CHEMICAL ENGINEERING 4903-2
FALL SEMESTER – 2014SCHEDULE OF LABORATORY EXPERIMENTS

(Revised 8/28/2014)

Project Period / I
Formal Report / II
Report / II
Report
Receive Lab Assignment / 8/26 / 9/25 / 11/6
Lab Prelim. ConferenceDeadline / 9/2 / 9/30 / 11/11
Report Due (1:00 PM) / 9/25 / 11/6 / 12/11
Technical Rewrite Due (1:00 PM) if necessary / One week after receiving instructor graded report / One week after receiving instructor graded report / None due
Group I
LITKA,ANDREW SIMON
MOE,GULIA ABSATOVA
STOCKING,DEREK ALLEN
/ Shell & Tube Heat Exchanger-1 / Extruder-2 / Stirred Tank Reactor-3
Group II
BURGER,MASON JAMES
SJOBECK,COLLIN GLEN
ZHANG,YI
/ Stirred Tank Reactor-1 / Ultrafiltration/Reverse Osmosis-
2 / Shell and Tube Heat Exchanger-3
Group III
DE MEDEIROS SILVA,MARCEL
DUFFIN,TAYLOR GREGORY
HUYNH, Chung
/ Distillation Column-1 / Shell & Tube Heat Exchanger-2 / Liquid Level Control-3
Group IV
ALVES ANGHINONI,LEONARDO ELOY
DE OLIVEIRA PACHECO,GUILHERME V.
SCHEFFER,MAYARA
/ Fluidized Bed-1 / Spray Dryer-2 / Distillation Column-3
Group V
DALY,RONALD MAGALSO
SINGH,TEJ PARKASH
TELENKO,DANIEL JOSEPH MARVIN
/ Glass Lined Reactor-1 / Distillation-2 / Fluidized Bed-3
Group VI
KOOYMAN,LUKE MITCHELL
MBONISI, Sibanda
SCOTT,MICHAEL DAVID
/ Absorption Column-1 / Liquid Flow Bench-2 / Double-pipe Heat Exchanger-3
Group VII
COX,BETHANY RENEE
HACKING,ERIK P
HAMILTON,NATHAN JAMES
/ Ultrafiltration/Reverse Osmosis-1 / Fluidized Bed-2 / Heat Control-3
Group VIII
BUABSSI YARED,MARIANA
CHAVES ALMEIDA DE OLIVEIRA,MATEUS
PEREIRA RAMOS,LUIZA LORRANE
/ Heat Conduction-1 / Glass Lined Reactor-2 / pH Control-3
Group IX
BODILY,GEOFFREY NATHANIEL
NGUYEN,VAN T
TRAN,HONG PHUONG THI
/ Liquid Flow Bench-1 / Double Pipe Heat Exchanger-2 / Absorption Column-3
Group X
BUCHMULLER,ROBERT NICHOLAS
JONES,TIMOTHY REED
WARBY,MICHAEL O
/ Vacuum Drying Oven-1 / Gas Flow Bench-2 / Glass Lined Reactor-3
Group XI

Shell and Tube Heat Exchanger-1

The shell and tube heat exchanger in the laboratory has not been used for several months. Beehive Engineering would like you to measure the fouling resistance in this unit so that it can be used for a new design. To measure the fouling resistance you will need to first determine the overall heat transfer coefficient for the transfer of heat from the jacket to the liquid inside the shell. The wall conduction and inside and outside heat transfer resistances must be determined by predictions so that they can be subtracted from the overall heat transfer coefficient leaving the fouling resistance. In this process, there are errors in experimental measurements and errors in the various predictions which will have an effect on the accuracy of the fouling resistance.

For your safety review meeting you will have to establish a protocol for these measurements (including accuracy assessment) and a dimensionless number correlation for the shell side and tube side heat transfer coefficient that is reasonable for this type of equipment. Note, your Reynolds numbers may not be in the fully turbulent range. Also be prepared to discuss the propagation of error in all of the calculations needed for this lab.

For you laboratory report, you should compare your experimental results for the inside and outside heat transfer coefficients with theoretical correlations to generated credibility for using them in determining the fouling resistance. The final report should also clearly report the fouling factor.

Finally using this fouling factor and this shell and tube heat exchanger determine the flow rate for SiH2Cl2 which enters as a vapor at it boiling point at 10 psig and is condensed and cooled to -55 C using Syltherm XLT as the coolant operating from -95C to -60C. see

Be prepared in your oral quiz to address the following:

a) Safety issues with this experiment

b) Equipment operation

c) Data sheets

d) Other germane points with respect to this experiment

Please include this assignment in your report as an appendix but do not cite it in the body of your report.

Stirred Tank Reactor-1

A client is running his CSTR without baffles and a top feeding location for both reactants. Both of these changes were done at the same time and now his reactor conversion is much too low. His engineer told him that the thermal well and feed tubes would provide sufficient mixing in this reactor so baffles were not needed. He wants to know which change is responsible for the low conversions being reported. The other operating conditions for the reactor are a total reactant flow rate of 100 mL/min, a reactor volume of 1.3 L and a Rushton impeller speed of 10 rpm. The reaction being performed in the reactor is the saponification of ethyl acetate with the reactants being fed at equimolar flow rates.

Uniform mixing of reactants is critical to the conversion in a CSTR. You are to develop a series of data and calculations to show the effect of residence time on reactor conversion for presentation to the client. Since the laboratory hoods are not functioning no chemicals with toxic vapors can be used so only residence time distributions and model calculations can be used to prove your point.

Please run a CSTR with and without baffles and with top and bottom feed locations to establish the degree of micro/macro-segregation that is observed as a function of stirring rate (1, 10, 100 rpm) using the residence time distribution as your test case. Start with an unbaffled tank and proceed to add baffles until four are added and do these measurements for top and bottom feed locations. Please determine the residence time distribution for each experimental condition. Compare the residence time distributions and the micro/macro-segregation models given in Chapt 14. of Fogler’s “Elements of Reaction Engineering” 2nd edition.

The client uses the saponification of ethyl acetate

Et-Ac + NaOH ↔NaAc + Et-OH

for his reaction. The kinetics of this reaction is reported in Hovarka, R.B. and Kendall, ;H.B. "Tubular reactor at low flow rates" CEP56(8),58-62(1960). In equimolar experiments they found this reaction to be second order overall. The kinetics provided by Hovarka and Kendall can be used for prediction purposes.

In your final report, use reactor-mixing models to fit the results you have obtained from measurements of the residence time distribution. Use your best mixing model and the reaction kinetics to predict the real reactor conversion and compare it to the ideal CSTR reactor conversion. So that we can show the client we can clearly predict the effects of poor mixing in his CSTR. Clearly identify which of the two changes, removal of baffles and top feeding, is responsible for the low conversion the client is experiencing in his/her saponification reactor.

Please include this assignment in your report as an appendix but do not cite it in the body of your report.

Bubble-cap Distillation Column –1

Please operate the laboratory distillation column in two modes: 1) at total reflux and 2) when top and bottom products are being taken with a recycle ratio of approximately twice the minimum recycle ratio. Determine the overall and stage-by-stage efficiency of the laboratory distillation column under these two modes of operation. Please assure that the distillation column is operating at steady state before samples are taken for your analysis of the efficiency.

For your oral exam please predict the overall stage efficiency from a correlation available in the literature. For this calculation, assume that the column capacity is limited by flooding considerations and make your estimate of overall efficiency at 80% of flooding. Also be prepared to discuss errors in your experimentally measured quantities and error propagation of the overall stage efficiency determined. Which mode of analysis and operation will give the lowest errors?

An estimate is needed of the capacity (GPM of Feed) of the laboratory distillation column to process a 15% ethanol in water stream and to produce a 95% ethanol product. The approximate reflux ratio, the reboiler duty required, the optimum feed plate location and the expected percent ethanol recovery are to be specified.

You are to make this estimate based upon the results of operation of the same laboratory column on the water-isopropanol solution available. Necessary corrections to these laboratory data are to be made based upon standard correlations, to permit the evaluations needed for the ethanol-water system.

Be prepared in your oral quiz to address the following:

a) Safety issues with this experiment

b) Equipment operation

c) Data sheets

d) Other germane points with respect to this experiment

Please include this assignment in your report as an appendix but do not cite it in the body of your report.

Fluidized Bed-1

Fluid bed reactors are used for many applications in industry from pulverized coal burning to catalytic crackers to silicon purification. Since there is excellent heat transfer in the fluid bed, coils are often inserted to heat or cool the bed allowing the reaction heat to be dissipated in exothermic reactions. Heat transfer and fluidization characteristics are different for different powders. A client has several powders (carbon, sand and glass beads) that need to be tested for their fluidization characteristics. The most important fluidization characteristic is that of the minimization fluidization velocity; the velocity of the gas just necessary to fluidize the powder. Please measure the minimization fluidization velocity for the client’s powders. Compare the minimization fluidization velocities to a correlation in Leva, (“Fluidization “ p. 63 McGraw-Hill, NY 1959). To make this comparison the particles in the powder must be characterized with respect to their density, particle diameter, and shape factor. In addition determine the bed expansion as a function of the pressure drop and compare these results for the various powders to those calculated using the correlation in Leva, Chapt 4.

Using the fluidization results for the client’s carbon sample design a fluid bed combustor for the reaction

C + O2 CO2

with the surface reaction rate given by Parker and Hottel (Ind. Eng. Chem. 28,1334,(1936))

Rate=,

for 1 tonne/hr carbon combustion rate operating at 10% excess air at 1300K. Please note that you should also consider the rate of boundary layer diffusion as well as the surface reaction rate in the kinetic model used for design of the fluid bed combustor.

Please include this assignment in your report as an appendix but do not cite it in the body of your report.

Glass Lined Reactor-1

The client needs a Heat transfer correlation for a glass-lined reactor of odd geometry. Using the glass lined reactor determine the heat transfer coefficient for the transfer of heat from the steam jacket to the liquid inside the reactor. Please make these measurements with the baffle in place at various liquid levels and stirring rates. For your oral exam you will have to establish a protocol for these measurements (including accuracy assessment) and a correlation (of the type Nusselt Number versus Reynolds number) that is reasonable for this type of equipment.

Based upon a reaction the saponification of ethyl acetate

Et-Ac + NaOH  NaAc + Et-OH

determine a design for this glass-lined reaction using this reactor. The kinetics of this reaction is reported in Hovarka, R.B. and Kendall, ;H.B. "Tubular reactor at low flow rates" CEP56(8),58-62(1960). In equimolar experiments they found this reaction to be second order overall. This reaction conversion may be limited by either kinetics or heat transfer. Assuming 1 M feed of both reactants and a conversion of reactants to the product of 0.85,determine the capacity (kg/hr of NaAc that the glass-lined reactor can produce.

Be prepared in your oral quiz to address the following:

a) Safety issues with this experiment

b) Equipment operation

c) Data sheets

d) Other germane points with respect to this experiment

Please include this assignment in your report as an appendix but do not cite it in the body of your report.

Absorption Column-1

Operate the packed absorption column in the Chemical Engineering Laboratory to absorb C02 from a gas stream with 0.01% NaOH solution and water. Determine, for each of the packed columns, the number of transfer units and height of a transfer unit for C02 absorption for both solutions. The groupwho operated the packed columns during the previous laboratory period was unable to close the material balances. The principal problem seemed to be obtaining reliable flow rate information for the air and water streams; it appears, therefore, that the air and water flow meters should be calibrated before you begin.

Be prepared in your oral quiz to derive the equations governing absorption in a packed column with and without reaction and present your experimental plan including how you propose to make a feed streams containing C02 and NaOH as well as the CO2 mole fractions you propose to employ. Discuss the measurements required, what analytical procedures you will use to determine C02 concentrations in the air and water streams, and how the data will be analyzed to determine the information requested.

Be prepared in your oral quiz to address the following:

a) Safety issues with this experiment

b) Equipment operation

c) Data sheets

d) Other germane points with respect to this experiment

Please include this assignment in your report as an appendix but do not cite it in the body of your report.

Ultrafiltration/Reverse Osmosis-1

Great Salt Lake Minerals has a brine that consists of 10% wgt MgCl2 and 1.5% wgt NaCl. It is suggested that ultrafiltration can be used to make the separation between the different salts in the brine.

Using the laboratory ultrafiltration/reverse osmosis unit and membranes provided determine the conditions of pressure, flow rate and temperature that gives the largest purification. Be particularly aware that membrane fouling caused by increased solute concentration at the membrane surface causes concentration polarization which decreases permeate flux.

To start this project you will need to develop analytical methods to measure the concentration of Na and Mg ions in solution. Your boss thinks Atomic Absorption sepectroscopy can be used. Dana Overracher is an expert on this instrument.

Use the best experimental conditions to design an ultrafiltration/reverse osmosis unit for this aqueous solution to process 1,000 gallons per day for the client. Using the concentration polarization results determine the lifetime of the membrane for this application. Determine the cost for membrane replacement as well as the pumping costs over the course of 1 year’s operation giving a cost per million gallons of water produced.

Please include this assignment in your report as an appendix but do not cite it in the body of your report.

Heat Conduction-1

Your older car antenna made of shiny 304 stainless steel which is 0.6 cm diameter and 30cm tall is attached to your black car. The black car keeps the bottom of the car antenna at a constant temperature of 120C due to the car sitting in the sun on a sunny day. The air temperature is 28C and there is no wind blowing. You are to use the heat condition apparatus to perform experiments to determine an appropriate heat transfer coefficient for modeling purposes to make predictions of the temperature profile in your car’s antenna. Before proceeding to model the car’s antenna, it is necessary to verify that you have an accurate simulation by making comparisons with experiments performed on the aluminum, steel and stainless steel rods that are part of the heat conduction apparatus. These measurements should be made with the apparatus with rods in the horizontal and the vertical direction. Show the differences in rod orientation between the heat transfer coefficients measured. Does the rod’s vertical position make difference in the heat transfer coefficient that should be applied? After verifying the accuracy of the simulations with the rods in both positions proceed to the simulation of the car’s antenna. For the vertical position of the antenna determine the height above its base is the antenna 100C, the boiling point of water.

For the preliminary oral exam, be prepared to describe the apparatus, correlations for natural convection given various geometries, the appropriate equations that govern the conduction of heat down a rod that has radial heat transfer at is surface, methods of error analysis to be applied to all calculations performed in this laboratory report.

Please include this assignment in your report as an appendix but do not cite it in the body of your report.

Liquid Flow Bench-1

Flow through packed beds are essential for many unit operations including trickle bed reactors used for biological clean-up of phenol from process waters in a Salt Lake City refinery. Phenol at concentrations above 10 ppm is toxic to bacteria in waste water treatment facilities and must be removed before refinery waste water is discharged to the sewer. As a result, waste water is caused to flow through a packed bed bioreactor made of porous sand impregnated and bound with an enzyme from unique strain of bacteria that considers phenol food. The enzyme in the acid form catalyzes the oxidation of phenol rendering it non-toxic. The kinetics of this oxidation reaction follows the Michaelis Menton kinetic relation