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Kuwait University

College of Engineering and Petroleum

Mass Transfer Operations


Laboratory Manual

ChE 443

Edited by: Khaled A. Mahdi


Chemical Engineering Department
2007
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This is the second edition of the mass transfer operations laboratory manual. The
manual is the product of previous works by talented engineers in the chemical
engineering department. I have to mention the typing of the previous collections
of experiments by eng. Hala Al-Fulaij, and Dr. Amal Al-Kilani. As of this new
manual, I appreciate the comments from eng. Intesar Al-Gunaim and the help of
eng Mubarak Ghanim. I enjoyed the practical comments by the technician in the
mass lab, Mr. Essam Abdul Ali. The figures of this manual were scanned by eng.
Khaled Dhamiyar. To them I give my full appreciation and gratuities.

2
CONTENTS

1 VAPOR-LIQUID EQUILIBRIA 5

2 PACKED AND BUBBLE CAP COLUMN CONTINUOUS DIS-


TILLATION 12

3 Solid-Liquid Extraction (Leaching) 20

4 SPRAY DRYING 27

5 Fixed and Fluidized bed 32

6 DOUBLE EFFECT EVAPORATOR 39

7 TUBULAR REACTOR 44

8 Writing a Formal Technical Report

9 Sample Report

3
Llvw Oi Fljxuhv

1.1 Schematic diagram of Ellis Still. . . . . . . . . . . . . . . . . . . . 11


2.1 Schematic diagram of a distillation column. . . . . . . . . . . . . . 17
2.2 Refractive Index versus Mol% of Methanol in Water. . . . . . . . 18
2.3 Flow diagram of combined bubble-cap and packed distillation column. 19
3.1 Block diagram of solid-liquid extraction and solvent recovery. . . . 25
3.2 Flow diagram of leaching unit. . . . . . . . . . . . . . . . . . . . . 26
4.1 Spray Drying Equipment. . . . . . . . . . . . . . . . . . . . . . . 31
6.1 Schematic diagram of multiple effect evaporator. . . . . . . . . . . 42
6.2 Double effect evaporator expiremntal setup. . . . . . . . . . . . . 43
7.1 Differential mass balance of tubular reactor. . . . . . . . . . . . . 47
7.2 Schematic diagram of tubular reactor. . . . . . . . . . . . . . . . 48

4
1. VAPOR-LIQUID EQUILIBRIA

1.1. Background
The study of vapor-liquid equilibria is important due to its applications in sep-
aration processes involving volatile mixtures. For example, one major applica-
tion of vapor-liquid equilibrium analysis is the calculation of dew and bubble
points. Chemical thermodynamics provides us with tools to understand vapor-
liquid equilibrium in different solutions. Generally, there are two types of solu-
tions, ideal solutions such as Benzene-Toluene solutions and non-ideal solutions
such as tetrachloride-methanol and acetone-chloroform solutions. The reason for
non-ideality is mainly due to the influence of molecular interactions whereas ideal
solutions show very weak molecular interactions that can be neglected. Simple
thermodynamics laws can describe ideal solutions, for instance, Roault’s law and
Henry’s law. On the other hand, more advance models are needed to describe
the thermodynamics of real systems. Examples of these models are Margules
equations and Van Laar equations.

1.2. Objectives
• To understand vapor-liquid equilibria of solutions.

• To determine the activity coefficients of each components.

• To evaluate the parameters of different thermodynamics models such as Van


Laar, and Margules.

1.3. Theory
Under certain pressure and temperature, a binary solution of two volatile compo-
nents can exist in 2 phases, liquid and vapor. Each component distributes its self
between the two phases. According to the phase rule, the compositions at each
phase are predetermined if the pressure and temperature are both fixed. When a
liquid mixture of two components of different volatility is heated in a closed vessel,

5
vaporization of both components will occur until the pressure of the vapor attains
a steady state corresponding to the bubble point of the mixture. If the tempera-
ture of this mixture is maintained constant, vaporization and condensation of the
two components will proceed until equilibrium between the vapor and the liquid is
attained. This equilibrium depends on temperature and the total pressure of the
vessel. The pressure exerted by each component will depend on the composition
of the mixture and the saturated vapor pressure of each component. According
to Roult’s law, in an ideal mixture of components 1 and 2, the partial pressure
exerted by each components is proportional to its mole fraction, where the pro-
portionality constant is the vapor pressure of that component. Mathematically
expresses as,

P1 = x1 P1∗ , (1.1)
P2 = x2 P2∗ , (1.2)

Where: Pi is partial pressure of component i at a fixed temperature; Pi∗ is the


vapor pressure of component i at a given temperature; xi is the liquid mole fraction
of component i at equilibrium. The total pressure P according to Dalton’s law of
partial pressures is given by

P = P1 + P2 ,
= x1 P1∗ + x2 P2∗ , (1.3)

since the total mass is conserved, x1 +x2 = 1. The total pressure can be expressed
as
P = x1 P1∗ + (1 − x1 )P2∗ . (1.4)
In the vapor phase, the partial pressure of a component is given by, Pi = yi P ,
where yi is the vapor mole fraction of component i. Using equations 1.1 and 1.2,

y1 P = x1 P1∗ , (1.5)
y2 P = x2 P2∗ . (1.6)

In practice, most mixtures are not ideal; therefore, equations 1.5 and 1.6 should
be modified. This can be done by introducing the activity coefficients γ in the
liquid phase and the fugacity coefficient in the vapor phase φ.

y1 φ1 P = γ 1 x1 P1∗ , (1.7)
y2 φ2 P = γ 2 x2 P2∗ . (1.8)

For simplicity we will assume that the vapor phase is ideal hence the fugacity
coefficients are 1. The activity coefficient of a component in a mixture is a function

6
of temperature, pressure and composition. Thus, it has to be determined from
experiments.. Often, it is calculated from the vapor-liquid equilibria data at
specified conditions.

1.4. Procedure
Apparatus
The apparatus, shown in figure 1.1, consists of a boiling chamber A in which the
mixture under test is vigorously bullated to produce a vapor liquid mixture that
passes through the glass spiral tube B at a high velocity. The rising vapor entrains
drops of the liquid, which equilibrates with the vapor, and the mixtures emerge
from the tube at equilibrium, striking the thermocouple pocket C that contains
a thermocouple to measure the boiling temperature. The vapor then rises gently
through the central tube E while the liquid drops fall back into chamber F. The
vapor emerging from the tube E passes through the annulus G which is heated
electrically in order to prevent condensation and therefore all the vapors pass to
condenser H where they are totally condensed (the branch at H is fitted with
a vapor trap). The liquid formed accumulates in the receiver J from which a
sample of the vapor phase is obtained. When the receiver J is full of condensate it
overflows and passes through tube P to mix with the liquid flowing down tube K
from chamber F. This mixture enters heater A to be re-vaporized and discharged as
a mist into spiral B where it is equilibrated on emerging against the thermocouple
pocket C.
The contents of the still are recirculated in this manner for about 1.5 hours to
ensure that the equilibrium is attained. When the equilibrium is attained between
the liquid and the vapor phases, a sample of the vapor phase is taken from tap
M and a sample of the liquid phase is taken from tap N. This concludes the
experiment with this specific mixture and the contents of the still are therefore
drained through drain cock Q. A fresh mixture of different composition is then
charged and the experiment is repeated.

Experimental steps
Pleas make sure that THE SAFETY SHIELD MUST ALWAYS BE IN
PLACE BEFORE THE EXPERIMENT COMMENCES. Follow the steps
of the experiment carefully,

1. Prepare 350 ml of the mixture (provided by your lab instructores).

2. Remove access panel from base of safety case.

7
3. Transfer the prepared mixture into equilibrium still until the mixture covers
the coil B and is above the thermocouple C.

4. Replace the vapor trap H and turn on the cooling water ensuring that there
is a rapid flow of water through the condenser. Do not drain the receiver J.

5. Ensure that the thermocouple pocket R and C are filled with sufficient oil
to immerse the tips of the thermocouples and vent S is closed.

6. Replace access panel.

7. Switch on the still heater to boil the liquid, ensure that the jacket is switched
off.

8. Once boiling starts, slowly adjust the jacket heater control until the ther-
mocouple in the jacket indicate 2 - 5 C higher than the still’s temperature.

9. Adjust the still heater control so that only 20 drops per minute fall from
the base of the condenser into the distillate receiver J.

10. Continue the boiling process for at least 1.5 hours. Monitor the still and
jacket temperatures every 15 minutes and adjust the still and jacket heater
controls as required.

11. After 45 minute, take samples (one from the still and one from the distillate
receiver) then measure their refractive indices to find their compositions
using the calibration curve provided to you by your lab instructor.

12. After 1.5 hours, switch off the equipment then take another set of samples
as in step 11.

1.5. Practice Questions


(1) A pressurized pot always cook the food faster than a regular (non-pressurized)
pot, explain using phase equilibrium thermodynamics.

(2) Does the system you studied in this experiment exhibit negative or positive
deviation from ideality? Use figures 3 and 4 to support your answer.

(3) How do you make sure that the solution, in your experiment, reach steady
state (equilibrium)?

(4) Name four non-ideal binary systems and specify if the system is positively
or negatively deviated from ideality.

8
(5) How do your results change if the fugacity of the vapor is considered?

(6) ”According to the phase rule, the compositions of a two-phase binary solution
are predetermined if the pressure and temperature are both fixed.” Explain
this statement.

(7) A Water/Ethanol solution is in equilibrium at 760 mmHg and 80o C. The


equilibrium data of the solution is shown in the table.

Material xi yi Ai Bi Ci
Water 0.320 8.16 1623 229
Ethanol 0.506 7.97 1668 228

Use Antoine equation to calculate the vapor pressures (in mmHg) and Tem-
perature (o C) in of the components.

Bi
log Pi∗ = Ai −
T + Ci
Calculate: (1) The K-values of Water and Ethanol?. (2) The activity coeffi-
cients, γ of Water and Ethanol?

1.6. Report
You are expected to suggest answers to the practice questions in your report.
Some of your answers can be used in the introduction and/or discussion. In your
reports, the following calculations MUST be reported and discussed:

• Find the composition from the refractive index using the calibration curve.

• Find the activity coefficient experimentally using equations 1.7 and 1.8.

• Using the experimentally determined activity coefficients, evaluate the pa-


rameters A and B in the 3-suffix Margules equation. If you are given the
excess free energy of the model,

g E = x1 x2 [A + B(x1 − x2 )] (1.9)

Note: you have to derive the activity coefficients from the excess energy
before you determine the constants.

9
• Determine the Van-Laar Equation parameters A and B using the activity
coefficients equations
A
ln γ 1 = (1.10)
(1 + Ax1 /Bx2 )2
B
ln γ 2 = (1.11)
1 + (Bx2 /Ax1 )2

• Discuss the use of your equilibrium data to predict the equilibrium at an-
other set of conditions using 2-suffix Margules and Van Laar equations ??
to 1.11.

References
H. C. Smith and J. M. Van ness. Introduction to Chemical Engineering Thermo-
dynamics. McGraw-Hill, 4th edition, 1987.

J. M. Prausnitz. Molecular Thermodynamics of Fluid Phase Equilibria. Prentice-


Hall, 1969.

B. G. Kyle. Chemical and Process Thermodynamics. Prentice Hall, 2nd edi-


tion, 1992.

K. S. Pitzer. Thermodynamics. McGraw-Hill, 3rd edition, 1995.

10
Figure 1.1: Schematic diagram of Ellis Still.

11
2. PACKED AND BUBBLE CAP COLUMN
CONTINUOUS DISTILLATION

2.1. Background
Distillation is one of the major operations in the chemical and petroleum indus-
tries, especially oil refineries. The main purpose of a distillation column is to
separate two or more volatile components; an example of a distillation column is
shown in figure 2.1. This experiment examines two types of distillation columns,
bubble-cap and packed. Other types, not examined here, include ballast trays
and perforated (Sieve) plates. Bubble-cap columns are classical in the chemical
industries, they are known as early as 1800’s. Packed columns were introduced
later. The use of one type over the other is governed by the objectives of the
process.
The distillation column operates as follows, the feed, in a liquid state, is in-
troduced continuously at a midpoint in the column. The midpoint divides the
column into enriching and stripping sections. By mean of a reboiler located in
the bottom of the column, the liquid feed is vaporized. The vapor ascends within
the column and contacts with the descending liquid. The plate or the packing in
the column allows for a thorough contact of the vapor and liquid. The reminder
of the bottom liquid is withdrawn as bottoms. Vapor reaching the top of the
column is condensed to liquid in the overhead condenser. A portion of the con-
densed liquid is returned to the column, known as a reflux liquid. The remainder
of the condensate becomes the distillate product. The reboiler vapor and reflux
liquid lead to higher-purity products and provides a much greater recovery of the
feed. Vapor and liquid phases on a given tray approach thermal equilibrium to
an extent dependent upon the efficiency of the contacting trays.

2.2. Objectives
• To examine and operate bubble cap and packed bed distillation columns
under total and finite reflux.

• To determine and compare the separation efficiencies of bubble cap and

12
packed bed columns.

2.3. Theory
The number of theoretical stages (NTS) can be calculated graphically by means of
a McCabe-Theile diagram, or numerically by step wise solution of the component
mass balances for stage compositions for the enriching and stripping sections.
Upon the calculation of NTS, we can determine the overall efficiency of the column
E0 simply from the following expression
NT S
E0 = ∗ 100, (2.1)
NA
where NA is the actual number of stages (trays or plates) to achieve a given
separation.
For packed column distillation, two simple concepts are used to analyze the
column: height equivalent to a theoretical stage (HETS) and the height of the
transfer unit (HTU), which is related to the mass transfer coefficient. HETS is
based on the number of theoretical stages (NTS) calculated above. If we know
the height of the packing Z, HETS is calculated from the following equation:
Z
HET S = (2.2)
NT S
where Z is the height of the packing in the column. This method is attractive
because it provides a direct link to well-known heuristics in the design of packed
column. For example, an HETS of 50 cm, a 10 meter packed column will be
equivalent to 20 theoretical stages. However, this approach is not theoretically
sound. The other approach uses a differential mass balance of the packed column.
The mass balance gives,
G dy = KOG a(y ∗ − y) dz. (2.3)
Upon integration, one obtains the following familiar expression for packed column
operations;
] y2
G dy
Z = ∗
,
KOG a y1 y − y
] y2
dy
= G ∗
, (2.4)
y1 y − y

where Z is the height of the packing and G is a mass transfer parameter. The
integral maybe evaluated graphically or numerically. Graphically, by calculating
the area under the plot y vs. (y ∗ − y)−1 , where y is the mole fraction at this stage
and y ∗ is the ”equilibrium” mole fraction at this stage.

13
2.4. Procedure
Main equipment is shown on figure 2.2. Beside we need a stopwatch, sampling
bottles, beaker and thermometer. The outline of the experiment steps are given
next.

Start-up (Atmospheric Operation)


1. Ensure that the concentration of feed in the reboiler vessel is correct and
that the liquid level is at the vessel equator (25L of a solution).
- Complete valve check list.
- Set-up for a bubble cap column (By closing V13 and V12 ).

2. Set column to total reflux condition (Check reflux control valve RCV.1 is
closed).
- Start-up cooling water circuit:
- Open slowly, FCV.2 to prevent a pressure surge to cooling system.
- Don’t allow the water pressure to exceed 2.7 bar maximum as indicated
by PI.2

3. Start-up heating circuit:


- Open slowly PCV.4, to prevent a sudden surge of steam condensate to the
reboiler.
- Do not close V.11 until a steady flow of steam issues from condensate
drain.
- Ensure that the steam-trap drain hose is safely positioned.

4. Set the reboiler temperature, to approximately 90 C.


- Keep the return line of the product distillate to the reboiler vessel open
(open V.2 , close V.3 ).

Sampling and Readings


1. Allow equilibrium to be established and record the values of temperature,
flow rate, etc. as given in the log sheet.

2. Collect a sample from the distillate by opening the sampling valve; then
determine the refractive index of the sample taken

3. Adjust the reflex control valve, RCV.1 to obtain the desired reflex ratio,
which is the ratio of rotameter (RI.1A and RI.1B) scale readings, (i.e. the
scale reading RI.1A / scale reading RI.1B) = Reflux Ratio, to set reflux

14
ratio, slowly open reflux control valve RCV.1 to obtain a distillate product
flow through RI.1A. Monitor the ratio RI.1A : RI.1B.

4. Record the value of temperature indicators, flow meters, reflux indicators,


etc. as given in the log sheet.

5. Collect a sample from distillate as you did before, then determine it’s re-
fractive index. Read the composition from the chart in figure 2.3.

6. Measure the flow rate of distillate:


- Close V2, and start timing.
- When the distillate approach the top graduation , stop timing.
- Open V2.

7. Measure the flow rate of steam condensate.

Set-up for the packed column


1. Ensure that the cooling water is passing through a packed-column overhead
condenser.
- Set the reflux flow valve to the packed column.
- Open V13, and close V12.

2. Repeat the steps in the sampling and readings section §2.4.

2.5. Practice Questions


(1) What are the advantages and disadvantages of the bubble-cap and packed
columns?

(2) What is the different between the overall and plate efficiency parameters?

(3) What are the measures you should consider if you have a cold feed?

(4) Name four different commercial packed bed column’s packings?

(6) Why a 100% separation of Water-Ethanol system is impossible to achieve


using only distillation? What is the name of the phenomenon associated
with the Water-Ethanol system at higher ethanol liquid composition?

(7) Distillation columns exhibit different behavior at different vapor-liquid flow


rates. List 4 different phenomena happened during distillation column op-
eration at different vapor and liquid flows.

15
(8) A saturated liquid solution of 55wt% ethanol and 45 wt% water is fed into a
distillation column to give a distillate containing 87 wt% of ethanol and a
bottom containing 3 wt% ethanol. The feed rate is 500 kg/h. If the molal
overflow is variable, estimate the following:

(i) Minimum reflux, Rm and Minimum rectifying ∆Rm and Stripping ∆Rm oper-
ating points

(ii) Minimum number of stages Nm .

(iii) The number of stages for a reflux equals 1.85 and the location of the feed
plate

(vi) The Condenser duty, Qc , kW and Reboiler duty, QR , kW

(v) If you assume a constant molal overflow, estimate minimum reflux and
number of minimum stages.

(vi) If you assume a constant molal overflow, determine the number of stages
for RD = 1.75Rm , using the new minimum reflux found in part (v) for
superheated feed (q = −1.0).

(vii) Write down the three operating lines mathematical equations.

(viii) Is a 100% wt Ethanol is possible to be obtained ? Explain your an-


swer.Suggest a solution to this problem

The enthalpy and equilibrium charts are provided

2.6. Report
You are expected to suggest answers to the practice questions in your report.
Your answers may be included in the discussion. In your report, the following
calculations MUST be reported and discussed:

• Calculate the number of theoretical stages (NTS) in the column using the
McCabe-Thiele method.

• Determine the height equivalent to a theoretical stage (HETS) in the packed


column.

• Evaluate the mass transfer coefficient G .

16
• Estimate the overall plate efficiency (E0 ) and Murphree plate efficiency
(EM ).

• Calculate the heat loss from the distillation column.

References
J. M. Coulson, J. F. Rihardson, J. R. Backhurst, and J. H. Harker. Particle Tech-
nology and Separation Processes, volume 2 of Chemical Engineering. Pergamon,
Oxford, 4th edition, 1991.

C. J. Geankoplis. Transport Processes and Unit Operations. McGraw Hill, New


York, 3rd edition, 1993.

W. L. McCabe, J. C. Smith, and P. Harriott. Unit Operations of Chemical Engi-


neering. McGraw-Hill, 5th edition, 1993.

P. C. Wankat. Equilibrium Staged Separations. Elsevier, New York, 1988.

17
Figure 2.1: Schematic diagram of a distillation column.

18
Figure 2.2: Refractive Index versus Mol% of Methanol in Water.

19
Figure 2.3: Flow diagram of combined bubble-cap and packed distillation column.
20
3. Srolg-Lltxlg E{wudfwlrq (Lhdfklqj)

3.1. Background
Leaching is one of many solid-fluid separation processes that are carried out in
the chemical, mineral and related industries. In fact, it is one of the oldest unit
operations in the chemical industries. The fundamental principle behind leaching
is the removal of a soluble material from an insoluble, permeable solid phase. The
soluble fraction, solid or liquid, may exist mechanically in the pore structure of
the insoluble material or chemically combined with that material. This soluble
material is removed through dissolution in a dissolving solvent. The most familiar
example of leaching is the extraction of tea and coffee, and most importantly
mineral recovery.
The rate of leaching (extraction) is affected by many physical and chemical
phenomena. Mass transfer and equilibrium phenomena obviously play major roles.
The process of leaching consists of the following steps: (i) The solvent diffuses into
the solid phase; (ii) The diffused solvent dissolves the solutes (i.e. transfer the
solute to the liquid phase). Leaching is always followed by solvent recovery, which
involves another mass transfer operation; such as filtration. Block diagram of
leaching and solvent recovery is shown in figure 3.1.

3.2. Objectives
• To examine leaching operation.

• To demonstrate solid extraction using upward and/or downward flow of the


solvent.

3.3. Theory
The model equations for the system described in this experiment are obtained from
simple unsteady solute mass balances around the leaching and reboiler vessels;

21
assuming no solute exists in the stream leaving the leaching vessel.
dCL
−CL Q = VL , and (3.1)
dt
dCB
CL Q = VB , (3.2)
dt
where Q is the solvent flow rate, V is the fluid volume and C is the solid con-
centration; the subscripts L and B refer to the leaching and boiler vessels. K.
Solving these equations simultaneously should lead to

CL = CL0 exp(−Q/VL t), (3.3)


CL0 VL
CB = [1 − exp(−Q/VL t)] , (3.4)
VB
fromk equation l3.4 we can easily evaluate the rate constant Q/VL if we plot
− ln 1 − CCL0
B VB
VL
vs. time. This rate constant can be viewed as an empirical mass
transfer coefficient.

3.4. Procedure
Start-up
1. Weigh out the appropriate quantity of solids into the fibre bag (typically 4
kg)

2. Carefully remove the solvent feed line and the vent line fitted to the extrac-
tion vessel cover.

3. Undo the vessel-cover retaining clips and remove the cover to the ground
level.

4. Place the fibre bag containing the solids into the extraction vessel, ensure
that the top of the bag is closed for upward flow (a suitable weight should
be placed on top of the bag to keep it closed).

5. Replace the vessel cover and hand-tighten the securing clips.

6. Replace the vent and solvent feed lines; Ensure that the solvent feed line
below the distillate cooler is firmly attached to the bottom of the extraction
vessel.

7. Close V.5.

22
8. Open the cooling water line through the condenser and distillate cooler by
opening and closing respective valves.
9. Set the steam on to the reboiler, ensure that the steam pressure nearly
0.0 bar. Please, consult your technician before opening the steam to the
reboiler.

Experiment
1. Fifteen minutes after solvent has begun to pass through the product cooler,
measure the flow rate, as follows:
- Set the equipment for return of solvent to reboiler section. Keep valve V.5
in open position.
- Close valve V.5 and when the solvent reaches the bottom mark on FI.1
begin timing (the interval at which the solvent reaches the top mark of FI.1).
- Adjust the heat input to give a flow rate of approximately 500 ml/min.
- Repeat the measurement of flow rate till it comes to the steady state.
2. When a steady valve for FI.1 has been determined, record its value and also
record the reboiler temperature (TI.1). Record as well the steam pressure
to the reboiler.
3. Carefully take a sample from the reboiler, by :
- Opening sampling valve V.2 and remove sample.
- Close V.2 when sample is removed.
4. Close valves V.5 and V.7 and begin solvent transfer to the extraction vessel.
5. Take sample of first effluent, as follows:
- Close stop valve V.8.
- Carefully open sampling valves V.3 and remove sample.
- Close sampling valve V.3.
- Open stop valve V.8.
6. Record the collection of this sample as t = 0 .
7. Record the temperature indicated by TI.2 (solvent temperature in extraction
chamber).
8. Samples of reboiler contents and effluent should be taken every 2 minutes
for the first 10 minutes and then every 5 minutes until 60 minutes have been
reached.
9. Record the final temperature indicated by TI.1 and TI.2.

23
10. Open valve V.7.

11. Shut down as instructed by the technician.

12. Record the final volume in the reboiler to check the loss of solvent.

13. Determine the refractive index for each of the sample drawn.

3.5. Practice Questions


(1) Is the leaching process described in this experiment, batch, semi-batch or
continuous? Justify your answer.

(2) How do you expect leaching rate to vary with solid pore size, i.e. the area of
contact?

(3) What are some of the properties you would look for in a good solvent?

(4) What is the opposite of leaching?

(5) Give one example for the use of leaching process in Kuwait.

(6) Explain briefly why the effluent refractive index decreases during the course
of the experiment but the refractive index of the reboiler contents increase.

(7) A continuous countercurrent leaching process is used to extract a rose water


oil from a rose petals using ether as solvent. 558 kg/hr of feed stream (that
contains 38 kg oil, 95 kg ether and the rest is inert). The feed stream is
treated with 340 kg/hr of FRESH ether. The leached solid contains 5 kg of
rose oil and the flower petals (inert solid) per solution ratio is 1.67.

(1) Calculate the amounts of the stream leaving the process.


(2) Calculate the number of stages using McCabe-Theile method using the
( y vs. x) chart.
(3)Calculate the number of stages required for the leaching of rose oil using
the (N vs. x, y)

3.6. Report
You are expected to suggest answers to the practice questions in your report. Your
answers can be included in the introduction and/or discussion. In your reports,
the following calculations MUST be reported and discussed:

24
• Plot the graphs of: (a) refractive index of reboiler contents vs. time and (b)
refractive index of effluent vs time.

• Use the calibration graph to convert the data for the refractive index of efflu-
ent to effluent composition (kg solute / kg solvent). (Alternatively estimate
the composition by calculation).

• Estimate the amount of solute extracted during the course of the experiment
using the effluent composition vs. time plot. Compare it to the change in
weight of solid change before and after the extraction process.

• Using the final refractive index and corrected volume for the reboiler con-
tents, calculate the amount of solute extracted.

• Determine the empirical mass transfer coefficient using equation 3.4.

• Derive and solve equations 3.1 and 3.2.

References
J. M. Coulson, J. F. Rihardson, J. R. Backhurst, and J. H. Harker. Particle Tech-
nology and Separation Processes, volume 2 of Chemical Engineering. Pergamon,
Oxford, 4th edition, 1991.

C. J. Geankoplis. Transport Processes and Unit Operations. McGraw Hill, New


York, 3rd edition, 1993.

W. L. McCabe, J. C. Smith, and P . Harriott. Unit Operations of Chemical


Engineering. McGraw-Hill, 5th edition, 1993.

P. C. Wankat. Equilibrium Staged Separations. Elsevier, New York, 1988.

25
Figure 3.1: Block diagram of solid-liquid extraction and solvent recovery.

26
Figure 3.2: Flow diagram of leaching unit.

27
4. SPRAY DRYING

4.1. Background
Drying generally refers to the removal of a liquid from a solid by evaporation, in
other words, dryers produce a dry solid from a wet feed. Drying equipments are
classified based on the method of heat transfer to the wet material and the type
of the material itself. In general, there are direct and indirect dryers. One type
of direct drying is spray drying, the subject of this experiment. Spray drying is
suitable when the feed is in liquid state, slurry, or paste capable of being dispersed
in a liquidlike spray. The main application of spray dryers is for ordinary drying
of aqueous solutions and slurries, especially in food industry.. In practice, there
are three fundamental steps in spry drying process: (1) liquid atomization, (2) hot
gas-droplet contact, and (3) liquid evaporating from droplets. The evaporation
rate of the liquid from the droplet critically depends on the size of the droplet.
The droplets formed by most industrial atomizers are 2-500μm in size. The largest
droplet rarely exceeds 500μm. For efficient drying, the hot gas should be thourouly
mixed with the droplets to be dried.

4.2. Theory
There is no single theory of drying that explains the drying process regardless
of the materials or the dryer types. covers all materials and dryer types. Solids
drying goes through two main time zones: constant rate period, and falling rate
period and. During the constat rate period, moisture vaporize into the stream
and the controlling factor is the transfer coefficient for diffusion across the gas
film. In the falling rate periods, the surface is no longer wetted and the rate of
drying falls. The movement of water is proportional to a concentration gradient
between the moisture content and the water content in the drying gas.
In spry drying, a large interfacial area is produced by mean of atomizer. Con-
sequently, a high rate of evaporation is obtained. The amount of drying a drop
largely depends upon the evaporation rate and the contact time, which depends
on the velocity of the fall and the length of path through the dryer. When the
drop is first ejected from the atomizer, its initial velocity relative to the surround-

28
ing gas is high hence high rate of evaporation is achieved.. However, the drop
decelerates to its terminal velocity, therefore, the large portion of mass transfer
occurs during the free-fall period. For a pure liquid drop, Marshall suggested the
following relation for evaporation time
(d20 − d2t )
t∝ (4.1)
∆T
Since most drops contains solids in suspension of solution, as in our case, it is
found that evaporation initially proceeds in accordance to the above equation for
pure liquid. Once the solids deposition starts, a solid film is rapidly formed which
increase the resistance of water transfer.

4.3. Objectives
• To be acquainted with spray drying operation.
• To determine the efficiency of the drying equipment

4.4. Procedure
Please make sure before starting that YOU HAVE YOUR SAFETY GLASSES
AND HEAT RESISTANT GLOVES ON. Then proceed with the experimental
procedure safely.

1. Switch the system on with the blower and heater under a specified condition.
2. Prepare about 1 liter of the solution for drying.
3. Determine the flow rate of the feed pump for a particular speed using mea-
suring cylinder and stopwatch.
4. Record surrounding air temperatures (wet bulb and dry bulb temperatures).
5. Switch on the air compressor to the atomizer.
6. Wait until the inlet temperature reaches the set point and check both the
inlet and outlet temperatures to be constants.
7. Insert distilled water through the feed pump till the inlet and outlet tem-
peratures are constants.
8. Introduce the solution to the atomizer and observe the phase of atomization.
Start the stopwatch and record the temperatures every 5 minutes.

29
9. After 20 minutes, stop the pump and weigh the collected powder.

10. Repeat the experiment for another two flow rates of the feed.

11. Once you finish your experiments, introduce again distilled water before
shutting down the equipment.

12. Wait for cooling down, then switch off the pump, heater, blower and com-
pressor. At the end, switch off the main.

13. Clean the parts with water.

4.5. Practice Questions


(1) What are the differences between the wet bulb and dry bulb temperatures?
How are they measured?

(2) If an average person of 70 kg was totally dried, for instance an Egyptian


mummy!, estimate the final weight. Hint, estimate the water percentage in
the human body.

(3) Why dried food doesn’t rot faster than raw food?, explain in scientific terms.

(4) What is the opposite of drying operations in the chemical processes?

(5) What is the role of the atomizer in the spray dryer?

(6) Air at 75o F and 70% humidity is cooled to 50o F at a constant pressure of
1 atm, The heat capacity of water is 4.186 J/g.o C. Use the psychometric
chart to calculate

• (a) The fraction of water that condenses


• (b) The rate at which heat must be removed to deliver 1000 ft3 /min of
humid air at the final condition.

4.6. Report
You are expected to suggest answers to the practice questions in your report.
Your answers can be included in the discussion. In your reports, the following
calculations MUST be reported and discussed:

• Determine the overall evaporative efficiency and the collection efficiency.

30
• Calculate overall mass losses.

• Do rigorous overall material and energy balances.

References
D. Perry and R. H. Green. Perry’s Chemical Engineers’ Handbook. McGraw-Hill,
6th edition, 1984.

C. J. Geankoplis. Transport Processes and Unit Operations. McGraw Hill, New


York, 3rd edition, 1993.

W. L. McCabe, J. C. Smith, and P . Harriott. Unit Operations of Chemical


Engineering. McGraw-Hill, 5th edition, 1993.

K. Masters. Spray Drying Handbook. 4th edition, 1985.

R. E. Treybal. Mass-Transfer Operations. McGraw Hill, New York, 3rd edition,


1980.

31
Figure 4.1: Spray Drying Equipment.

32
5. Fl{hg dqg Foxlgl}hg ehg

5.1. Background
The concept of fluidization is best visualized by reference to a simple experiment..
Consider a bed of particles supported by a perforated place in a vertical tube.
Further, consider that fluid is forced upward through the bed of particles and
that the particles have a density greater than that of the fluid. A pressure drop
is obviously necessary to cause the fluid to flow through the bed and when the
upward pressure force on the bed becomes equal to the net weight of the bed
acting ”incipient fluidization”. However, unless the particles agglomerate, the
bed does not lift as a unit but rather expands to give an increased porosity. If
the fluid flow rate is continuously increased the bed continues to expand until in
the limit the upward fluid velocity becomes equal to the terminal falling velocity
of the particles and the particles are carried out of the tube. Between the limits
of incipient fluidization and particle carry-over, the bed is usually reasonably well
defined and, because of the appreciable circulation of particles within the bed, the
bed is said to be ”fluidized”.
Obviously, the fluidized bed provides an excellent means to bring fluid and
solid into intimate contact. Applications fall into two categories: chemical reac-
tions (e.g., the catalytic cracking of hydrocarbons) and physical processes (e.g.,
the heating and drying of particulate solids). Despite the advantages of fluidized
beds outline above, fluidized systems do have certain disadvantages which may
prevent the use of fluidized beds for some applications. For example, it is diffi-
cult to fluidize a bed of particles which agglomerate and it is sometimes difficult
to maintain uniform fluidization in large diameter beds where channelling often
results, in the absence of baffles. Furthermore, particle attrition may be an over-
riding disadvantage.

5.2. Objectives
• Determine the pressure drop through a fixed and fluidized bed.

• Verify Carman-Kozeny equation.

33
• Observe the onset of fluidization..

5.3. Theory
To determine the pressure drop through a fixed bed we can show that the Carman-
Kozeny can be expressed in the form
  3
∆P DP 1−
2 = 150 + 1.75, (5.1)
L ρ (Vsm ) 1 − Re

where

Vsm : Superficial velocity, m/s

Dp : Size of the particles (μm)

L : Height of the bed (m)

Re : Renolds Number

: The bed voidage,


mass of particles
=1−
particles density * Total bed volume

If the flow rate is measured in liters/second, and Vsm is the superficial velocity
m/s, then
Q ∗ 10−3
Vsm =
A
where A is the cross-sectional area.
The pressure drop at fluidization can be predicted by using the equation,
 
∆P = L(1 − )g ρs − ρf

where

ρs : The density of solid

ρf :The density of the fluid

34
Another important process variable in fluidized bed is the minimum fluidizing
velocity. It is frequently used in fluid-bed calculations and in quantifying one
of the particle properties.. This parameter is best estimated using Baeyens and
Gelard correlation
0.0076(ρs − ρf )0.934 d1.8
Umf =
μ0.87 ρ0.006
f

where

d : The size of the particle, m

μf :The viscosity of the fluid

5.4. Procedure
Study the attached schematic diagram, figure 7.2 for the equipment setup. Follow
the procedure in the laboratory and prepare your own data sheet. If you have
any problem, please check with your lab instructor. You will be asked to perform
the experiment for two types of fluid: water and air. To perform the experiment,
check that the manometer reads zero, if it does not, adjust the level accordingly.
Switch on water pump. Adjust water flow rate in increments of 0.1 l/min. read
the height of the bed, manometer reading, and the state of the bed. In case of
air, adjust the air flow control valve to give a flow rate of 2.0 l/min. Increase flow
rate by 1.0 l/min. Report your data in the data sheet.

5.5. Practice Questions


(1) In your car, there is a fluidized bed tubular reactor for the oxidation of NO
to NO2 , what is this equipment is called? and what is its main purpose?

(2) What do you expect to happen if the flow rate under a fluidized bed in very
large? What if the flow is really small?

(3) In gas reactor, catalytic fluidized bed are very often been used, explain.

(4) What factors influence the pressure drop in a fluidized bed?

(5) Describe a Fixed-Bed adsorption column.

(6) Explain the advantages of fluidization in chemical processes.

35
(7) A waste stream of alcohol vapor in air from a process was adsorbed by
activated carbon particles in a packed bed having a diameter of 4 cm and
length of 14 cm containing 79.2 g of carbon. The inlet gas stream having
a concentration (c0 ) of 1500 ppm and a density of 0.00225 g/cm3 entered
the bed at a flow rate of 800 cm3 /s. The break-point concentration is set at
c/c0 = 0.01 and the breakthrough curve is given.

(a) Determine the length of the unused bed.

(b) Determine the saturation loading capacity of the carbon.?

5.6. Report
• Draw a graph of bed pressure drop against air flow rate from the experi-
mental data obtained.

• Compare the predicted fluidization point with the actual fluidization point
obtained from the graph

• Give reasons for any differences between the two values.

• Calculate the minimum fluidizing Velocity

References
D. Perry and R. H. Green. Perry’s Chemical Engineers’ Handbook. McGraw-Hill,
6th edition, 1984.

C. J. Geankoplis. Transport Processes and Unit Operations. McGraw Hill, New


York, 3rd edition, 1993.

W. L. McCabe, J. C. Smith, and P . Harriott. Unit Operations of Chemical


Engineering. McGraw-Hill, 5th edition, 1993.

36
Figure of the fluidised bed expirement.

37
Schematic drawing of the fluidised bed equipment.

38
Water and Air properies.

39
6. DOUBLE EFFECT EVAPORATOR

6.1. Background
Evaporation process is one of the major operations to concentrate aqueous solu-
tions. It is based on the removal of water from a solution by boiling the solution in
a vessel, which is called evaporator. If the solution contains dissolved solids, the
resulting evaporated solution may become saturated. There are three major types
of solutions: (1) Those that can be heated to high temperature without decom-
position as opposed to one decomposes at low temperature; (2) Those that yield
different crystal sizes of solid; (3) Those that boils at the same boiling temperature
of water as opposed to a higher boiling temperature.
Evaporation occurs when heat is added to the solution to vaporize the solvent
(more volatile component). The supplied heat is to provide the latent heat of
vaporization. Evaporation can be carried out in one step (one effect) or in more
stages (multi-effect). The use of more than a single evaporator is related to the
economy of heat utilization. For example, in a single effect evaporator, large
quantities of heat are wasted because the latent heat in the vapor leaving the
boiling liquor is simply lost to the cooling water in the condenser. It would be
more efficient if the hot vapor leaving the first evaporator to be utilized to heat
liquid in a second evaporator. In a double effect system, vapor from the first
effect loses its heat to the liquor in the second effect. The major variable used
industrially to control the efficient operation of a double effect evaporator, is the
heat input to the first effect.

6.2. Objectives
• Investigate the effect of variation in steam pressure on the capacity of a
double effect evaporator.

• Calculate the economy of a double effect evaporator operating at vacuum


pressure.

40
6.3. Theory
Evaporator capacity is determined from the material balance equation. It is to be
noted that the capacity is proportional to the rate of heat transfer, Q, through
the heating surface of the evaporator
Q
= U ∆T,
A
where U is the overall heat transfer coefficient, W/m2 K, A is the heat transfer
surface, m2 , and ∆T is the overall temperature driving force, C.
The evaporator economy may be determined by heat balance assuming that
heat losses are negligible and heat the condensate leaves the heat exchanger at
steam temperature. For the double effect evaporator in figure 6.1. The steam
economy is given by:
Mtot
E= ,
M0
where Mtot is the total evaporation flow rate and M0 is the input steam flow rate
into the first evaporator. For example in figure 6.1, the steam economy is
D1 + D2 + D3
E= .
D0

6.4. Procedure
Follow the procedure in the laboratory and prepare the data sheet.

6.5. Practice Questions


(1) What is the major possible application of multi-effect evaporator in Kuwait?

(2) Name two products from your grocery store that use evaporation process?
Hint: one product is diary product, name it, the other is used as sweet.

(3) What are the differences between evaporation and distillation?

(4) If you can build an infinite number of evaporators, what is the efficiency of
the process? Why is it impossible to have this efficiency?

41
6.6. Report
• Briefly describe the experiment in your own words.

• Do energy balance around first and second evaporators.

• Determine the capacity of each effect and the overall capacity at each steam
pressure.

• Calculate the heat removed in the condenser Qc for each steam pressure and
illustrate results on a graph.

• Calculate the economy of each effect and the overall value for double effect
operation. Which of the systems has the best economy and why?

• Construct a heat balance over the two effects and for each steam supply
pressure calculate the heat loss QL for each effect. Draw a graph of steam
supply pressure against heat loss for each of the two effects. Explain how
QL should vary with steam pressure and compare this with your graph.

• Calculate the overall heat transfer coefficient U for each effect, given that
the heat transfer area of the boiler is 0.5 m2 .

References
J. M. Coulson, J. F. Rihardson, J. R. Backhurst, and J. H. Harker. Particle Tech-
nology and Separation Processes, volume 2 of Chemical Engineering. Pergamon,
Oxford, 4th edition, 1991.

W. L. McCabe, J. C. Smith, and P . Harriott. Unit Operations of Chemical


Engineering. McGraw-Hill, 5th edition, 1993.

D. Perry and R. H. Green. Perry’s Chemical Engineers’ Handbook. McGraw-


Hill, 6th edition, 1984.

42
Figure 6.1: Schematic diagram of multiple effect evaporator.

43
Figure 6.2: Double effect evaporator expiremntal setup.

44
7. TUBULAR REACTOR

7.1. Background
There three major types of reactors in the chemical industries: Batch, continuous
stirred tank reactor (CSTR), and plug flow reaction (PFR) also known as tubular
reactor. It consists of cylindrical pipe and is normally operated at steady state.
For the purpose of the material presented here, we consider systems in which
the flow is highly turbulent and the flow field can be modeled as plug flow, i.e.
there is no radial distribution of velocity. In the tubular reactor, the reactants
are consumed as they flow down the pipe. In practice, tubular reactors can be
a single continuous tube or several tubes in parallel. The use of tubular reactor
is favorable when the back mixing of reaction mixture is not important. The
heat transfer to or from the reactor may be accomplished by means of a jacket
or shell-and-tube. Also the reactor can be packed with catalyst pellets or inert
solids.

7.2. Objectives
• Recognize plug flow reactor in practice.

• Determine the variation of conversion with respect to the reactor’s residence


time.

7.3. Theory
For a tubular plug flow reactor, shown in figure 7.1, mass balance for a particular
reactant A is ] CAi
dCA V
= = τ, (7.1)
CA0 rA Q
where CAi and CA0 (mole/litre) are the inlet and outlet concentrations of A re-
spectively, and rA is the reaction rate of A in moles/seconds, V is the reactor
volume and Q is the total volumetric flow rate. For the reaction between ethyl
acetate and caustic soda, it is equi-molar and is second order in nature, thus

45
rA = k CA CB , (7.2)
where A is NaOH and B is CH3 COOC2 H5 and k is the reaction rate constant. It
is algebraically simpler if it is arranged for the initial concentrations in the mixed
feed stream of A and B to be equal,
FA CAF FB CBF
= = CAi = CBi (7.3)
FA + FB FA + FB
where CAF and CBF are concentrations in the feed tanks of NaOH and CH3 COOC2 H5
respectively, and FA and FB are the individual feed flow rates (ml/min). The con-
version is defined as
CAi − CA0
X= (7.4)
CAi
Then equation can be solved to become
X
= k τ CAi (7.5)
1−X
Thus the conversion factor X/(1 − X) should be directly proportional to the
residence time, τ , provided k is kept constant (i.e. at constant temperature) for
this reaction

7.4. Procedure
Study the attached schematic diagram, figure 7.2 for the equipment setup. Follow
the procedure in the laboratory and prepare your own data sheet, please check
with your lab instructor.

7.5. Practice Questions


(1) In your car, there is a very important tubular reactor for the oxidation of NO
to NO2 , what is this equipment is called? and what is its main purpose?

(2) Why is it essential that the flow in the tubular reactor to be turbulent?

(3) What is back mixing? and what are the reactors that have back mixing?

(4) What is the conversion if the reactor is CSTR? Show detailed calculations.

46
7.6. Report
• Consider 0.4 litre as the reactor volume, calculate conversion and plot it
against X/(1 − X). Comment on the graph calculated.

• Consider that the reaction rate is second order, derive equation 7.5.

• How do you prove that a reaction is first order?[?][?]

References
H.S. Fogler. Elements of Chemical Reaction Engineering. PTR Prentice Hall, 2nd
edition, 1992.

K.B. Froment, G.F. ; Bischoff. Chemical Reactor Analysis and Design. Wiley,
2nd edition, 1990.

D. Perry and R. H. Green. Perry’s Chemical Engineers’ Handbook. McGraw-


Hill, 6th edition, 1984.

47
Figure 7.1: Differential mass balance of tubular reactor.

48
Figure 7.2: Schematic diagram of tubular reactor.

49
8. Wulwlqj d Frupdo Thfkqlfdo Rhsruw

50
9. Sdpsoh Rhsruw

51