Abstract:
The primary project goal is to design an industrial plug flow reactor (PFR) system to treat a 10 L/min waste stream composed of 0.2 weight percent aqueous ethyl acetate (EtOAc) down to 0.02 weight percent to comply with current regulations. Aqueous EtOAc is treated via hydrolysis, or saponification, with sodium hydroxide (NaOH) to form sodium acetate (NaOAc) and ethanol (EtOH). The lab team will determine kinetics of hydrolysis in a batch reactor at varying temperatures (20-30°C), such as the second order rate constant, k [L/mol*s], and the activation energy, Ea [kJ/mol]. Measured kinetics will be compared to literature values. Bench scale results will be used to propose a large scale system to treat waste water to specifications.
Background Research:
The hydrolysis of EtOAc with NaOH is a second order reaction according to several pieces of research. Danish et al. [footnoteRef:1] compared the saponification reaction between a PFR and continuously stirred tank reactor (CSTR). The PFR and CSTR were kept at constant temperatures. Three independent variables were chosen: temperature of the reaction, the feed rate of 0.1 M sodium hydroxide and ethyl acetate, and the type of reactor. As seen in Figures 1 & 2, a fractional conversion of 0.9 is not satisfied. [1: Danish M. and Al Mesfer M.K. et al. A Comparative Study of Saponification Reaction in a PFR and CSTR (Research Journal of Chemical Sciences: Vol. 5(11), 13-17) November 2015 http://www.isca.in/rjcs/Archives/v5/i11/3.ISCA-RJCS-2015-137.pdf]
Figure 1: Feed rate, F [mL/min], of 0.1 M sodium hydroxide and ethyl acetate at a constant temperature (30°C) vs conversion rate, XA, and the second order rate constant, k (L/mol*s)
Figure 2: Temperature, T [°C], of 0.1 M sodium hydroxide and ethyl acetate at a constant feed rate (60 mL/min) vs conversion rate, XA, and the second order rate constant, k (L/mol*s)
The optimal feed is 60 mL/min for this 0.4 L PFR and the temperature needs to be above 40°C to reach a conversion of 90%. The current experiment will also test differing feed ratios as well finding the optimal temperature, which will likely be above 40°C.
Kuheli Das et al.[footnoteRef:2] published a research paper studying the kinetics of hydrolysis of EtOAc in a batch reactor. Researchers gathered a collection of rate constants at various temperatures as seen in Table 1 and Figure 3. Conductivity measurements were used to determine compositions, similar to the current experiment. [2: Kuheli Das et al. Kinetic Studies on Saponification of Ethyl Acetate Using an Innovative Conductivity-Monitoring Instrument with a Pulsating Sensor (International Journal of Chemcial Kinetics 19(vol. 43): 648-656, November 2011) https://www.researchgate.net/publication/229360677_Kinetic_Studies_on_Saponification_of_Ethyl_Acetate_Using_an_Innovative_Conductivity-Monitoring_Instrument_with_a_Pulsating_Sensor]
Table 1 provides several rate constants at varying temperatures to compare to the current .
AbstractThe primary project goal is to design an industrial plu.docx
1. Abstract:
The primary project goal is to design an industrial plug flow
reactor (PFR) system to treat a 10 L/min waste stream composed
of 0.2 weight percent aqueous ethyl acetate (EtOAc) down to
0.02 weight percent to comply with current regulations.
Aqueous EtOAc is treated via hydrolysis, or saponification,
with sodium hydroxide (NaOH) to form sodium acetate
(NaOAc) and ethanol (EtOH). The lab team will determine
kinetics of hydrolysis in a batch reactor at varying temperatures
(20-30°C), such as the second order rate constant, k [L/mol*s],
and the activation energy, Ea [kJ/mol]. Measured kinetics will
be compared to literature values. Bench scale results will be
used to propose a large scale system to treat waste water to
specifications.
Background Research:
The hydrolysis of EtOAc with NaOH is a second order reaction
according to several pieces of research. Danish et al.
[footnoteRef:1] compared the saponification reaction between a
PFR and continuously stirred tank reactor (CSTR). The PFR and
CSTR were kept at constant temperatures. Three independent
variables were chosen: temperature of the reaction, the feed rate
of 0.1 M sodium hydroxide and ethyl acetate, and the type of
reactor. As seen in Figures 1 & 2, a fractional conversion of 0.9
is not satisfied. [1: Danish M. and Al Mesfer M.K. et al. A
Comparative Study of Saponification Reaction in a PFR and
CSTR (Research Journal of Chemical Sciences: Vol. 5(11), 13-
17) November 2015
http://www.isca.in/rjcs/Archives/v5/i11/3.ISCA-RJCS-2015-
137.pdf]
Figure 1: Feed rate, F [mL/min], of 0.1 M sodium hydroxide and
ethyl acetate at a constant temperature (30°C) vs conversion
rate, XA, and the second order rate constant, k (L/mol*s)
2. Figure 2: Temperature, T [°C], of 0.1 M sodium hydroxide and
ethyl acetate at a constant feed rate (60 mL/min) vs conversion
rate, XA, and the second order rate constant, k (L/mol*s)
The optimal feed is 60 mL/min for this 0.4 L PFR and the
temperature needs to be above 40°C to reach a conversion of
90%. The current experiment will also test differing feed ratios
as well finding the optimal temperature, which will likely be
above 40°C.
Kuheli Das et al.[footnoteRef:2] published a research paper
studying the kinetics of hydrolysis of EtOAc in a batch reactor.
Researchers gathered a collection of rate constants at various
temperatures as seen in Table 1 and Figure 3. Conductivity
measurements were used to determine compositions, similar to
the current experiment. [2: Kuheli Das et al. Kinetic Studies on
Saponification of Ethyl Acetate Using an Innovative
Conductivity-Monitoring Instrument with a Pulsating Sensor
(International Journal of Chemcial Kinetics 19(vol. 43): 648-
656, November 2011)
https://www.researchgate.net/publication/229360677_Kinetic_St
udies_on_Saponification_of_Ethyl_Acetate_Using_an_Innovati
ve_Conductivity-
Monitoring_Instrument_with_a_Pulsating_Sensor]
Table 1 provides several rate constants at varying temperatures
to compare to the current experiments’ results when completed.
Das also compared his results regarding the second order rate
constant and activation energy of saponification to others whom
used different concentration measuring techniques as seen in
Table 2.
Table 2: Comparison of 2nd order rate constants, k(L/mol*s),
and activation energy, Ea [kJ/mol], of the sodium hydroxide and
ethyl acetate saponification reaction between studies and
3. techniques.
Das attributes the low rate constant (0.11 L/mol*s) and high Ea
(61.4 kJ/mol) of the Smith study to the poor precision of the
volumetric titration method for measuring concentration. All
other studies provide rate constants and activation energies in
the same order of magnitude as Das. The research team expects
to obtain a similar rate constant of 0.16 L/mol*s at 30°C and
predicts that the rate constant will be larger for a PFR at a
higher temperature achieving a fractional conversion of 0.9.
Unit 3 [GM592: Project Planning and the Project Plan]
1 of 3
Assignment 2: Team Assignment
This Assignment is designed to evaluate your ability to
research, organize, and demonstrate
project data and financial information pertaining to the
development of the cost baseline within
the project planning phase. These exercises mimic actual
situations one could expect to occur
between the project manager and their sponsor or key
stakeholders. Its assessments are
4. directed toward measuring mastery in synthesis of information,
proper classifications, critical
thinking, and attention to detail, explanations, and professional
acumen.
Given the information provided for your assigned rocket
assembly project (See Course
Resources):
assembly project.
rocket assembly project.
lop the procurement management plan for your assigned
rocket assembly project.
Ensure that your project documents address the criteria of the
rubric below and follows the
stated requirements.
Directions for Submitting your Team Assignment:
submit your Unit 3 Team assignment, have one person
designated by the team
upload all assignment documents to the Unit 3 Assignment 2
5. Dropbox. Make sure that
you have saved a copy of each of the tools to submit for this
assignment.
r must submit a peer evaluation
individually to your Unit 3
Assignment 2 Dropbox.
GM592 Unit 3 Team Assignment: 50 Points
Points
Possible
Points
Earned
Content (0-30 points)
1. Tool Development (Cost Management Plan)
a) Units of measure. Each unit used in measurements (such as
staff hours, staff days, weeks
for time measures; or meters, liters, tons, kilometers, or cubic
yards for quantity measures; or
lump sum in currency form) is defined for each of the resources.
10
6. b) Level of precision. The degree to which activity cost
estimates will be rounded up or down
(e.g., US $100.49 to US $100, or US $995.59 to US $1,000),
based on the scope of the
activities and magnitude of the project
c) Level of accuracy. The acceptable range (e.g., :10%) used in
determining realistic activity
cost estimates is specified, and may include an amount for
contingencies
d) Process that specifies how formal acceptances of the
completed project deliverables will be
obtained?
e) Process to control how requests for changes to the detailed
scope statement will be
processed as defined in the Integrated Change Control process
(PMBOK section 4.5)?
f) Organizational procedures links. The W BS component used
for the project cost accounting is
called the control account. Each control account is assigned a
unique code or account
number(s) that links directly to the performing organizations
accounting system.
Unit 3 [GM592: Project Planning and the Project Plan]
2 of 3
7. g) Control thresholds. Variance thresholds for monitoring cost
performance may be specified to
indicate an agreed—upon amount of variation to be allowed
before some action needs to be
taken. Thresholds are typically expressed as percentage
deviations from the baseline plan.
h) Rules of performance measurement. Earned value
management (EVM) rules of
performance measurement are set.
i) Reporting formats. The formats and frequency for the various
cost reports are defined.
j) Process descriptions. Descriptions of each of the other cost
management processes are
documented.
2. Tool Development (Human Resource Management Plan)
a) Roles and responsibilities of assigned skill sets?
10
i) Role?
ii) Authority?
iii) Responsibility?
8. iv) Competency?
b) Project organization charts?
c) Staffing management plan?
i) Staff acquisition?
ii) Resource calendars?
iii) Staff release plan?
iv) Training needs?
v) Recognition and rewards?
vi) Compliance?
vii) Safety?
3. Tool Development (Procurement Management Plan)
a) Procurement management approach? Identifies the necessary
steps and responsibilities for
procurement from the beginning to the end of a project.
b) Procurement definition? Describes, in specific terms, what
items will be procured and under
what conditions.
c) Type of contract to be used? Describes the type of contract to
be used so the contracts and
purchasing department can proceed accordingly.
9. d) Procurement risks? Identifies any potential risks associated
with procurement for the project.
e) Procurement risk management? Describes how risks related
specifically to procurement
activities will be managed.
f) Cost determination? Describes how costs will be determined
and if/how they will be used as
part of the selection criteria (RFQ, RFP, RFB).
g) Standardized procurement documentation? Describes what
standard procurement
documentation will be used as part of the procurement
(Organizational procurement forms).
h) Procurement constraints? Describes any constraints which
must be considered as part of
the project’s procurement management process.
i) Contract approval process? Defines the process through which
contracts must be approved.
10
10. Unit 3 [GM592: Project Planning and the Project Plan]
3 of 3
j) Decision criteria? Defines the criteria used by the contract
review board to decide on what
contract(s) to award.
k) Vendor management? Describes the roles and actions the
project team and purchasing and
contracts department will take
l) Performance metrics for procurement activities? Describes
the metrics to be used for
procurement activities associated with the project.
Analysis (0-11 points)
Response exhibits strong higher-order critical thinking and
analysis (e.g., evaluation). Paper
shows original thought.
3
Analysis includes proper classifications, explanations,
comparisons and inferences.
11. 4
Critical thinking includes appropriate judgments, conclusions
and assessment based on
evaluation and synthesis of information. 4
Writing (0-9 points)
Grammatical skills are strong with typically less than one error
per page. Correct use of APA
when assigned. 3
Appropriate to the assignment, fresh (interesting to read),
accurate, (no far-fetched,
unsupported comments), precise (say what you mean), and
concise (not wordy).
3
Project is in 12-point font. Narrative sections are double-spaced
with a double space between.
Project is free of serious errors; grammar, punctuation, and
spelling help to clarify the meaning
by following accepted conventions.
3
Peer Evaluation
12. Minus points lost on Peer Evaluation (15= 0, 14= -1, 13= -2,
etc.) 0
Total 50
Table of Contents
Cost Management Plan
1.1 Units of Measure
1.2 Level of Precision
1.3 Level of Accuracy
1.4 Process for Formal Acceptances
1.5 Process to Control Requests for Changes
1.6 Organizational Procedural Links
1.7 Control Thresholds
1.8 Rules of Performance Measurement
1.9 Reporting Formats
1.10 Process Descriptions
Human Resource Management Plan
2.1 Roles and Responsibilities
2.2 Project Organization Charts
2.3 Staffing Management Plan
Procurement Management Plan
3.1 Procurement Management Approach
3.2 Procurement Definition
3.3 Type of Contract to be Used
3.4 Procurement Risks
3.5 Procurement Risk Management
3.6 Cost Determination
3.7 Standardized Procurement Documentation
3.8 Procurement Constraints
3.9 Contract Approval Process
3.10 Decision Criteria
3.11 Vendor Management
13. 3.12 Performance Metrics
CHE 415: Chemical Engineering Laboratory Winter 2018
PLUG FLOW REACTOR
Equipment Description
A continuous-flow plug flow reactor (PFR) for liquid-phase
reactions is located in the NE corner of JOHN 214. The reactor
consists of a clear glass tube filled with glass beads. The
reactor is inclined slightly so that liquid will completely fill the
tube. Two liquid feed streams are pumped at independent flow
rates into the reactor. Each feed stream has its own pump and
feed reservoir. The reactor effluent flows into the sewer.
Underneath each feed reservoir is a shut-off valve. When the
shut-off valve is opened, the liquid contents of the feed
reservoir empty into the drain. Lab equipment for
characterizing reaction kinetics in batch mode is also available.
Conductivity probes and recording equipment are available.
Figure 1. The CHE 415 PFR system in Johnson Hall 214
consists of two 17.5 L reservoirs for dilute ethyl acetate and
sodium hydroxide solutions, pumps and instrumentation to
record conductivities and temperatures. The feed solutions are
mixed in a header and reactor effluent is plumbed to the storm
sewer.
Overview of Experimental Procedures
Note: Personal protective equipment is of paramount importance
in this lab. In addition to the lab minimum of protective
eyewear and a lab coat, you will wear an apron and face shield
14. during concentrated solution preparation (see below) and nitrile
gloves if operating or working around the batch reactor or PFR.
Be sure to identify roles so that the dry working lab space and
computer are not exposed to gloves or chemicals.
Conductivity Probe Calibration
Note: It is critical that the conductivity probe at the PFR outlet
does not block the flow of your reactor. Consult an available
instructor or TA to ensure the probe is positioned correctly
before conducting your PFR experiments. Consult an available
instructor or TA for assistance to assemble and connect the
probe correctly and to locate the appropriate standards.
On your computer desktop, launch LoggerPro. At the top menu
bar, select Experiment > Calibrate > Channel 1: Conductivity
Probe. This will launch a dialogue box to set your conductivity
standards. Ensure that your sensitivity setting is set to 0 –
20,000 µS/cm2 both on your conductivity probe and on your
calibration dialogue box. Once verified, sufficiently submerge
the probe in a vessel of water and establish low level point at 0
µS/cm2 and select Keep,
Decant approximately 30 mL of (2764 µS/cm2) standard
solution into a small glass beaker from the stock bottle. Dry the
probe before inserting into the standard. Establish high level
point as previously described. Leave the probe in the standard
solution to verify calibration by the in-time conductivity read
out. Discard your standard solutions to the drain after use.
Batch Experiments
Equipment is provided for conducting batch experiments to
characterize reaction kinetics. Select useful stock
concentrations for aqueous solutions of ethyl acetate
(CH3COOC2H5) and sodium hydroxide (NaOH) and prepare
them at your lab bench using process water and the beakers
15. provided. The equipment includes hot plates, external
temperature controller, 250 mL and 400 mL beakers, graduated
cylinders, Vernier conductivity probes and Vernier data
recording equipment. Hot plates and external temperature
controller are used to heat the solution at a constant
temperature. Literature data should be used to inform your
laboratory plans (runs, temperatures, durations, etc.). Consider
having one of your team members at a time working to
familiarize yourselves with the PFR process equipment, valving,
etc. That will help ensure productivity in your second lab
session.
Figure 2. Hot plates with external temperature controller and
magnetic stirrers are used for batch experimentation. The
external temperature probe (the orange wire) is used to the
control the temperature of your solution. Always submerge the
temperature probe to the middle of the liquid height in order to
accurately measure the temperature of your solution. Note that
operating temperature is approximately 3°C higher than
setpoint.
!!!! CAUTION !!!! CAUTION !!!! CAUTION !!!! CAUTION
!!!!
The heating surface can be extremely hot and cause severe
burns!
The external temperature controller, temperature probe and
conductivity probe wire should not come into contact with
heating surface!
The external temperature controller should always be placed in
vessel full of liquid, whenever the heater control is on. If not,
this will cause the hot plate to heat up to 550°C!
16. Safety information
· Remove minor exterior liquid spills promptly.
· Disconnect the power cord before moving or cleaning the unit.
· DO NOT touch the top surface even after disconnecting the
cord because the top surface may still be hot enough to cause
severe burns.
· Use tongs to handle hot glassware
Hot plate symbols
Caution – Hot Surface: Cautions that the top plate is too hot to
touch.
Indicates that the accessory external temperature controller is
properly plugged into the unit.
Heating instructions for temperature-controlled hot plates
· Connect the External Temperature Controller to the connector
on the back of the unit. - Temperature Probe in Use Indicator:
This will illuminate when External Temperature Controller is
properly connected.
· Fill vessel with solution to be heated.
· place stir bar into vessel.
· Place vessel in the center of the top surface.
· Insert the tip of the External Temperature Probe into the
solution.
· Secure the position of the External Temperature Controller by
using a ring stand/support rod and clamp. - Assure that the
17. cable of the External Temperature Controller does not come into
contact with the heating surface.
· Turn Heat Control Knob until the Heating Temperature
Display shows the desired heating temperature.
· Flashing Display: The number shown on the Heating
Temperature Display will FLASH when the actual heating
temperature is not at the set temperature.
· Constant Display: The number shown on the Heating
Temperature Display will remain constantly ON when the
measured solution temperature is at the set temperature. - Hot
Top Indicator: The Hot Top Indicator will be ON at all times
when the temperature of the top surface is too hot to touch
(greater than ~60°C). - The Hot Top Indicator will FLASH when
the Heat Control Knob is turned OFF but the top surface is still
too hot to touch. - The Hot Top Indicator will be OFF when the
temperature of the top is less than ~60°C.
Plug Flow Reactor Experiments
Prepare concentrated solutions of ethyl acetate (CH3COOC2H5)
and sodium hydroxide (NaOH) feed solutions in the fume hood
adjacent to the PFR using process water and the 1 L labeled
Nalgene bottles provided. The feed reservoir volumes are both
17.5 liters. Determine in advance the required mass of sodium
hydroxide pellets and ethyl acetate. Prepare concentrated stock
solutions to be diluted in each reservoir to the desired feed
concentrations. Safety note: ethyl acetate vapor is flammable
and presents a serious fire risk if spilled or if solvent is allowed
to openly vent to the lab. Ethyl acetate also has a strong odor
when concentrated. Take measures to minimize fumes as
breathing ethyl acetate vapor may cause respiratory irritation
and headache.
Figure 3. After calibration of the conductivity probe. Place the
18. conductivity probe as shown in the picture
Figure 3. The fume hood in JOHN 214 NE is shared by the
CSTR and PFR teams for preparation of concentrated solutions.
Be extra careful and communicative while working in close
quarters with others. Leave the workspace as you found it, with
stir plate, stir bar, graduated cylinders, etc.
CAUTION! Significant heat evolves when NaOH dissolves in
water! Start with cold water and continuously stir while slowly
adding pellets to the water to dissipate the heat of solution. The
resulting concentrated NaOH solution is also extremely caustic
– wear appropriate PPE (gloves, goggles, face shield, and lab
coat) at all times when mixing and handling the solution.
Always use a rubber bucket or other secondary containment
when transporting containers of strong acids or bases.
Make sure the NaOH pellets have completely dissolved.
Carefully pour each concentrated solution into the respective
feed reservoir while continuing to fill the reservoir with water
from the available hose (wear your PPE and pour along the side
of the reservoir to prevent splashing). NOTE: Do not walk
away from a reservoir as you fill it with a hose. Fill the
reservoir with 17.5 L. Determine when you think it’s
sufficiently well-mixed.
Calibrate each pump separately by measuring the liquid volume
accumulated over a given time at a fixed "frequency control"
setting. Repeat and get an average flow rate (liquid
volume/time) at a given frequency control setting. Vary the
frequency control setting to obtain a calibration curve of
19. volumetric flow rate vs. frequency control setting. The
calibration curve is valid only at a fixed stroke setting.
Therefore, record the stroke setting. If you change the stroke
setting even slightly, then you must re-calibrate the pump. If
desired, you may calibrate the pump at a different stroke setting
to change the range of flow.
Remember, you are conducting a reaction kinetics experiment.
Periodically measure room, effluent stream, and feed reservoir
temperatures.
At a fixed set of operating conditions, it is a good idea to take
several samples of reactor effluent at various times to insure
that steady-state operation has been achieved. Remember, the
residence time in the reactor is set by the inlet liquid flow rates.
Also, since the reaction rate is temperature dependent, be sure
that you measure the temperature over the course of your
experiments.
Shut Down
Drain each feed reservoir to the sewer. Rinse the reservoirs
with tap water then pump at least 1 L of water through each
pump and the reactor to thoroughly flush the system. Drain the
remaining water in the reservoirs to the sewer. Pour the
remainder of the concentrated solutions into the nearby lab sink
simultaneously in order to neutralize each. It is important that
you leave the lab station as you found it.
PFR SPECIFICATIONS
Design: 274 cm length
2.54 cm inner diameter
Packing: 0.6 cm beads, void volume 550 mL
20. Feed: 0.05-0.2M ethyl acetate (aq)
0.05-0.2M NaOH (aq)
Flow Rates: ethyl acetate feed solution:
134 to 255 mL/min at a stroke setting from 30 to 100
NaOH feed solution pump:
115 to 236 mL/min at a stroke setting from 30 to 100
Temperature: ambient (record feed, effluent, and air
temperatures)
21. Appendix: Questions to Consider
The following is a list of questions that might be useful to
discuss with your group:
1. How was steady-state operation verified?
2. Was the reactor system really isothermal? How was the
isothermal condition verified?
3. How did the rate constant calculated from experimental data
compare with literature values at the same temperature?
4. Was the reactor truly in plug flow?
22. 5. What was the residence time for 90% conversion based on
your measurement?
4