ENGINEERING 536

MASS TRANSFER
OPERATIONS
FALL 1997

TEAM MEMBERS:
Dr. Jim Henry, P.E.
Sean Cunningham
Mark Koss, P.E.
Sandy Koss
Tara Ostrander, E.I.
Nittaya Pittayataree
Beth Ruta
Nitipol Suksathaporn
 Introduction
 Study of mass transfer operations
using the distillation column
 Approach to the study of the
distillation column included
- Literature search
- Operating the column
- Computer modeling
+ Ponchon-Savarit
+ PROII

 This report will cover

- column calibrations
- experimental results
- computer modeling
 DISTILLATION COLUMN
TI

Cooling Water Supply

Condenser
TI
TI
Cooling Water Return
Electromagnetic Reflux Control
TI
1 Product Cooler
TI
2
TI 3
LI
TI
4 Distillate
TI 5
Pump
TI TI
6
TI Feed Tank
7
(Product Tank)
TI
8 Feed Pump
TI 9

TI
10
TI 11
PI
TI
12
Reboiler
TI LI

Reboiler Pump
COLUMN DESCRIPTIONS
 Condenser
 Reflux valve
 Trays
 RTDs
 Pumps
- Feed pump
- Reboiler pump
- Distillate pump
- Auxiliary pump
 Reboiler
 Level Control
- Condenser
- Reboiler
 FEED LOCATIONS
Column Calibrations

 Heat loss study

 RTD calibration
 Pump and cooling water
calibration
Heat Loss Study
 Previous heat loss calculations
seemed excessive
 Parameters of the study are
- selected reboiler amperage
- 100% reflux
- no condensate produced
 Column losses are equal to the
energy input into the column
 Minimum amperage to maintain the
temperature on tray 1 is between 6
and 7 amps
 Estimated column heat loss is
between 1230 Watts and 1435 Watts
 Temperature of tray 1 at 7 amps
Reboiler Amps = 7

Temperature (C) 66.0

65.8

65.6
65.4

65.2
65.0
70 72 74 76 78 80
Time

Temperature of tray 1 at 6 amps

Reboiler Amps = 6

65.5
Temperature (C)

65.0

64.5
64.0
63.5
63.0
78 79 80 81 82 83 84 85
Time
RTD Calibration
 Temperature is calculated by
multiplying the voltage by the
scale and then adding the offset
 Steps to calibrate RTDs

- fill reboiler with pure

methanol
- allow steady state
- set offset to zero
- set scale to one
- collect voltage readings
- repeat with water
 Voltage is taken at 100oC (pure
water) and 64.5oC (pure
methanol)
 Straight line was fit between
the two points
 Slope of the line is the scale
 y intercept is the offset
 Pump and Cooling Water
Calibration

 Pump and cooling water

calibrations seem to be reliable
 Pump calibration
- by measuring the outflow
of the pump for a timed
period
 Cooling water calibration
- by measuring the flow at
the cooling water system
drain at various valve
openings
Pump Calibration Curve

Feed Pump Calibration Curve

600
Flowrate (ml/min)

500
400
300 2
F = -2.3996M + 98.326M - 81.102
200 2
R = 0.9942

100
0
0 2 4 6 8 10
Pump : 7017-21 Pattern No. 3.358.609 Pump S etting
Conclusions
(calibrations)

 Pump and cooling water

calibrations seem to be reliable
 Calibrations performed on the
glass RTDs were unsuccessful (
repeated several times)
 Replacement of the glass RTDs
with stainless steel improved the
calibrations
- three RTDs do not give
reliable temperature
indication
Recommendation
(calibrations)

 Perform calibrations
- after a period of inactivity
- whenever equipment is changed
or modified
 Reduce time spent on
calibrations
- Calibrate the RTDs individually
with ice and boiling water
- UTC engineering/maintenance
personnel should complete
calibrations
Experimental Results

 Energy and mass balance

 Capacity test
 Feed location impact
 Reflux ratio impact
Energy and Mass
Balance

 Excel spreadsheet was developed to

facilitate mass and energy
calculations
 Calculations showed an increase in
water and a decrease in methanol
 Column had not reached steady-
state conditions
Flowrate (gms/min)
Mixture Methanol Water
Feed 321 315 12
Bottoms 205 168 12
Distillate 116 147 0
 DISTILLATION COLUMN EXPERIMENT (10/15/97)
MASS BALANCE
Inputs
Reflux Ratio= 1.78 Tank Temp= 30.00
Distillate: Reboiler: Feed:
Pump Setting: 1.20 Pump Setting: 2.10 Pump Setting: 5.00
RTD Reading: 64.57 RTD Reading: 75.67 %MeOH(Molar): 0.50
Density: 0.79 Density: 0.94 Density 0.92

Distillate Reboiler: Feed Pump:

%MeOH (Molar) 99.55 %MeOH (Molar) 39.15 %MeOH (Molar) 50.00
Frac (Wt) 1.00 Frac (Wt) 0.53 Frac (Wt) 0.64
Flow Rate (ml/min) 15.05 Flow Rate (ml/min) 336.57 Flow Rate (ml/min) 350.54
Mass flow rate (g/min) 11.91 Mass flow rate (g/min) 315.13 Mass flow rate (g/min) 320.95
Mass MeOH (g/min) 11.88 Mass MeOH (g/min) 168.14 Mass MeOH (g/min) 205.41
Mass H2O(g/min) 0.03 Mass H2O(g/min) 147.00 Mass H2O(g/min) 115.54

water balance 31.48 gm/min

MeOH balance -25.39 gm/min

ENERGY BALANCE
ENERGY IN AT REBOILER
Reboiler (Amps) 15.43
Energy In(watts) 3394.60

CONDENSER RE BOILER
Cool Water Temp-in(°C) 19.74 Delta T 45.67
Cool Water Temp-out (°C) 20.63
Cool Water Flow (ml/min) 9000.00
Water Cp (KJ/KgoK) 4.18 MeOH Cp 2.55
Energy Out Cond(watts) 557.94 Qcond Reboiler Energy 794.47 Qr
Latent Heat(watts) 615.07 Qlatent
Capacity Test

 Performed to determine the

maximum capacity of the
column to produce distillate
 Parameters for the test are
- reboiler was filled with a mixture
of methanol and water
- reboiler current set at 20 amps
(maximum)
- reflux set 95 % Methanol distillate
- steady-state conditions were
established
- Set various feed pump settings
- Set various reflux ratios
- Determine distillate and reboiler
flowrate
- Column did not produce distillate at
pump setting of 7
Capacity Test Comparison
Feed Pump Feed Flowrate Percent Distillate Reboiler
Setting (ml/min) Reflux Flowrate Flowrate
(ml/min) (ml/min)
3 192 76 25 180
5 350 75 32 332
6 420 76 21 390
7 490 - - -
Feed Location Impact

 Parameter
- Pump setting of 3
- Reboiler amps at 20
- 70% reflux
 Results
- Tray 4 - 89%
- Tray 5 - 93%
- Tray 6 - 97%
Reflux Impact

 Parameter
- Feed location tray 4
- Pump setting of 3
- Reboiler amps at 20
 Results
- Reflux 50% - 78% at 43
ml/min
- Reflux 70% - 89% at 23
ml/min
Conclusions
(Experimental Results)

 Design and execution of

experiments
- useful way of gaining experience
- found column performed in a
predictable manner
- increased the students’ level of
confidence
 energy and mass balance
calculations demonstrated
- purity of the product was surpassed
with a reduction in the quantity of
the product
 Based on observations from the
capacity test
- maximum output of the reboiler heaters
could not maintain boiling conditions
above a feedwater flowrate of 420ml/min
 Based on observations from the
feed location experiment
- optimum feed tray location - tray 6
- due to the higher methanol composition
in the distillate
 Based on observations from the
percent reflux experiment
- between 50- and 70-percent reflux
* two times the distillate flowrate
* 1.6 times the amount of methanol
Recommendation
(Experimental Results)

 Review the RTD calibrations to

account for the discrepancies
in the mass balance
 Perform additional feed
location impact experiments
 Take physical measurement of
the distillate flow (not pump
flowrates)
Computer Modeling

 Pro II
 Ponchon-Savarit
PRO II

 Steady-state heat and material

balance simulator
 Simulates any number of
components, streams, units,
and recycle loops
 Requirement
- Feed stream
- composition
- temperature
- flowrate
- pressure
- Tray efficiency
 Specify two of the following
parameters

- Any specific tray temperature

- Heat duty of the condenser
- Temperature of the distillate
- Composition of the distillate
- Flowrate of the distillate
- Reflux ratio
- Temperature of the bottoms
- Composition of the bottoms
- Flowrate of the bottoms
- Heat duty of the reboiler
 PROII will calculate remaining
parameters
PRO II - Optimizing Distillation Column
Stream Name 1 2 3
Stream Description
Phase Liquid Liquid Liquid
Temperature C 25 65.53888 99.82745
Pressure ATM 0.994603 0.994603 0.994603
Flowrate G-MOL/MIN 12.00385 6.488153 5.515693
Composition
MEOH 0.5 0.925 6.91E-05
H2O 0.5 0.075 0.999931
Total Stream
Rate G-MOL/MIN 12.00385 6.488153 5.515693
G/MIN 300.4381 201.0676 99.37048
Std. Liq. Rate CM3/MIN 350 250.4837 99.51627
Temperature C 25 65.53888 99.82745
Pressure ATM 0.994603 0.994603 0.994603
Molecular Weight 25.0285 30.98997 18.01597
Enthalpy M*J/MIN 0.023033 0.034942 0.041537
J/G 76.66611 173.7827 417.998
Mole Fraction Liquid 1 1 1
Reduced Temperature 0.514083 0.647976 0.576169
Reduced Pressure 0.006671 0.011017 0.004556
Acentric Factor 0.45835 0.552148 0.348015
UOP K-Value 9.962891 10.55651 8.76176
Std. Liquid Density G/CM3 0.858395 0.802717 0.998535
Sp. Gravity 0.859242 0.803509 0.999521
API Gravity 33.18008 44.60248 10.06786
Vapor
Rate G-MOL/MIN n/a n/a n/a
G/MIN n/a n/a n/a
CM3/MIN n/a n/a n/a
Molecular Weight n/a n/a n/a
Z (from Density) n/a n/a n/a
Enthalpy J/G n/a n/a n/a
CP J/G-C n/a n/a n/a
Density G/CM3 n/a n/a n/a
Th. Conductivity KCAL/HR-M-C
n/a n/a n/a
Viscosity CP n/a n/a n/a
Liquid
Rate G-MOL/MIN 12.00385 6.488153 5.515693
G/MIN 300.4381 201.0676 99.37048
CM3/MIN 352.8752 265.9261 103.6818
Molecular Weight 25.0285 30.98997 18.01597
Z (from Density) 0.001195 0.001467 0.000611
Enthalpy J/G 76.66611 173.7827 417.998
CP J/G-C 3.115483 2.895487 4.21597
Density G/CM3 0.851401 0.756103 0.958418
Surface Tension DYNE/CM n/a n/a n/a
Ponchon-Savarit Theory

 Graphical Method
• Plots Enthalpy Against
Composition
 Provides Exact Solutions
 Incorporates Effects of Heat
Losses
• Inputs of Individual Tray Losses
• Inherent Material and Energy
Balances
Ponchon-Savarit
Diagram on Excel

 Inputs Needed (highlighted in

yellow)
• Distillate and Bottoms
Compositions Desired
• Distillate and Bottoms Flowrates
• Heat Losses on Each Tray
 Works For Up To 13 Stages
 Tested For Bottoms
Concentrations down to 0.01%
and Distillate Concentrations up
to 97.9%
Conclusion
(Computer Modeling)

 PROII
- user friendly
- fast
- not accurate
- limited by constraints

 Ponchon-Savarit
- heat loss on individual trays
must be known
- only valid for methanol-water
mixtures
Recommendations
(Computer Modeling)

 Modify the PROII model to more

closely approximate the UTC
distillation column
 Conduct training for students
on the use of modeling tools
 Determine the heat losses on
the individual trays (Ponchon-
Savarit)
Conclusions
(Final)

 Technical
- Study of mass transfer operations
using the distillation column
- Approach to the study of the
distillation column included
- Literature search
- Operating the column
- Computer modeling
* Ponchon-Savarit
* PROII
- Each student had the opportunity
to participate in
- operation
- calibration
- repair
- Provided a better understanding
through
- research
- classroom discussion
- design of experiments
 Accomplishments
- Ponchon-Savarit spreadsheet
developed
- PROII model developed
- Energy and mass balance
spreadsheet developed
- Determination of the column
capacity
- Determination of heat lost to the
environment
- Performed feed input experiments
Recommendations
(Final)

 Allow for more continuous

laboratory time
- Modify class schedule
- Maintain the distillation column
components
- Establish course objectives,
perform calibrations, research
literature, and familiarize
students with modeling programs
within the first month of the
semester