. From it, the
temperature and the enthalpy of the interface can be determined at any point for which the
liquid temperature (T ), the gas enthalpy (H ), and the ratio of the liquid-phase heat transfer
L V
coefficient to the gas- phase heat transfer coefficient to the gas-phase mass transfer coefficient
based upon mole-ratio driving forces are known.
The interface conditions can be obtained through equation (18) using a graphical method.
A plot is drawn with coordinates of liquid-phase temperature versus enthalpy of the gas phase. On it,
the locus of interface H and T values can be plotted by realizing that at the interface the vapor phase
i i
will be saturated at the interface temperature if the assumption that equilibrium exists at a phase
boundary is tenable. From the saturation curve on the air-water humidity chart, the saturation molal
humidity can be obtained for any desired temperature. The saturation, or interface, enthalpy can then
be calculated or read from the humidity chart.
On the same plot, an “operating line” of H versus T can be plotted by combining equations (5) and
V L
(6) and integrating. This curve represents the path of bulk-phase conditions as the fluids pass through
the unit. Thus,
where the limits again refer to the bottom and top of the column. Integrating,
And rearranging,
1
This equation gives the slope of the H versus T “operating” line as L C /V . For the air-water
V L aV L
system and for most other dilute gas-solution systems, this ratio is constant over a moderate
humidity range, and the straight H versus T line can be determined from knowledge of the liquid-
V L
and gas-phase flow rates and the conditions of both streams at one end of the column, or
alternatively the line can be located from the conditions at both ends of the column.
From this construction, Equation (15) can now be integrated graphically. The necessary driving force
in terms of enthalpy is determined for representative points throughout the column. For point B on
1
Fig.3, this would be (H – H ). Values of V /SK a(H – H ) are then plotted against H and the area
in Vn Y i V V
under this curve determined between the limits of H and H in order to find the column height (z).
V1 V2
Psychrometric chart is shown in appendix at the end of this report. From the wet bulb and dry bulb
temperature of the air, other air properties like absolute humidity, relative humidity, enthalpy of
saturated and unsaturated air can be found out from the psychrometric chart and are used for
estimating the tower height.
Procedure:
1. Start the fan.
2. Start water pump and adjust the flow rate to a desired value.
3. Start the water heater and set the inlet temperature to a desired value.
4. Measure wet bulb temperature and dry bulb temperature of outlet water.
5. Wait till the steady state is obtained. The attainment of the steady state is confirmed by the
constancy in the outlet temperature.
6. Measure air velocity by anemometer.
7. Measure inlet temperature and outlet temperature of air.
8. Repeat steps 2 to7 by changing water flow rate or inlet temperature of water.
Calculations:
1. Verify the overall material and energy balance
2. Calculate heat and mass transfer coefficients by a graphical method described above.
Safety precautions:
1. Ensure the valve V (cooling tower inlet water valve) in partly open position and remaining
1
valves in fully open position.
2. Restrict the flow rate of inlet water to cooling tower to 100 LPM.
3. Don’t touch any electrical connections.
4. Don’t put hands in any rotating equipment like fan, pump shaft etc.
5. If any equipment malfunctions, turn off electric mains immediately.
Nomenclature:
L = liquid flow rate into the top of the column, lb mole/hr (or mol/s)
2
V = flow rate of gas phase entering the column, lb mole/hr (or mol/s)
1
1
V = flow rate of solvent, or “dry” gas, lb mole/hr (or mol/s)
Y = mole ratio of solute to solvent gas at the top of the column
2
H = enthalpy of gas phase entering the column, Btu/lb mole of “dry” gas
V1
(or joule/mol)
H = enthalpy of liquid phase entering the top of the column, Btu/lb mole of liquid
L2
(or joule/mol)
q = heat transferred to the column from its surroundings, Btu/hr (or joule/s)
T , T = temperature of liquid and gas phases, respectively
L v
dz = a differential height of column packing, ft (or m)
2 2
A = interfacial surface, ft (or m )
2 3 3
a = interface area, ft /ft of column volume (or m2/m of column volume)
2 2
S = tower cross section, ft (or m )
Cooling Tower
Experiment No 12
Objective:
To determine average heat and mass transfer coefficients and to estimate the tower height
Theory:
When a component is transferred from a gas phase to solution in a liquid phase, the latent heat
associated with the condensation is evolved. In the operations where mass transfer proceeds by
equimolar counter diffusion, as in distillation or in operations where latent heat effect are small, as in
liquid –liquid extraction, gas absorption in dilute solutions, and leaching, heat transfer is of minor
importance as a rate controlling mechanism. In others, particularly where there is a net transfer of
mass from gas phase to condensed phase or vice versa, the heat transfer rate is important. In these
cases, heat transfer significantly limits the rate at which mass can be transferred.
Of those operations where both heat transfer and mass transfer affect the rate, humidification and
dehumidification involve two components and two phases. The liquid phase, most often water, is
single component, and the gas phase consists of a non-condensable gas, usually air, in which some
vapor from the liquid phase is present.
HUMIDIFICATION: INDUSTRIAL APPLICATIONS
Humidification process may be carried out to control the humidity of a space or, more usually, to
cool and recover water by contacting it with low humidity air. The water that has lost heat to the
atmosphere can then be reused in heat exchanger throughout a plant. Alternatively, the water could
be cooled in the surface heat exchanger. The choice is one of economics, with the designer balancing
the loss of cooling water inherent in the air- water contact cooler against the cost of supplying and
handling the cooling source to the surface cooler and the higher cost of surface units.
HUMIDIFICATION EQUIPMENT
The most obvious form of humidification equipment is the spray chamber. Here, the contacting
liquid is sprayed as a mist into the gas stream. Gas velocity is kept low so that the contact time is
high so that there will be only small amount of liquid physically entrained in the gas stream. These
units are usually restricted to the small-scale operations and are frequently used in humidity control
of a room or plant where either humidification or dehumidification of the inlet air is required.
Types of cooling towers
Cooling towers are generally used for humidification operations. Cooling towers fall into two main
sub-divisions: natural draft and mechanical draft. Natural draft designs use very large concrete
chimneys to introduce air through the media. Due to the tremendous size of these towers (500 ft high
and 400 ft in diameter at the base) they are generally used for water flow rates above 200,000
gal/min. Usually these types of towers are only used by utility power stations. Mechanical draft
cooling towers are much more widely used. These towers utilize large fans to force air through
circulated water. The water falls downward over fill surfaces that help increase the contact time
between the water and the air. This helps maximize heat transfer between the two. The experimental
setup for UG lab uses mechanical draft cooling tower, which is shown in Fig.1.
The physical arrangement is shown in Fig.2. The subscripts 1 and 2 refer to the bottom and top of the
column.
On the basis, for a tower of constant cross section, an overall material balance gives
Most commonly, the column will operate nearly adiabatically with q→0. The approach to adiabatic
operation will be closer the larger the column diameter. For this situation, similar balances for the
differential height (dz) will be written. The condensable component balance becomes
If the rate of solute transfer between phases is small compared to the total flow stream, an average
value of L may be used, and the change in enthalpy of the liquid phase may be expressed as if it
resulted solely from the change in temperature at constant specific heat. Thus,
where
For the change in gas–phase enthalpy, the expression in terms of temperature is rigorous if c is
h
constant.
Rate equations for heat and mass transfer can also be written. Here, however,
complications arise because of the fact that heat is transferred from the bulk of the liquid
phase to the liquid-gas interface entirely as a result of the temperature potential, but from
the interface to the bulk of the gas phase, heat is transferred as the result by two
mechanisms. On the gas-phase side of the interface, heat is transferred as the result of a
temperature potential, and the latent heat associated with the mass transfer is transferred by
these two mechanisms are separated as the two terms on the right side of the equation (8).
With these ideas, equations for the heat- transfer processes indicated in equations (6) and (8) can be
written separately. For the liquid phase transfer
for the gas phase. Separating k a from the right side of the equation and designating h /k c as r, the
y c y h
psychrometric ratio, give
In putting r into this equation for h a/ k ac , the assumption is made that a, the area per unit
c y h
volume of tower, is the same for heat transfer as it is for mass transfer. This will be true only at such
high liquid rates that the tower packing is completely wet. If r is equal to 1, as it is for the air-water
system under normal conditions, the terms within parentheses in equation (13) are enthalpies as
defined by equation (13a).
Equation (15) is a design equation; the driving force is expressed as an enthalpy difference. Enthalpy
is an extensive thermodynamic property. As such, it cannot be a driving force for any transfer
operation. Thus, the mathematical treatment that leads to equation (15) should be examined. First,
in the energy balances, the total flow per unit time is fixed. The enthalpy terms are then “specific
enthalpy”, based upon a fixed mass of material. Second, in the basic design equation, Equation (13),
the driving force is a function of T and Y, the quantities that would be expected to control rates of
heat and of mass transfer. Only in the fortuitous case that r=1 can H be substituted for these T and
Y functions. In all other cases, Equation (15)would be written as
Equation (18) applies at any point in an air-water contacting device. From it, the
temperature and the enthalpy of the interface can be determined at any point for which the
liquid temperature (T ), the gas enthalpy (H ), and the ratio of the liquid-phase heat transfer
L V
coefficient to the gas- phase heat transfer coefficient to the gas-phase mass transfer coefficient
based upon mole-ratio driving forces are known.
The interface conditions can be obtained through equation (18) using a graphical method.
A plot is drawn with coordinates of liquid-phase temperature versus enthalpy of the gas phase. On it,
the locus of interface H and T values can be plotted by realizing that at the interface the vapor phase
i i
will be saturated at the interface temperature if the assumption that equilibrium exists at a phase
boundary is tenable. From the saturation curve on the air-water humidity chart, the saturation molal
humidity can be obtained for any desired temperature. The saturation, or interface, enthalpy can then
be calculated or read from the humidity chart.
On the same plot, an “operating line” of H versus T can be plotted by combining equations (5) and
V L
(6) and integrating. This curve represents the path of bulk-phase conditions as the fluids pass through
the unit. Thus,
where the limits again refer to the bottom and top of the column. Integrating,
And rearranging,
1
This equation gives the slope of the H versus T “operating” line as L C /V . For the air-water
V L aV L
system and for most other dilute gas-solution systems, this ratio is constant over a moderate
humidity range, and the straight H versus T line can be determined from knowledge of the liquid-
V L
and gas-phase flow rates and the conditions of both streams at one end of the column, or
alternatively the line can be located from the conditions at both ends of the column.
From this construction, Equation (15) can now be integrated graphically. The necessary driving force
in terms of enthalpy is determined for representative points throughout the column. For point B on
1
Fig.3, this would be (H – H ). Values of V /SK a(H – H ) are then plotted against H and the area
in Vn Y i V V
under this curve determined between the limits of H and H in order to find the column height (z).
V1 V2
Psychrometric chart is shown in appendix at the end of this report. From the wet bulb and dry bulb
temperature of the air, other air properties like absolute humidity, relative humidity, enthalpy of
saturated and unsaturated air can be found out from the psychrometric chart and are used for
estimating the tower height.
Procedure:
1. Start the fan.
2. Start water pump and adjust the flow rate to a desired value.
3. Start the water heater and set the inlet temperature to a desired value.
4. Measure wet bulb temperature and dry bulb temperature of outlet water.
5. Wait till the steady state is obtained. The attainment of the steady state is confirmed by the
constancy in the outlet temperature.
6. Measure air velocity by anemometer.
7. Measure inlet temperature and outlet temperature of air.
8. Repeat steps 2 to7 by changing water flow rate or inlet temperature of water.
Calculations:
1. Verify the overall material and energy balance
2. Calculate heat and mass transfer coefficients by a graphical method described above.
Safety precautions:
1. Ensure the valve V (cooling tower inlet water valve) in partly open position and remaining
1
valves in fully open position.
2. Restrict the flow rate of inlet water to cooling tower to 100 LPM.
3. Don’t touch any electrical connections.
4. Don’t put hands in any rotating equipment like fan, pump shaft etc.
5. If any equipment malfunctions, turn off electric mains immediately.
Nomenclature:
L = liquid flow rate into the top of the column, lb mole/hr (or mol/s)
2
V = flow rate of gas phase entering the column, lb mole/hr (or mol/s)
1
1
V = flow rate of solvent, or “dry” gas, lb mole/hr (or mol/s)
Y = mole ratio of solute to solvent gas at the top of the column
2
H = enthalpy of gas phase entering the column, Btu/lb mole of “dry” gas
V1
(or joule/mol)
H = enthalpy of liquid phase entering the top of the column, Btu/lb mole of liquid
L2
(or joule/mol)
q = heat transferred to the column from its surroundings, Btu/hr (or joule/s)
T , T = temperature of liquid and gas phases, respectively
L v
dz = a differential height of column packing, ft (or m)
2 2
A = interfacial surface, ft (or m )
2 3 3
a = interface area, ft /ft of column volume (or m2/m of column volume)
2 2
S = tower cross section, ft (or m )
0 He alth
1 0 Fire
Re activity
Pe rs onal
Prote ction
Composition:
Toxicological Data on Ingredients: Sodium chloride: ORAL (LD50): Acute: 3000 mg/kg [Rat.]. 4000 mg/kg [Mouse].
DERMAL (LD50): Acute: >10000 mg/kg [Rabbit]. DUST (LC50): Acute: >42000 mg/m 1 hours [Rat].
Section 3: Hazards Identification
Potential Acute Health Effects: Slightly hazardous in case of skin contact (irritant), of eye contact (irritant), of
ingestion, of inhalation.
Potential Chronic Health Effects:
CARCINOGENIC EFFECTS: Not available. MUTAGENIC EFFECTS: Mutagenic for mammalian somatic cells. Mutagenic for
bacteria and/or yeast. TERATOGENIC EFFECTS: Not available. DEVELOPMENTAL TOXICITY: Not available. Repeated or
prolonged exposure is not known to aggravate medical condition.
Skin Contact:
Wash with soap and water. Cover the irritated skin with an emollient. Get medical attention if irritation
develops. Cold water may be used.
Prepared by: Aasia Farrukh Section 4: First Aid Measures Date: 09-08-2017
Signature: ____________________
Eye Contact:
Department of Chemical Engineering Separation Processes
Transfer Lab Manual
Wah Engineering College, WahCantt.
Small Spill:
Use appropriate tools to put the spilled solid in a convenient waste disposal container. Finish cleaning by spreading water on
the contaminated surface and dispose of according to local and regional authority requirements.
Large Spill:
Use a shovel to put the material into a convenient waste disposal container. Finish cleaning by spreading water on the
contaminated surface and allow to evacuate through the sanitary system.
Section 7: Handling and Storage
Precautions:
Keep locked up.. Do not ingest. Do not breathe dust. Avoid contact with eyes. Wear suitable protective clothing. If ingested,
seek medical advice immediately and show the container or the label. Keep away from incompatibles such as oxidizing
agents, acids.
Inhalation:
If inhaled, remove to fresh air. If not breathing, give artificial respiration. If breathing is difficult, give
oxygen. Get medical attention if symptoms appear.
Incompatibility with various substances: Reactive with oxidizing agents, metals, acids.
References:
-Hawley, G.G.. The Condensed Chemical Dictionary, 11e ed., New York N.Y., Van Nostrand Reinold, 1987. -SAX, N.I. Dangerous
Properties of Indutrial Materials. Toronto, Van Nostrand Reinold, 6e ed. 1984. -The Sigma-Aldrich Library of Chemical Safety
Data, Edition II.
Other Special Considerations: Not available.
Created: 10/11/2005 12:33 PM
Special Remarks on the Products of Biodegradation: Not available.
Waste Disposal:
Waste must be disposed of in accordance with federal, state and local environmental control regulations.
The information above is believed to be accurate and represents the best information currently available to u
However, we make no warranty of merchantability or any other warranty, express or implied, with respect to suc
information, and we assume no liability resulting from its use. Users should make their own investigations
determine the suitability of the information for their particular purposes. In no event shall ScienceLab.com be liab
for any claims, losses, or damages of any third party or for lost profits or any special, indirect, incidenta
consequential or exemplary damages, howsoever arising, even if ScienceLab.com has been advised of th
possibility of such damages.
0 He alth
1 0 Fire
Re activity
Pe rs onal
Prote ction
Potential Acute Health Effects: Slightly hazardous in case of skin contact (irritant), of eye contact (irritant), of ingestion,
of inhalation.
Potential Chronic Health Effects:
CARCINOGENIC EFFECTS: Not available. MUTAGENIC EFFECTS: Mutagenic for mammalian somatic cells. Mutagenic for
bacteria and/or yeast. TERATOGENIC EFFECTS: Not available. DEVELOPMENTAL TOXICITY: Not available. The substance may
be toxic to blood, cardiovascular system. Repeated or prolonged exposure to the substance can produce target organs
damage.
Composition:
Toxicological Data on Ingredients: Potassium chloride: ORAL (LD50): Acute: 2500 mg/kg [Guinea pig]. 2600 mg/kg [Rat].
mg/kg [Mouse].
1500
Prepared by: Aasia Farrukh Section 4: First Aid Measures Date: 09-08-2017
Signature: ____________________
Eye Contact:
Department of Chemical Engineering Separation Processes
Transfer Lab Manual
Wah Engineering College, WahCantt.
Check for and remove any contact lenses. In case of contact, immediately flush eyes with plenty of water
for at least 15 minutes. Cold water may be used. Get medical attention.
Skin Contact:
Wash with soap and water. Cover the irritated skin with an emollient. Get medical attention if irritation
develops. Cold water may be used.
Small Spill:
Use appropriate tools to put the spilled solid in a convenient waste disposal container. Finish cleaning by spreading water on
the contaminated surface and dispose of according to local and regional authority requirements.
Large Spill:
Use a shovel to put the material into a convenient waste disposal container. Finish cleaning by spreading water on the
contaminated surface and allow to evacuate through the sanitary system.
Section 7: Handling and Storage
Precautions:
Do not ingest. Do not breathe dust. If ingested, seek medical advice immediately and show the container or the label. Keep
away from incompatibles such as oxidizing agents, acids, moisture.
Storage: Keep container tightly closed. Keep container in a cool, well-ventilated area. Hygroscopic
Inhalation:
If inhaled, remove to fresh air. If not breathing, give artificial respiration. If breathing is difficult, give
oxygen. Get medical attention.
Waste Disposal:
Waste must be disposed of in accordance with federal, state and local environmental control regulations.
The information above is believed to be accurate and represents the best information currently available to us.
However, we make no warranty of merchantability or any other warranty, express or implied, with respect to such
information, and we assume no liability resulting from its use. Users should make their own investigations to
determine the suitability of the information for their particular purposes. In no event shall ScienceLab.com be liable
for any claims, losses, or damages of any third party or for lost profits or any special, indirect, incidental,
consequential or exemplary damages, howsoever arising, even if ScienceLab.com has been advised of the
possibility of such damages.
Prepared by: Aasia Farrukh Date: 09-08-2017
Signature: ____________________
Department of Chemical Engineering Separation Processes
Transfer Lab Manual
Wah Engineering College, WahCantt.