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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.

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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

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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

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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,

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y1 φ1 P = γ 1 x1 P1∗ . (1. (1.3) since the total mass is conserved. most mixtures are not ideal. in an ideal mixture of components 1 and 2. vaporization and condensation of the two components will proceed until equilibrium between the vapor and the liquid is attained.2. This equilibrium depends on temperature and the total pressure of the vessel.1 and 1. xi is the liquid mole fraction of component i at equilibrium. (1. Using equations 1. This can be done by introducing the activity coefficients γ in the liquid phase and the fugacity coefficient in the vapor phase φ.2) Where: Pi is partial pressure of component i at a fixed temperature. (1. Pi∗ is the vapor pressure of component i at a given temperature. The activity coefficient of a component in a mixture is a function 6 .1) P2 = x2 P2∗ .8) For simplicity we will assume that the vapor phase is ideal hence the fugacity coefficients are 1. the partial pressure of a component is given by. where the pro- portionality constant is the vapor pressure of that component.5 and 1. According to Roult’s law.4) In the vapor phase.6) In practice.5) y2 P = x2 P2∗ . (1. therefore. Pi = yi P . If the tempera- ture of this mixture is maintained constant. where yi is the vapor mole fraction of component i. the partial pressure exerted by each components is proportional to its mole fraction. The total pressure P according to Dalton’s law of partial pressures is given by P = P1 + P2 . = x1 P1∗ + x2 P2∗ . The pressure exerted by each component will depend on the composition of the mixture and the saturated vapor pressure of each component.6 should be modified. x1 +x2 = 1. (1.vaporization of both components will occur until the pressure of the vapor attains a steady state corresponding to the bubble point of the mixture. Mathematically expresses as. P1 = x1 P1∗ . equations 1. y1 P = x1 P1∗ . (1. The total pressure can be expressed as P = x1 P1∗ + (1 − x1 )P2∗ .7) y2 φ2 P = γ 2 x2 P2∗ . (1.

which equilibrates with the vapor. shown in figure 1. striking the thermocouple pocket C that contains a thermocouple to measure the boiling temperature. a sample of the vapor phase is taken from tap M and a sample of the liquid phase is taken from tap N.. Experimental steps Pleas make sure that THE SAFETY SHIELD MUST ALWAYS BE IN PLACE BEFORE THE EXPERIMENT COMMENCES.5 hours to ensure that the equilibrium is attained. and the mixtures emerge from the tube at equilibrium. The liquid formed accumulates in the receiver J from which a sample of the vapor phase is obtained. Prepare 350 ml of the mixture (provided by your lab instructores). The vapor then rises gently through the central tube E while the liquid drops fall back into chamber F. 7 . 2. A fresh mixture of different composition is then charged and the experiment is repeated.1.4. This concludes the experiment with this specific mixture and the contents of the still are therefore drained through drain cock Q. 1. pressure and composition. Procedure Apparatus The apparatus. Thus. When the equilibrium is attained between the liquid and the vapor phases. The contents of the still are recirculated in this manner for about 1. Remove access panel from base of safety case. Follow the steps of the experiment carefully.of temperature. Often. it is calculated from the vapor-liquid equilibria data at specified conditions. 1. 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. 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 rising vapor entrains drops of the liquid. 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. 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. it has to be determined from experiments.

(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.5 hours. After 45 minute. Adjust the still heater control so that only 20 drops per minute fall from the base of the condenser into the distillate receiver J. Do not drain the receiver J. 7. Once boiling starts. Switch on the still heater to boil the liquid. 6. Transfer the prepared mixture into equilibrium still until the mixture covers the coil B and is above the thermocouple C. 8. 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. 10. 11. 4. Continue the boiling process for at least 1.5 hours. switch off the equipment then take another set of samples as in step 11. ensure that the jacket is switched off. 9. explain using phase equilibrium thermodynamics. 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. 5. Replace the vapor trap H and turn on the cooling water ensuring that there is a rapid flow of water through the condenser. 1.5 C higher than the still’s temperature.5. 12. (3) How do you make sure that the solution. Practice Questions (1) A pressurized pot always cook the food faster than a regular (non-pressurized) pot. Replace access panel. Monitor the still and jacket temperatures every 15 minutes and adjust the still and jacket heater controls as required. reach steady state (equilibrium)? (4) Name four non-ideal binary systems and specify if the system is positively or negatively deviated from ideality. in your experiment. After 1. 3. slowly adjust the jacket heater control until the ther- mocouple in the jacket indicate 2 . 8 .

(5) How do your results change if the fugacity of the vapor is considered? (6) ”According to the phase rule.9) Note: you have to derive the activity coefficients from the excess energy before you determine the constants. • Using the experimentally determined activity coefficients. Report You are expected to suggest answers to the practice questions in your report. The equilibrium data of the solution is shown in the table.” Explain this statement. (7) A Water/Ethanol solution is in equilibrium at 760 mmHg and 80o C.506 7. the compositions of a two-phase binary solution are predetermined if the pressure and temperature are both fixed.6. evaluate the pa- rameters A and B in the 3-suffix Margules equation. γ of Water and Ethanol? 1.7 and 1.320 8.8. Some of your answers can be used in the introduction and/or discussion. g E = x1 x2 [A + B(x1 − x2 )] (1.97 1668 228 Use Antoine equation to calculate the vapor pressures (in mmHg) and Tem- perature (o C) in of the components. • Find the activity coefficient experimentally using equations 1. Material xi yi Ai Bi Ci Water 0.16 1623 229 Ethanol 0. 9 . In your reports. (2) The activity coeffi- cients. the following calculations MUST be reported and discussed: • Find the composition from the refractive index using the calibration curve. Bi log Pi∗ = Ai − T + Ci Calculate: (1) The K-values of Water and Ethanol?. If you are given the excess free energy of the model.

M. McGraw-Hill. 1987. B. Thermodynamics. K.10) (1 + Ax1 /Bx2 )2 B ln γ 2 = (1. 3rd edition. Prentice Hall.11. Van ness. McGraw-Hill. 10 . M. Chemical and Process Thermodynamics. Prentice- Hall. 4th edition. Kyle. C. 2nd edi- tion. • Determine the Van-Laar Equation parameters A and B using the activity coefficients equations A ln γ 1 = (1. 1995.11) 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. Prausnitz. Molecular Thermodynamics of Fluid Phase Equilibria. 1969. Smith and J. G. Introduction to Chemical Engineering Thermo- dynamics. Pitzer. S. References H. J. 1992.

11 .1: Schematic diagram of Ellis Still.Figure 1.

not examined here. Objectives • To examine and operate bubble cap and packed bed distillation columns under total and finite reflux. known as a reflux liquid. include ballast trays and perforated (Sieve) plates. is in- troduced continuously at a midpoint in the column. Vapor reaching the top of the column is condensed to liquid in the overhead condenser. The midpoint divides the column into enriching and stripping sections. A portion of the con- densed liquid is returned to the column.2. The plate or the packing in the column allows for a thorough contact of the vapor and liquid.1. Background Distillation is one of the major operations in the chemical and petroleum indus- tries. The main purpose of a distillation column is to separate two or more volatile components. they are known as early as 1800’s. Packed columns were introduced later. the liquid feed is vaporized. The reboiler vapor and reflux liquid lead to higher-purity products and provides a much greater recovery of the feed. The use of one type over the other is governed by the objectives of the process. The remainder of the condensate becomes the distillate product. Bubble-cap columns are classical in the chemical industries. bubble-cap and packed. This experiment examines two types of distillation columns. in a liquid state.1. The vapor ascends within the column and contacts with the descending liquid. 2. The reminder of the bottom liquid is withdrawn as bottoms.2. The distillation column operates as follows. the feed. Vapor and liquid phases on a given tray approach thermal equilibrium to an extent dependent upon the efficiency of the contacting trays. By mean of a reboiler located in the bottom of the column. PACKED AND BUBBLE CAP COLUMN CONTINUOUS DISTILLATION 2. especially oil refineries. an example of a distillation column is shown in figure 2. • To determine and compare the separation efficiencies of bubble cap and 12 . Other types.

Upon the calculation of NTS. (y ∗ − y)−1 . Theory The number of theoretical stages (NTS) can be calculated graphically by means of a McCabe-Theile diagram. 13 . one obtains the following familiar expression for packed column operations.1) NA where NA is the actual number of stages (trays or plates) to achieve a given separation. KOG a y1 y − y ] y2 dy = G ∗ . by calculating the area under the plot y vs. a 10 meter packed column will be equivalent to 20 theoretical stages. The other approach uses a differential mass balance of the packed column. an HETS of 50 cm.3. Graphically. or numerically by step wise solution of the component mass balances for stage compositions for the enriching and stripping sections. However.2) NT S where Z is the height of the packing in the column. ] y2 G dy Z = ∗ .3) Upon integration. two simple concepts are used to analyze the column: height equivalent to a theoretical stage (HETS) and the height of the transfer unit (HTU).4) y1 y − y where Z is the height of the packing and G is a mass transfer parameter. The mass balance gives. (2. (2. (2. which is related to the mass transfer coefficient. where y is the mole fraction at this stage and y ∗ is the ”equilibrium” mole fraction at this stage. 2. HETS is calculated from the following equation: Z HET S = (2. G dy = KOG a(y ∗ − y) dz. packed bed columns. This method is attractive because it provides a direct link to well-known heuristics in the design of packed column. If we know the height of the packing Z. For packed column distillation. we can determine the overall efficiency of the column E0 simply from the following expression NT S E0 = ∗ 100. For example. this approach is not theoretically sound. The integral maybe evaluated graphically or numerically. HETS is based on the number of theoretical stages (NTS) calculated above.

1B) scale readings.2. Start-up heating circuit: .Set-up for a bubble cap column (By closing V13 and V12 ). Start-up (Atmospheric Operation) 1. to prevent a sudden surge of steam condensate to the reboiler. to set reflux 14 . the scale reading RI. Sampling and Readings 1.e. Allow equilibrium to be established and record the values of temperature.Open slowly. 2. Set column to total reflux condition (Check reflux control valve RCV. .11 until a steady flow of steam issues from condensate drain.Do not close V. Adjust the reflex control valve. to approximately 90 C. etc. . close V.Keep the return line of the product distillate to the reboiler vessel open (open V. FCV. Procedure Main equipment is shown on figure 2. (i.2. as given in the log sheet.Ensure that the steam-trap drain hose is safely positioned.Start-up cooling water circuit: .2 to prevent a pressure surge to cooling system.1A / scale reading RI.2 3.7 bar maximum as indicated by PI. . The outline of the experiment steps are given next.1B) = Reflux Ratio. Set the reboiler temperature. .Don’t allow the water pressure to exceed 2. RCV. Collect a sample from the distillate by opening the sampling valve. which is the ratio of rotameter (RI. then determine the refractive index of the sample taken 3.1 is closed). sampling bottles. 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). . . . 4.Open slowly PCV.2 .1 to obtain the desired reflex ratio. 2. flow rate.4.4.3 ).Complete valve check list. beaker and thermometer.1A and RI. Beside we need a stopwatch.

List 4 different phenomena happened during distillation column op- eration at different vapor and liquid flows. . Monitor the ratio RI.Close V2. Read the composition from the chart in figure 2. Collect a sample from distillate as you did before. Ensure that the cooling water is passing through a packed-column overhead condenser.1A : RI. stop timing. and close V12. then determine it’s re- fractive index.1A. 15 .Open V2. . 4. etc.1 to obtain a distillate product flow through RI. 5. 6.When the distillate approach the top graduation .4. Measure the flow rate of steam condensate. flow meters. Measure the flow rate of distillate: . . 2.Set the reflux flow valve to the packed column.5. Set-up for the packed column 1. .3. 2. ratio. reflux indicators. 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. 7. as given in the log sheet. Record the value of temperature indicators. Repeat the steps in the sampling and readings section §2.1B. slowly open reflux control valve RCV. and start timing.Open V13.

• Evaluate the mass transfer coefficient G . (iii) The number of stages for a reflux equals 1. • Determine the height equivalent to a theoretical stage (HETS) in the packed column.85 and the location of the feed plate (vi) The Condenser duty. kW (v) If you assume a constant molal overflow. Rm and Minimum rectifying ∆Rm and Stripping ∆Rm oper- ating points (ii) Minimum number of stages Nm . 16 . using the new minimum reflux found in part (v) for superheated feed (q = −1. (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. estimate the following: (i) Minimum reflux.Suggest a solution to this problem The enthalpy and equilibrium charts are provided 2.75Rm .0). the following calculations MUST be reported and discussed: • Calculate the number of theoretical stages (NTS) in the column using the McCabe-Thiele method.6. The feed rate is 500 kg/h. (vii) Write down the three operating lines mathematical equations. determine the number of stages for RD = 1. If the molal overflow is variable. kW and Reboiler duty. (viii) Is a 100% wt Ethanol is possible to be obtained ? Explain your an- swer. Report You are expected to suggest answers to the practice questions in your report. (vi) If you assume a constant molal overflow. In your report. estimate minimum reflux and number of minimum stages. Your answers may be included in the discussion. Qc . QR .

Wankat. M. New York. J. C. Oxford. J. J. Coulson. 3rd edition. Harriott. 1993. 1988. 4th edition. Rihardson. P. J. Elsevier. Geankoplis. W. Pergamon. R. volume 2 of Chemical Engineering. 5th edition. 17 . Equilibrium Staged Separations. • Estimate the overall plate efficiency (E0 ) and Murphree plate efficiency (EM ). Harker. • Calculate the heat loss from the distillation column. Transport Processes and Unit Operations. and J. New York. References J. McGraw-Hill. C. McCabe. and P. F. L. Particle Tech- nology and Separation Processes. Backhurst. 1993. Unit Operations of Chemical Engi- neering. H. McGraw Hill. 1991. Smith. C.

18 .1: Schematic diagram of a distillation column.Figure 2.

2: Refractive Index versus Mol% of Methanol in Water.Figure 2. 19 .

20 .3: Flow diagram of combined bubble-cap and packed distillation column.Figure 2.

3.2. solid or liquid. it is one of the oldest unit operations in the chemical industries. Srolg-Lltxlg E{wudfwlrq (Lhdfklqj) 3. and most importantly mineral recovery. Mass transfer and equilibrium phenomena obviously play major roles. may exist mechanically in the pore structure of the insoluble material or chemically combined with that material. 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. The process of leaching consists of the following steps: (i) The solvent diffuses into the solid phase. Objectives • To examine leaching operation. The most familiar example of leaching is the extraction of tea and coffee.3. (ii) The diffused solvent dissolves the solutes (i. transfer the solute to the liquid phase).e. mineral and related industries. • To demonstrate solid extraction using upward and/or downward flow of the solvent. 21 .1. which involves another mass transfer operation. Leaching is always followed by solvent recovery. The rate of leaching (extraction) is affected by many physical and chemical phenomena.1. The fundamental principle behind leaching is the removal of a soluble material from an insoluble. Block diagram of leaching and solvent recovery is shown in figure 3. 3. Background Leaching is one of many solid-fluid separation processes that are carried out in the chemical. such as filtration. In fact. This soluble material is removed through dissolution in a dissolving solvent. The soluble fraction. 3. permeable solid phase.

3. Solving these equations simultaneously should lead to CL = CL0 exp(−Q/VL t).assuming no solute exists in the stream leaving the leaching vessel. the subscripts L and B refer to the leaching and boiler vessels. 22 . and (3.4. Replace the vent and solvent feed lines.4 we can easily evaluate the rate constant Q/VL if we plot − ln 1 − CCL0 B VB VL vs.3) CL0 VL CB = [1 − exp(−Q/VL t)] . This rate constant can be viewed as an empirical mass transfer coefficient. 7. Ensure that the solvent feed line below the distillate cooler is firmly attached to the bottom of the extraction vessel. (3. 4. 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). Place the fibre bag containing the solids into the extraction vessel. Replace the vessel cover and hand-tighten the securing clips. K. Weigh out the appropriate quantity of solids into the fibre bag (typically 4 kg) 2.1) dt dCB CL Q = VB . Undo the vessel-cover retaining clips and remove the cover to the ground level. Close V. Carefully remove the solvent feed line and the vent line fitted to the extrac- tion vessel cover. 6. 3.5.4) VB fromk equation l3. Procedure Start-up 1. (3. (3.2) dt where Q is the solvent flow rate. dCL −CL Q = VL . 5. time. V is the fluid volume and C is the solid con- centration.

ensure that the steam pressure nearly 0. Fifteen minutes after solvent has begun to pass through the product cooler.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.Carefully open sampling valves V.2 (solvent temperature in extraction chamber). Close valves V. by : . 4.Close stop valve V. Please. 8. . Keep valve V.3. Experiment 1. Take sample of first effluent.2.Open stop valve V.2 when sample is removed. Record as well the steam pressure to the reboiler.0 bar. 9.Close sampling valve V. 23 .1).8.1 has been determined. measure the flow rate.Repeat the measurement of flow rate till it comes to the steady state. . Carefully take a sample from the reboiler.Close V. Record the collection of this sample as t = 0 . 9. .Adjust the heat input to give a flow rate of approximately 500 ml/min.2 and remove sample.1 and TI. 5. as follows: .7 and begin solvent transfer to the extraction vessel.5 in open position. Set the steam on to the reboiler.3 and remove sample. 7. as follows: . . consult your technician before opening the steam to the reboiler. 8. When a steady valve for FI.5 and V. Record the temperature indicated by TI. 2.Opening sampling valve V.Close valve V. .8. 6. . 3. . 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.1). Record the final temperature indicated by TI. Open the cooling water line through the condenser and distillate cooler by opening and closing respective valves.Set the equipment for return of solvent to reboiler section. record its value and also record the reboiler temperature (TI.

(7) A continuous countercurrent leaching process is used to extract a rose water oil from a rose petals using ether as solvent. y) 3. the following calculations MUST be reported and discussed: 24 . batch. (6) Explain briefly why the effluent refractive index decreases during the course of the experiment but the refractive index of the reboiler contents increase. The leached solid contains 5 kg of rose oil and the flower petals (inert solid) per solution ratio is 1. x) chart. 10. In your reports.67. (2) How do you expect leaching rate to vary with solid pore size. (1) Calculate the amounts of the stream leaving the process. Your answers can be included in the introduction and/or discussion. 11. Practice Questions (1) Is the leaching process described in this experiment. 558 kg/hr of feed stream (that contains 38 kg oil.e. semi-batch or continuous? Justify your answer. 95 kg ether and the rest is inert). 13. 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. Open valve V. 12. Shut down as instructed by the technician. i.7. Record the final volume in the reboiler to check the loss of solvent. Determine the refractive index for each of the sample drawn. 3.5. x. Report You are expected to suggest answers to the practice questions in your report. The feed stream is treated with 340 kg/hr of FRESH ether. (3)Calculate the number of stages required for the leaching of rose oil using the (N vs. (2) Calculate the number of stages using McCabe-Theile method using the ( y vs.

Wankat. J. calculate the amount of solute extracted. Smith. 1993. 1991. 4th edition. and J. W. 3rd edition. Particle Tech- nology and Separation Processes. Oxford. Elsevier. References J. Pergamon. Backhurst. McGraw-Hill. time plot. Harker. 5th edition. Equilibrium Staged Separations. J.2. R. Harriott. • Plot the graphs of: (a) refractive index of reboiler contents vs. and P . New York. • Derive and solve equations 3. P.4. 1993. L. F. McGraw Hill. Unit Operations of Chemical Engineering. 25 . (Alternatively estimate the composition by calculation).1 and 3. C. M. • Estimate the amount of solute extracted during the course of the experiment using the effluent composition vs. Transport Processes and Unit Operations. J. Geankoplis. McCabe. volume 2 of Chemical Engineering. • Determine the empirical mass transfer coefficient using equation 3. H. Rihardson. Coulson. C. Compare it to the change in weight of solid change before and after the extraction process. C. • Use the calibration graph to convert the data for the refractive index of efflu- ent to effluent composition (kg solute / kg solvent). J. • Using the final refractive index and corrected volume for the reboiler con- tents. New York. time and (b) refractive index of effluent vs time. 1988.

Figure 3. 26 .1: Block diagram of solid-liquid extraction and solvent recovery.

27 .Figure 3.2: Flow diagram of leaching unit.

dryers produce a dry solid from a wet feed. Con- sequently. in other words. which depends on the velocity of the fall and the length of path through the dryer. its initial velocity relative to the surround- 28 . or paste capable of being dispersed in a liquidlike spray. The movement of water is proportional to a concentration gradient between the moisture content and the water content in the drying gas. the subject of this experiment. moisture vaporize into the stream and the controlling factor is the transfer coefficient for diffusion across the gas film. slurry. For efficient drying.4. there are three fundamental steps in spry drying process: (1) liquid atomization. 4. The largest droplet rarely exceeds 500μm.2. covers all materials and dryer types. (2) hot gas-droplet contact. there are direct and indirect dryers. Solids drying goes through two main time zones: constant rate period. Spray drying is suitable when the feed is in liquid state. The amount of drying a drop largely depends upon the evaporation rate and the contact time. In spry drying. the hot gas should be thourouly mixed with the droplets to be dried. and falling rate period and.. the surface is no longer wetted and the rate of drying falls. The evaporation rate of the liquid from the droplet critically depends on the size of the droplet. and (3) liquid evaporating from droplets. SPRAY DRYING 4. One type of direct drying is spray drying. In the falling rate periods. In general. Theory There is no single theory of drying that explains the drying process regardless of the materials or the dryer types. Background Drying generally refers to the removal of a liquid from a solid by evaporation. a high rate of evaporation is obtained. The main application of spray dryers is for ordinary drying of aqueous solutions and slurries. In practice. especially in food industry. Drying equipments are classified based on the method of heat transfer to the wet material and the type of the material itself.1. a large interfacial area is produced by mean of atomizer. When the drop is first ejected from the atomizer. During the constat rate period. The droplets formed by most industrial atomizers are 2-500μm in size.

1) ∆T Since most drops contains solids in suspension of solution. 8. a solid film is rapidly formed which increase the resistance of water transfer. Procedure Please make sure before starting that YOU HAVE YOUR SAFETY GLASSES AND HEAT RESISTANT GLOVES ON. the drop decelerates to its terminal velocity.4. 5. 4. Marshall suggested the following relation for evaporation time (d20 − d2t ) t∝ (4. Introduce the solution to the atomizer and observe the phase of atomization. 29 . 7. Once the solids deposition starts.. Wait until the inlet temperature reaches the set point and check both the inlet and outlet temperatures to be constants. Switch on the air compressor to the atomizer. therefore. Insert distilled water through the feed pump till the inlet and outlet tem- peratures are constants. it is found that evaporation initially proceeds in accordance to the above equation for pure liquid. However. Determine the flow rate of the feed pump for a particular speed using mea- suring cylinder and stopwatch. For a pure liquid drop. Objectives • To be acquainted with spray drying operation. 3. Start the stopwatch and record the temperatures every 5 minutes. the large portion of mass transfer occurs during the free-fall period.ing gas is high hence high rate of evaporation is achieved. 1. Then proceed with the experimental procedure safely. • To determine the efficiency of the drying equipment 4. 6. Switch the system on with the blower and heater under a specified condition.3. 2. Prepare about 1 liter of the solution for drying. Record surrounding air temperatures (wet bulb and dry bulb temperatures). 4. as in our case.

13. Hint. introduce again distilled water before shutting down the equipment.o C. the following calculations MUST be reported and discussed: • Determine the overall evaporative efficiency and the collection efficiency. Your answers can be included in the discussion. 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. then switch off the pump. 30 . (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. switch off the main. 4.5. Once you finish your experiments. 10. 9. Repeat the experiment for another two flow rates of the feed. blower and com- pressor. estimate the water percentage in the human body. heater. Report You are expected to suggest answers to the practice questions in your report.6.186 J/g. 11. At the end. Clean the parts with water. estimate the final weight. (3) Why dried food doesn’t rot faster than raw food?. In your reports. stop the pump and weigh the collected powder. The heat capacity of water is 4. for instance an Egyptian mummy!. explain in scientific terms. After 20 minutes. 12. 4. 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. Wait for cooling down.

• Calculate overall mass losses. 1980. Perry’s Chemical Engineers’ Handbook. Perry and R. C. Unit Operations of Chemical Engineering. 3rd edition. and P . 1985. Harriott. 3rd edition. H. Smith. Transport Processes and Unit Operations. 1993. • Do rigorous overall material and energy balances. L. W. Geankoplis. 1984. Spray Drying Handbook. 5th edition. 1993. J. Treybal. K. 6th edition. New York. 4th edition. R. J. McGraw Hill. Green. McGraw-Hill. McGraw Hill. Mass-Transfer Operations. Masters. C. References D. McGraw-Hill. 31 . McCabe. New York. E.

Figure 4.1: Spray Drying Equipment. 32 .

Furthermore. 33 .g. the fluidized bed provides an excellent means to bring fluid and solid into intimate contact. For example.. Background The concept of fluidization is best visualized by reference to a simple experiment. 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. in the absence of baffles.1.. fluidized systems do have certain disadvantages which may prevent the use of fluidized beds for some applications. the catalytic cracking of hydrocarbons) and physical processes (e. the bed does not lift as a unit but rather expands to give an increased porosity. particle attrition may be an over- riding disadvantage. Further. Objectives • Determine the pressure drop through a fixed and fluidized bed. the heating and drying of particulate solids). Obviously. • Verify Carman-Kozeny equation. Consider a bed of particles supported by a perforated place in a vertical tube. Between the limits of incipient fluidization and particle carry-over.g. Fl{hg dqg Foxlgl}hg ehg 5. the bed is said to be ”fluidized”. 5. unless the particles agglomerate. because of the appreciable circulation of particles within the bed.5.2. the bed is usually reasonably well defined and. consider that fluid is forced upward through the bed of particles and that the particles have a density greater than that of the fluid. However. Applications fall into two categories: chemical reac- tions (e.. 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. 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”. Despite the advantages of fluidized beds outline above.

mass of particles =1− particles density * Total bed volume If the flow rate is measured in liters/second. • Observe the onset of fluidization..75. 5. m/s Dp : Size of the particles (μm) L : Height of the bed (m) Re : Renolds Number : The bed voidage. The pressure drop at fluidization can be predicted by using the equation. 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. then Q ∗ 10−3 Vsm = A where A is the cross-sectional area.   ∆P = L(1 − )g ρs − ρf where ρs : The density of solid ρf :The density of the fluid 34 . and Vsm is the superficial velocity m/s. (5.3.1) L ρ (Vsm ) 1 − Re where Vsm : Superficial velocity.

It is frequently used in fluid-bed calculations and in quantifying one of the particle properties.934 d1. read the height of the bed. Practice Questions (1) In your car.1 l/min.0 l/min.5. manometer reading. You will be asked to perform the experiment for two types of fluid: water and air.8 Umf = μ0. (6) Explain the advantages of fluidization in chemical processes.006 f where d : The size of the particle.87 ρ0.2 for the equipment setup. Switch on water pump.4.. Adjust water flow rate in increments of 0. check that the manometer reads zero. (4) What factors influence the pressure drop in a fluidized bed? (5) Describe a Fixed-Bed adsorption column. m μf :The viscosity of the fluid 5. figure 7. catalytic fluidized bed are very often been used. explain. Procedure Study the attached schematic diagram.0 l/min. To perform the experiment. if it does not. adjust the level accordingly. Follow the procedure in the laboratory and prepare your own data sheet. This parameter is best estimated using Baeyens and Gelard correlation 0. Another important process variable in fluidized bed is the minimum fluidizing velocity. 5. In case of air. If you have any problem. please check with your lab instructor.0076(ρs − ρf )0. Increase flow rate by 1. 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. Report your data in the data sheet. 35 . and the state of the bed. there is a fluidized bed tubular reactor for the oxidation of NO to NO2 . adjust the air flow control valve to give a flow rate of 2.

McGraw-Hill.6. 3rd edition. Smith. W. 6th edition. L. • Compare the predicted fluidization point with the actual fluidization point obtained from the graph • Give reasons for any differences between the two values. McCabe. J. New York. Report • Draw a graph of bed pressure drop against air flow rate from the experi- mental data obtained. 1993. Transport Processes and Unit Operations. McGraw Hill. C. 1984. • Calculate the minimum fluidizing Velocity References D. Green. (a) Determine the length of the unused bed. Unit Operations of Chemical Engineering. 36 .01 and the breakthrough curve is given.2 g of carbon. (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. (b) Determine the saturation loading capacity of the carbon. 5th edition.? 5. 1993. Perry and R. The break-point concentration is set at c/c0 = 0. McGraw-Hill. and P . Harriott. C. H. J. Geankoplis. Perry’s Chemical Engineers’ Handbook.00225 g/cm3 entered the bed at a flow rate of 800 cm3 /s. The inlet gas stream having a concentration (c0 ) of 1500 ppm and a density of 0.

Figure of the fluidised bed expirement. 37 .

Schematic drawing of the fluidised bed equipment. 38 .

Water and Air properies. 39 .

The use of more than a single evaporator is related to the economy of heat utilization. If the solution contains dissolved solids. 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. Objectives • Investigate the effect of variation in steam pressure on the capacity of a double effect evaporator.1. (2) Those that yield different crystal sizes of solid. 40 . in a single effect evaporator. Background Evaporation process is one of the major operations to concentrate aqueous solu- tions.2. For example. It would be more efficient if the hot vapor leaving the first evaporator to be utilized to heat liquid in a second evaporator. the resulting evaporated solution may become saturated. It is based on the removal of water from a solution by boiling the solution in a vessel. The major variable used industrially to control the efficient operation of a double effect evaporator. is the heat input to the first effect. which is called evaporator. Evaporation occurs when heat is added to the solution to vaporize the solvent (more volatile component). (3) Those that boils at the same boiling temperature of water as opposed to a higher boiling temperature.6. In a double effect system. vapor from the first effect loses its heat to the liquor in the second effect. • Calculate the economy of a double effect evaporator operating at vacuum pressure. DOUBLE EFFECT EVAPORATOR 6. 6. 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. 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).

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.4. For the double effect evaporator in figure 6. m2 .1. 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.3. Q. D0 6. 6. what is the efficiency of the process? Why is it impossible to have this efficiency? 41 . (3) What are the differences between evaporation and distillation? (4) If you can build an infinite number of evaporators. For example in figure 6. C. the other is used as sweet.5. through the heating surface of the evaporator Q = U ∆T. name it. M0 where Mtot is the total evaporation flow rate and M0 is the input steam flow rate into the first evaporator. W/m2 K. A is the heat transfer surface.6. 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. Procedure Follow the procedure in the laboratory and prepare the data sheet. and ∆T is the overall temperature driving force. The steam economy is given by: Mtot E= . A where U is the overall heat transfer coefficient. the steam economy is D1 + D2 + D3 E= .1.

5 m2 . C. Green.6. F. L. H. 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 economy of each effect and the overall value for double effect operation. Particle Tech- nology and Separation Processes. 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.6. • Do energy balance around first and second evaporators. • Calculate the heat removed in the condenser Qc for each steam pressure and illustrate results on a graph. Unit Operations of Chemical Engineering. McGraw-Hill. Coulson. J. J. 1984. • Determine the capacity of each effect and the overall capacity at each steam pressure. McGraw- Hill. 1991. 5th edition. D. Report • Briefly describe the experiment in your own words. W. 42 . Smith. volume 2 of Chemical Engineering. Backhurst. References J. 4th edition. Perry and R. Harriott. given that the heat transfer area of the boiler is 0. 6th edition. J. Perry’s Chemical Engineers’ Handbook. H. and P . Harker. M. McCabe. Oxford. 1993. Rihardson. and J. • Calculate the overall heat transfer coefficient U for each effect. R. Pergamon.

43 .Figure 6.1: Schematic diagram of multiple effect evaporator.

44 .Figure 6.2: Double effect evaporator expiremntal setup.

(7.1. thus 45 . Theory For a tubular plug flow reactor.2. shown in figure 7. The heat transfer to or from the reactor may be accomplished by means of a jacket or shell-and-tube. It consists of cylindrical pipe and is normally operated at steady state. In the tubular reactor. For the reaction between ethyl acetate and caustic soda. we consider systems in which the flow is highly turbulent and the flow field can be modeled as plug flow. it is equi-molar and is second order in nature.1. • Determine the variation of conversion with respect to the reactor’s residence time. continuous stirred tank reactor (CSTR). For the purpose of the material presented here. 7. TUBULAR REACTOR 7. Also the reactor can be packed with catalyst pellets or inert solids. tubular reactors can be a single continuous tube or several tubes in parallel. 7. the reactants are consumed as they flow down the pipe.3. mass balance for a particular reactant A is ] CAi dCA V = = τ. i. Background There three major types of reactors in the chemical industries: Batch. V is the reactor volume and Q is the total volumetric flow rate.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. The use of tubular reactor is favorable when the back mixing of reaction mixture is not important.e.7. and plug flow reaction (PFR) also known as tubular reactor. Objectives • Recognize plug flow reactor in practice. there is no radial distribution of velocity. In practice.

4. there is a very important tubular reactor for the oxidation of NO to NO2 . The con- version is defined as CAi − CA0 X= (7. (7. rA = k CA CB . τ . FA CAF FB CBF = = CAi = CBi (7.e.4) CAi Then equation can be solved to become X = k τ CAi (7. Follow the procedure in the laboratory and prepare your own data sheet. and FA and FB are the individual feed flow rates (ml/min). figure 7. provided k is kept constant (i. 46 .2 for the equipment setup. Practice Questions (1) In your car. Procedure Study the attached schematic diagram. 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. at constant temperature) for this reaction 7. 7.5. please check with your lab instructor.5) 1−X Thus the conversion factor X/(1 − X) should be directly proportional to the residence time. It is algebraically simpler if it is arranged for the initial concentrations in the mixed feed stream of A and B to be equal.3) FA + FB FA + FB where CAF and CBF are concentrations in the feed tanks of NaOH and CH3 COOC2 H5 respectively.2) where A is NaOH and B is CH3 COOC2 H5 and k is the reaction rate constant.

2nd edition.S.7. 1984.F. • How do you prove that a reaction is first order?[?][?] References H. Perry’s Chemical Engineers’ Handbook. Perry and R. Bischoff.6. Fogler. Chemical Reactor Analysis and Design. derive equation 7.B. 1990. H. Wiley. Froment. 47 . . calculate conversion and plot it against X/(1 − X). G. 1992.5.4 litre as the reactor volume. 6th edition. Comment on the graph calculated. Green. PTR Prentice Hall. D. McGraw- Hill. K. 2nd edition. Elements of Chemical Reaction Engineering. Report • Consider 0. • Consider that the reaction rate is second order.

48 .1: Differential mass balance of tubular reactor.Figure 7.

Figure 7. 49 .2: Schematic diagram of tubular reactor.

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