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I will attach a source that i need someone to look at it and write one page background. please put the tables in the background research because the source has some. I will attach my experiment where yu can have an idea where to look and i will attach a sample of someone work.
website source: http://www.academia.edu/13019765/Kinetic_studies_on_saponification_of_ethyl_acetate_using_an_innovative_conductivity-monitoring_instrument_with_a_pulsating_sensor
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 ]
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 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 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.
Strong Foundations Engineering, Inc.
| T 541-737-4791 | http://cbee.oregonstate.edu |
SUBJECT:
Saponification of Ethyl Acetate Using a PFR
One of the main waste streams from our facility is an aqueous stream containing about 0.2 wt% ethyl acetate that can flow at up to 10 L/min. In order to dispose of this stream in the municipal wastewater system, we must reduce the concentration of ethyl acetate to less than 0.02 wt% to comply with current standards. It has been proposed that the ethyl acetate be hydrolyzed using a solution of caustic soda in water. In order to enable the choice of an appropriate reactor, you are requested to evaluate the performance of two reactor configurations, PFR and batch, and issue recommendations on reactor designs to treat the waste stream described above based on your observations and economical considerations.
A wall-mounted plug flow reactor is available in Gleeson 104 with some documentation available online. Feed stream concentrations of 0.1N for both NaOH and ethyl acetate should be used and conductivity measurements used to assess concentration. Investigate flow rate ratios to optimize performance. Planning, preparation, and understanding underpinnings are critical.
Ensure that sufficient data is collected to enable good statistical accuracy. Do not underestimate the challenges in using conductivity to measure concentration. Data from a previous team is provided online but it is recommended that at least part of that data be replicated.
Your team is asked to provide:
1. experimental determination of the rate expression at different temperatures using beaker-scale batch experiments and comparison to literature.
2. Arrhenius analysis of the rate data and comparison to literature.
3. prediction and experimental analysis of bench-scale PFR performance.
4. design of a PFR system to treat the waste stream described above.
5. suggestions you have for improving the experiment.
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 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. (Safety)
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 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!
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 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 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 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
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)
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?
5. What was the residence time for 90% conversion based on your measurement?
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