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CHE 4262 Cllimbfilmtue15 2 Blanked
CHE 4262 Cllimbfilmtue15 2 Blanked
CHE 4262 Cllimbfilmtue15 2 Blanked
Eric Henderson
Nadezda Mamedova
Andy Schultz
Xiaorong Zhang
Table of Contents
References……………………….………………………………………………………………..21
Appendices………………….…….….……………………………………………………….......22
1
Executive Summary – Nadezda Mamedova
Purpose: The purpose of the experiment was to determine operating conditions of a climbing
film evaporator that can recover triethylene glycol from a stream that contains 30 wt%
triethylene glycol. The desired concentration of the exit stream is at 88 wt% triethylene glycol. It
is required that 90,000 gallons of inlet liquid be processed per day.
How information was obtained: Our engineers had four laboratory days to operate a climbing film
evaporator over a range of vacuum pressures to determine which pressure was the most cost
efficient as well as which operating conditions could process the required inlet flow.
Key findings: We determined that in order to be cost efficient and handle the required inlet flow,
we require two climbing film evaporators operated at 20 inHg vacuum. The total cost of installation
and operation for a year is $2,718,483.00. The most expensive requirement is 2.8*107 kg of steam
per year.
Disclaimers and Recommendations: This experiment was performed under the assumption that the
vacuum and system pressures were in equilibrium. We used this assumption to calculate a goal
temperature at which the desired exit composition would be reached. We recommend testing the
exit product composition to determine the accuracy of this assumption. Due to time constraints,
our data gathered was not all started at the same temperature. If more time is allowed, we
recommend running the experiment from the same temperature and atmospheric pressure to allow
for better comparisons.
2
Introduction – Nadezda Mamedova
Our engineers are expanding our company by adding in a climbing film evaporator that can
remove water from a stream of triethylene glycol and recycle the glycol back into a previous
process. The entering stream is at a concentration of 70 wt. % water, and our goal is to have an
outlet stream of no more than 12 wt. % water. The process requires ninety thousand gallons of
mixture to be processed per day.
Climbing film evaporators, also known as rising film or vertical long tube evaporators, are used
in industry for effluent treatment, polymer production, food production, pharmaceuticals, and
solvent recovery.1 The liquid being evaporated is fed from the bottom into long tubes and is
heated with steam condensing on the outside of the tubes, bringing the liquid inside to a boil. The
produced vapors press the liquid against the walls of the tubes. The vapor has a higher velocity
which forces the liquid against the tube wall to rise. This gives the process its name.2
3
Theory – Nadezda Mamedova
A variety of evaporators are used in industry. Our engineers will focus on the climbing film
evaporator operated in batch mode. The evaporator will also be operated under vacuum. The
benefit of this is that it allows for operation at lower temperatures. The mixture of triethylene
glycol and water enter the bottom of a thin wall glass calandria tubes wherein the mixture is
heated to boiling. The water vapor carrying the triethylene glycol climbs the evaporator and
enters a cyclone separator. Here the triethylene glycol condenses and is returned to the
evaporator while the water is collected separately.
Bourgois and LeMaguer found that the dimensionless volumetric vapor flux may be used to
determine the most efficient point of operation. The dimensionless vapor flux, , is given by
[1]
Where:
= vapor density
= liquid density
= gravitational constant
= inside diameter of the tube
Operation efficiency increases with increasing until = 2.5. At this point steam
consumption is at a minimum and the steam temperature and vacuum pressure are optimal.
When the value of is greater than 2.5 the steam consumption needed to produce product at a
given concentration greatly increases as increases, and the process becomes inefficient.
To account for economic efficiency we considered a scale up factor, R. R was determined from
the amount of liquid needing to be processed and the amount our pilot equipment could process.
4
[2]
Where:
R = Scale up factor
Qrequired = Amount of liquid required for processing (90,000 Gallons)
QExperimental = Amount of liquid our laboratory could process
This R factor was carried out to determine other scaled up calculations and cost of the process.
5
Design Plan – Eric Henderson
During the operation of a climbing film apparatus, the continued use of steam becomes very
expensive; therefore, an attempt to minimize this use of steam will be made. A system
temperature at a given pressure will be related to steam flow rate to produce a 88% triethylene
glycol separation using figures from the DOW Chemical Triethylene Glycol manual (figure
below).4 This system temperature will be found by utilizing the Antoine equation in Excel’s
Solver. The Antoine constants are obtained by interpolation of 80% and 90% values in Figure 5
in this lab’s manual (Vapor Pressures of Aqueous Triethylene Glycol Solutions at Various
Temperatures) to produce constants for 88% triethylene glycol separation.
Using these experimental data (triethylene glycol flow, column pressure, steam temperature,
dehydrated triethylene glycol temperature, and condensed water volume), various relationships
between data can be calculated to estimate process cost. For example, once a strong relationship
between triethylene glycol separation, temperature, and pressure has been established, a steam
cost comparison ($/kg) will be analyzed by using data from Table 8.4 (Costs of Some Common
Chemicals).5
By taking the costs into consideration, the optimum steam flow rate will be related to vapor flux
(Equation 1) and feed flow rate to determine the economically optimum scale up plant size.
Equipment sizes will be predicted from using Figure 2, with the notion that the production
6
requirement of 90k gal/day of process mixture must be met. Analysis of these costs will also
require a raw materials cost estimation from Table 8.3, and ultimately, the total costs
examination by Table 8.2.5
Although correction factors are assumed to not apply, scale up factors must still be calculated
once the optimal steam pressure and vacuum pressure are found. The scale up factor calculated
from Equation 2 (from Theory) will be used when sizing the equipment and total steam
consumption from the pilot plant to the commercial plant. On the other hand, the size of the
tubes in the evaporator does not need to be scaled up since the heat transfer will not change.
However, an increased number of tubes in the evaporator would be optimal for the commercial
process.
The optimal steam pressure and vacuum pressure are found by experimental trials in which the
desired composition is achieved by the lowest steam consumption under a constant vacuum
pressure. These values will be used in the cost analysis, along with the amount of cooling water
in the condenser. The amount of cooling water in the condenser is found from the heat necessary
to condense the vapor from the cyclone separator.
7
Experimental Plan – Andrew Schultz
In this experiment, the group will analyze the separation of water from triethylene glycol (TEG)
via steam evaporation in a column. Several variables will be manipulated throughout the
experiment to evaluate the optimal conditions which yield the best separation of the two
substances. Variables of importance include: steam flow, saturated triethylene glycol flow,
column pressure, steam temperature, dehydrated triethylene glycol temperature, and condensed
water volume. The operating parameters for each are given below in Table 1.
Throughout the experiment, the independent variables which the group will manipulate include
steam flow, saturated triethylene glycol mix flow, and vacuum pressure. The group will
determine the flow rates for the steam and saturated TEG. These flow rates will be measured by
rotameters located on the operating panel and will remain constant throughout the experiment.
The group will manipulate the pressure inside the column via a vacuum pump. The separation of
water and TEG will then be evaluated at various vacuum pressures.
As the pressure inside the column is manipulated, each new system pressure will be used to
calculate the theoretical (goal) temperature that triethylene glycol must reach to obtain the
desired dehydration. The temperature of the steam flowing into the system is an important
parameter to monitor as it is the initial temperature of the system. The measured (dependent)
goal temperature is the final temperature of the system at a given vacuum pressure. The volume
of condensed water is also an important dependent variable that the group will measure. The
volume of water collected over a period of time as determined by the group will indicate the
effectiveness of separation at a given vacuum pressure.
8
The group will conduct the experiment over the next three laboratory periods according to Table
2 below. The order of evaluation for each vacuum pressure will be cycled during each laboratory
period to evaluate the effect of the temperature of the column being higher than ambient
conditions after the first experiment of each day. This will allow the group to identify and
evaluate the differences, if any, of starting an experiment at ambient conditions versus a system
at higher than ambient temperatures.
DATE TASK
Measure condensed water volume for vacuum pressures at 19, 20, 21, 22
10/06/2015
psi. Evaluate time taken to achieve goal temperature.
Measure condensed water volume for vacuum pressures at 20, 21, 22, 19
10/13/2016
psi. Evaluate time taken to achieve goal temperature.
Measure condensed water volume for vacuum pressures at 21, 22, 19, 20
10/20/2015
psi. Evaluate time taken to achieve goal temperature.
Due to the limitations of the laboratory, specifically the vacuum pump, the range of vacuum
pressures at which the group was able to conduct the experiment were limited. This may be a
factor when the group determines the optimum operating vacuum pressure to separate water
from triethylene glycol to the desired dehydration set point. You also changed the steam
pressure.
9
Apparatus – Andrew Schultz
Major equipment available in the laboratory for pilot tests for this experiment include an
evaporator, separator, condenser, batch reactor, vacuum pump, and recycle pump. The water-
triethylene glycol (H20/TEG) mixture is pumped from a storage tank into a shell and tube heat
exchanger. The H20/TEG mixture enters tube side at the bottom of the exchanger while steam
enters shell side at the top. As the steam condense around the tubes, the process fluid inside the
tubes is heated until water begins to vaporize. As the water vaporizes, the TEG is pushed to the
outside of the tubes and up the column, hence the namesake climbing film evaporator.6 The
water vapor and TEG then enter a vertical separator wherein the heavier liquid TEG flows to the
bottom of the separator into a recycle loop while the water vapor flows out of the top of the
separator to the condenser. Inside the column, the water vapor condenses downward into a batch
reactor. The condensed water is collected and measured via an outlet stream from the bottom of
the reactor. This volume is indicative of the efficiency of the system under the operational
vacuum pressure conditions – that is, the more water that is collected, the more water that is
separated from the TEG. Thus, the more efficient the system is at the specified operating
conditions. The vacuum recycle pumps facilitate the movement of the process throughout the
system. Rewrite last sentence to clarify.
Important operating variables for this experiment include the vacuum pressure of the system,
vacuum pump water flow, and steam pressure entering the evaporator. The group actively
manipulated the vacuum pressure throughout the experiment in order to evaluate the efficiency
of water evaporation from a water-triethylene glycol mixture. This procedure was predicated on
the idea that the boiling point of fluids decrease at higher vacuum pressures. In order to create
the vacuum inside the system, a fluid stream was necessary to cycle through the vacuum pump.
A water stream was used for this purpose. The group determined a water flow rate that allowed
the pump to create sufficient suction such that the desired vacuum pressure was reached without
causing cavitation. The water flow rate was measured by a rotameter located on the operating
panel. This flow rate was held constant throughout for each trial throughout the experiment. The
group also controlled the pressure of the steam entering the evaporator. This procedure was
based on the idea that there would be an increase in steam condensation at increased pressure.
This pressure was controlled by ball valve. The group attempted to keep the steam pressure
10
constant. However, due to the nature of the control valve, the actual steam pressure each day of
experimenting fluctuated somewhat.
For the experiment, the H20/TEG mixture is pumped from a storage tank tube side into the
evaporator while steam is allowed to flow shell side into the evaporator. As the steam condenses
around the tubes, the heat is transferred to the H20/TEG mixture by conduction, which causes the
water to evaporate and move the TEG up the evaporator into the separator. At this point, the
liquid TEG flows to the bottom of the separator and is recycled back into the system while the
water vapor flows to the top of the separator into a condenser. As the vapor liquefies in the
condensing column, it is collected in the batch reactor. The condensed water is then measured
and analyzed to evaluate the efficacy of the separation under the specified operating conditions.
Valves 14 and 15 were manipulated for each trial to control the vacuum pressure inside the
system. Steam pressure was operated at pressures of 17, 18, 19, 20, and 21 pounds per square
inch gauge (psig). These vacuum pressure set points were used in conjunction with the Antoine
equation to determine a calculated (goal) temperature for the TEG in the bottom of the separator.
Additionally, the position of valve -- was manipulated to control water flow into the vacuum
pump.
Safety hazards of concern for the experiment include chemical inhalation or contact, equipment
malfunction, injury by broken or shattered glass, and injury by contact with steam. The primary
chemical of concern for this experiment is triethylene glycol, which is slightly hazardous in cases
of inhalation, but is very hazardous in cases of eye contact.7 Disturbances in water and water-
triethylene glycol flow could potentially cause cavitation in the water vacuum and recycle
pumps, respectively. Conversely, an exceedingly high suction (vacuum) pressure set point could
cause the glass batch reactor to shatter and send glass shards airborne. Scalding while measuring
the condensed water from the batch reactor or burns from the steam are possible hazards while
conducting the experiment as well. The group employed various safety measures to avoid and
protect against the above hazards. These measures include wearing appropriate protective
equipment like pants, long sleeve shirts, and closed-toed shoes to protect our skin from glass
shards and safety glasses to protect our eyes from the same as well as TEG vapor. Additionally,
11
gloves were worn when handling the steam valves and measuring the condensed water to protect
against burns and scalding.
12
Experimental Results – Xiaorong Zhang
Our experimental data showed that a vacuum gauge pressure of 20 inches of mercury obtained the
highest efficiency, which achieved a product of at least 88 percent of triethylene glycol by weight.
Highest efficiency was achieve when the process required the least amount of time to reach the
goal temperature, while consuming the least Experiment #3 Conditions
amount of steam. Barometric pressure 29.2 inHg
741.68 mmHg
Vacuum pressure 20 inHg
Table 3 shows the experimental conditions for 558.8 mmHg
vacuum gauge pressure of 20 inches of Antoine pressure 182.88 mmHg
Temperature goal 84.23954 C
mercury. Other trials were run at similar 183.6312 F
barometric pressure, but different vacuum Start height 24 in
End height 18.75 in
pressures, which led to different temperature
Volume process 25.77527 gal
goals. The goal temperaturesshow an Process time 20 min
increasing trend with decreasing vacuum Thoroughput 77.32582 gal/hr
Scale-up factor, R 48.49609
gauge pressure.
13
the volume of water trend, since less water was evaporated at a higher temperature, which means
less heat was transferred.
Figure 3: Comparison of total steam consumption (in liters) at various vacuum steam
pressures (in inches of Mercury).
Figure 3 shows the steam consumption for each pilot run under different vacuum gauge pressures.
The consumptions for all of the runs, except for at 18 inches of mercury, are around 30 liters.
However, the pilot run at 20 inches of mercury required less process time, which makes it our most
14
desirable run for scale up. For the unexpectedly large steam value for 18 inches of mercury, our
group did not find any apparent reason for this abnormal value.
Propagation of Error
A propagation of error analysis was calculated on throughputs and on the scale-up factor (R).
These two values are the main error sources for the scale up design. The error in the
experimental throughputs is calculated as 46.22±30.88 and R is calculated as 121.34±88.52.
Unfortunately, these errors are large, which affects the scale up design substantially. The cause
of these big errors is that our group had a difficult time measuring the starting and ending height
of the feed tank. Our group will try to figure out a good way to measure the height of the tank
during the make-up experiment for our revised report. Good idea.
Scale Up
Pilot Commercial Size
Factor (r) 48.50
Evaporator SAscale
Table 6: The (ft^2) 1.55 on the pilot experiments.
up factor based 527.69
Cyclone Separator
0.44 21.42
The scaling factor was then
Areaused to scale the throughput as well as triethylene glycol and water
(ft^2)
Condenser
volumetric flow rates. SA (ft^2) were 1.87
These calculations based on the plant633.23
operating 24 hours per day,
Vacuum Pump (hp) 2 96.99
365 days per year and were calculated to meet the dehydration specification of 12 weight percent
water in triethylene glycol. These values are represented below in Table 7.
15
Required Production
System throughput 90,000 [gal/day]
87,424.62 [gal/day]
Triethylene Glycol
329.94 [m^3/day]
2,572.38 [gal/day]
Water Removed
9.71 [m^3/day]
Table 7: Scaled system throughput, triethylene glycol,
and water flow rates.
In evaluating the optimal conditions under which the system should be operated to most
efficiently reach the dehydration specification, the group determined that the most costly element
of the experiment was the cost of steam. Therefore, it was decided to hold the steam input
constant at four pounds per square inch while varying the system vacuum pressure. The Antione
Equation was used to calculate the temperature that was necessary to meet the 88 weight percent
triethylene glycol specification for each variation of vacuum pressure. The time required to reach
this temperature as well as the volume of the triethylene and water mixture processed were
recorded and evaluated to determine the optimal operating conditions. These values are outlined
in Table 8 below.
Tested System Conditions
Vacuum Pressure (inHg) System Temperature (F) Volume Processed (gal) Processing Time (min) Rate (gal/day)
17 208.0 8.5918 27.5 449.8957
18 203.9 8.5918 25 494.8852
19 199.4 30.6848 27 1636.5252
20 183.6 25.7753 20 1855.8196
21 183.6 1.9638 20 141.3958
Table 8: Experimental conditions and results from pilot tests performed at vacuum pressures from 17 to 21
inches of Mercury.
Based on these results, it was determined that the operation of the system was most efficient at a
vacuum pressure of 20 inches of mercury, and this pressure will be used as the basis for the scale
up. At this vacuum pressure, the system has the largest processing rate as well as requiring the
lowest system temperature. This is significant because it is desired to optimize the processing
rate while maintain an economical scale up – that is, process the largest volume of the triethylene
glycol and water mixture at the lowest temperature in order to utilize the least amount of steam
to meet the desired specifications.
16
Equation 2 was manipulated to scale the major equipment to meet commercial specifications.
The major equipment pieces which are necessary to scale up include the evaporator, cyclone
separator, and condenser. The scaled up values for the major equipment is included in Table 9
below.
Scale Up
Pilot Commercial Size
Factor (r) 48.50
Evaporator SA (ft^2) 1.55 527.69
Cyclone Separator
0.44 21.42
Area (ft^2)
Condenser SA (ft^2) 1.87 633.23
Vacuum Pump (hp) 2 96.99
Table 9: Scaled up values for major equipment.
The scaled up equipment costs were estimated using the CAPCOST cost analysis program.
Additional costing methods (e.g., cost of labor, raw materials, etc.) and correlations were derived
using Analysis, Synthesis, and Design of Chemical Processes by Turton et al. All correlations
and costing analyses should be consistent between CAPCOST and the textbook since the
program was designed by the authors of the textbook. Furthermore, all correlations are based on
industry averages and do not require the use of corrective factors.
17
EXPENSES
Total Manufactoring Costs General Expenses
Raw Materials $ 883
Labor $ 468,000.00 Administrative Costs $ 111,000.00
Utilites $ 828,000.00
Maintenance $ 223,000.00 Distribution & marketing $ 351,000.00
Operating Supplies $ 33,500.00
Laboratory Charges $ 70,200.00 Research & development $ 159,000.00
Royalties $ 115,000.00
Depreciation $ 318,000.00
Taxes $ 100,000.00
Insurance $ -
Rent $ -
Totals $ 2,156,583.00 $ 621,000.00
18
Process Flow
Diagram -
Nadezda
Mamedova
19
Propagation of Error Analysis – Eric Henderson
Propagation of error analysis sample hand calculations for the following table can be found in
Appendix III.
Overall, our error in equipment size yielded a very small standard deviation; therefore, our scale
up calculations are confirmed to be precise. Our average experimental error was found to be less
than five percent for all data in question. Consequently, our data are confirmed to be statistically
significant.
Due to time constraints, our data gathered were not all started at the same temperature. If more
time is allowed, we recommend running the experiment from the same temperature and
atmospheric pressure to allow for better comparisons.
The largest limitation to our experiment was the start and end height of the liquid level in ….,
which we used to calculate the amount of liquid processed. Errors in the amount of liquid processed
would carry through all the calculations and cost analysis.
20
Comparison with Design Based On Literature Values – Andrew Schultz
An experiment was conducted using an industrial climbing film evaporator to concentrate
pineapple juice for widespread commercial purposes. In Bourgois and LeMaguer’s experiment,
the evaporator had three sections, each being similar in length (2.13 meters) with differing
quantities of tubes – 66, 111, and 156. In total their system had a processing capacity of over
5,000 kilograms per hour or 120,000 kilograms per day. For our purposes, we are processing an
inlet feed of 90,000 gallons per day, so both systems are analogous in total processing
capabilities per day. Further, the overall heat transfer coefficient for our triethylene glycol
system was calculated to 26.31 kilojoules per square foot per degree Celcius or 283 Watts per
square meter per Kelvin, which is dissimilar to the calculated range Bourgois and LeMaguer
determined for their industry pineapple juice application (1,000 to 1,600 Watts per square meter
per Kelvin). This source of error do you mean differences or errors or both? could derive from
the measured tank height, compositional differences between triethylene glycol and pineapple
juice, the dehydration versus concentration processes not being directly comparable, as well as
improved present-day equipment compared to the equipment Bourgois and LeMaguer had
available.
21
Report Grade: 87/100
References
1. Aschner, F.S. & Schaal, M. & Hasson, D. (1971). “Large Long-Tube Evaporators for
Seawater Distillation”.
2. “Evaporation Handbook”, 4th edition, An Invensys Company, APV Americas, Engineered
Systems Separation Technologies. [1] Last Accessed on 4 October 2015
3. Bourgois, J., & LeMaguer, M. (1984). Modelling of Heat Transfer in a Climbing-Film
Evaporator: Application to an Industrial Evaporator. Journal of Food Engineering , 39-50.
4. Triethylene Glycol Manual (n.d.): n. pag. DOW Chemical, Feb. 2007.
5. Turton, Richard. Analysis, Synthesis, and Design of Chemical Processes. Upper Saddle River:
Prentice Hall, 2014. Print.
6. “Evaporation Handbook”, 4th edition, An Invensys Company, APV Americas, Engineered
Systems Separation Technologies. [1] Last Accessed on 4 October 2015
7. "Triethylene Glycol MSDS." Material Safety Data Sheet (MSDS). Science Lab, 21 May 2013.
Web. 6 Oct. 2015. <http://www.sciencelab.com/msds.php?msdsId=9927307>.
22
Vacuum Pressure = 21 inHg
Appendix I: Data Tables –
23
Commercial Process
Evaporator
Surface area 6925.902 ft2
Eric Henderson
Commercial Process
Evaporator
= 20 inHg
Commercial Process
Evaporator
= 19 inHg
Commercial Process
Evaporator
= 18 inHg
Commercial Process
Evaporator
= 17 inHg
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Appendix III: Error Calculations – Nadya Mamedova
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Appendix IV: Scale Up Calculations – Eric Henderson
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