MEMORANDUM

TO:
FROM:
DATE:
SUBJECT:

DanielGroom
ClaytonGregoryandAntonioHernandez
08June2015
DistillationOperationDraftReport

Introduction:
Themainobjectiveforthisexperimentisforthestudentssogainexperienceoperatingand
controllingindustrialdistillationequipment.Also,itisimportantforthestudentstolearnhowto
performfieldoperationalcapacitytestsofacolumnandunderstandthetheorybehindacolumns
floodpointandcolumnfloodingingeneral.Theexperimentwilloperatethecolumnatatotal
refluxcondition,obtainsamplesfromthereboiler,eachtray,andtheaccumulator,andanalyze
eachsampleinagaschromatographer.McCabeThielediagrams,Murphreeefficiencyequations,
andtraycompositionswillbeusedtodeterminetheefficiencyofthecolumn.
Methods:
Distillationscolumnsareusedtoseparatedifferentcomponentsofamixturebasedonthe
differencesintheboilingpointsofsuchspecies.Thecomponentsusedintheexperiment,water
andethanol,haveboilingpointsof100Cand78C,respectively.Themixtureofwaterand
ethanolformsanazeotrope,meaningthecompositionofthevaporandthecompositionofthe
liquidaredirectlyproportional.Theuseofanoptimumnumberoftraysinaseparationcolumn
canincreaseefficiencyandpurityoftheseparatedcomponents.
Themethodsandtheorygivenintheexperimentguidewereused.

PreLabQuestions:
1)
Thefloodingvelocitiesatthebottomofthecolumnandatthetopofthecolmnwere
3.01m/sand1.31m/s,respectively.
2)
Flooding Percentages
Steam Flow Rates (kg/min)

0.5
0.8
1
1.25
0.431773 0.690836 0.863546 1.079432

3)
The first part of the column to flood will be towards the top, since vapor entrains liquid in
its flow toward the top of the column (Pless, et al., 2002). From there, flooding will spread.
This answer was confirmed by experimental results; the flooding velocity (0.90 kg/min) is
closer to the value predicted by calculating for ethanol than the value predicted by
calculating for water.

4)
As the steam rate is increased, the vapor velocity and flow up the distillation column
increases, restricting the flow of liquid down the column. This results in the increase of
pressure drop (P) across the column.
Flooding occurs when the internal vapor rate is so high that the liquid is unable to flow
down the column. When flooding occurs in the distillation column, there is a very large
pressure drop (P) on the P curve.
5)
Entrainment is defined as the entrapment of one substance by another substance. In the
context of the experiment, vapor at high rates entrains the downward-flowing liquid. In
comparison, down-comer flooding occurs when the liquid backs up into the down-comer
due to a large pressure drop across the tray. When the back-up liquid in the down-comer
exceeds the tray spacing, liquid accumulates on the tray above.
8)McCabeThielePlots
a.Totalreflux4theoreticalstages
b.Murpheeefficiencyof0.82theoreticalstages

c.RefluxRatioof1.86theoreticalstages

Total Reflux
1.20

1.00

0.80
Equilibrium Line
45 degree line

0.60

0.40

0.20

0.00
0.00

0.20

0.40

0.60

0.80

1.00

1.20

Murphree Liquid Efficiency of 0.82

1.20

1.00

0.80
Equilibrium Line
45 degree line

0.60

0.40

0.20

0.00
0.00

0.20

0.40

0.60

0.80

1.00

1.20

Reflux Ratio of 1.8

1.20

1.00

Equilibrium Line

0.80

45 degree line
Rectifying Line
0.60

Stripping Line
q-Line

0.40

0.20

0.00
0.00

0.20

0.40

0.60

0.80

1.00

1.20

Appendices
AppendixA:Safety
Overall Hazard Analysis
Description/
Details of steps in
activities
Usage of ethanol
for distillation
experiment

Hazards

Possible accidents/
consequences

Existing Risk
Control

Fire/ explosive
hazard

May result in a fire

or explosion that
may cause burns,
other injuries and
even death.

1) Donning of PPE
such as safety
goggles, lab coats
and hard hats.
2) Cooling water
have be flowing
before the steam
valve is opened.
3) Noting location

of manual steam
valves and main
shut-offs in the
event of an
emergency.
Gas cylinders of
gas chromatograph
are pressurized
during experiments

Explosion /
cracking due to
pressurized
cylinders

May cause burns

and other injuries.
Projectiles flying at
high speed in the
event of an
explosion may hit
operators.

Distillation column
may be subjected
to overpressure
(excessive pressure
beyond what the
column is designed
for).

Explosion or
cracking of the
column due to high
pressure.

May cause burns

and other injuries.
Projectiles flying at
high speed in the
event of an
explosion may hit
operators.

Handling of hot
valves or surfaces
of hot objects.
Accidental contact
with steam pipes.

Burn hazard

May cause varying

degrees of burn
injuries.

Climbing the
column stairs

Sharp edges

May cause cuts or

lacerations.

Handling of

Electrical hazard

Electrocution and

1) Donning of PPE
such as safety
goggles, lab coats
and hard hats.
2) Ensuring
pressure values are
appropriately
monitored and
within the safe
limits.
3) Ensure cylinder
is properly
mounted and
chained.
1) Column is
protected against
overpressure by
pressure relief
devices such as
relief valves.
2) Donning of PPE
such as safety
goggles, lab coats
and hard hats.
Donning of PPE as
well as thick
gloves. Be alert
when in close
proximity of steam
pipes and other hot
surfaces.
Use care when
climbing the
column stairs. Be
careful not to back
into stairs when
working under
them.
Check for any

electrical hazard
during experiment
and data collection
purposes.

electric shocks.

damaged electrical
equipment or wires
and any liquid
pools near
electrical
connections.

MSDS (Ethanol)
Description:
Colorless clear liquid with a mild odor.

Flammable liquid and vapor. Flash point = 16.6C.

Molecular weight = 46.0414 g/ mole, Boiling point (1 atm) = 78C, Melting point =
-114.1C, Solubility: Miscible

Health Effects:
Causes severe eye irritation and moderate skin irritation when coming in contact.

Ingestion may cause gastrointestinal irritation with nausea, vomiting and diarrhea.
May cause central nervous system (CNS) depression characterized by excitement,
followed by headache, dizziness, drowsiness and nausea.

Causes respiratory tract irritation, dizziness or suffocation when inhaled.

May have an adverse reproductive and fetal effects in humans. Prolonged exposure
may also cause liver, kidney and heart damage.

First aid:
For eye contact, remove any contact lenses and immediately flush eyes with plenty
of water for at least 15 minutes. Get medical attention immediately.

For skin contact, immediately flush skin with plenty of water for at least 15 minutes
while removing contaminated clothing and shoes.

Do NOT induce vomiting when ingested. Give the victim 2-4 cupfuls of milk or
water if he is conscious and seek medical attention.

Storage & Handling:

Container should be tightly closed and kept away from heat, sparks and flame.
Keep away from sources of ignition and contact with oxidizing materials. Store in a
cool, dry, well-ventilated area.

MSDS (Water)
Description:

Colorless, odorless liquid

Molecular weight = 18.02 g/ mole, pH (1% soln/water) = 7 (Neutral), Boiling point

(1 atm) = 100C (212F)

Health Effects:
Non-corrosive for skin, non-irritant for skin. Non-sensitive for skin. Non-permeator
by skin. Non-irritating to the eyes. Non-hazardous in case of ingestion. Nonhazardous in case of inhalation. Non-irritant for lungs. Non-sensitive for lungs.
Non-corrosive to the eyes. Non-corrosive for lungs.

First aid:
Not applicable

Storage & Handling:

Not applicable

AppendixB:References
Friedman,K.(2015,Summer).DistillationOperationExperiment.LabHandoutChE264,The
UniversityofTexasatAustin.
Green, D.W., ed. (1984). Perrys Chemical Engineering Handbook. Sixth Edition. McGraw-Hill
Book Company, New York.
McCabe, W. L., Smith, J. C., & Harriott, P. (2005). Unit Operations of Chemical Engineering (7th
ed.). Boston: McGraw Hill.
Pless, L., & Xu, S. X. (2002, June). Distillation tower flooding--more complex than you think:
while other predictive methods tell too little, too late, gamma scans indicate where and
why flooding occursinvaluable insight for troubleshooters. (Feature Report). Chemical
Engineering, 109(6), 60+.
Smith, J.M. and H.C. Van Ness. (1975). Introduction to Chemical Engineering Thermodynamics,
Third Edition. McGraw-Hill book company, New York.
Weast, Robert C., et al. ed. (1985). CRC handbook of Chemistry and Physics, 66th Edition. CRC
Press, Boca Raton, FL.
AppendixC:SampleCalculations
FloodingVelocity:

Floodingvelocitycalculationatthebottomofthedistillationcolumn:
Assumption:PureWaterPhysicalProperties
V F =C F

( L G )
G

Where:

VF=FloodingVelocity(m/s)
CF=EmpiricalConstant(m/s)
L =LiquidDensity(g/cm3)
G =VaporDensity(g/cm3)

C F =0.075

m
g
=0.95
s L
c m3

Vapordensitycalculationusingtheidealgaslaw:
Assumption:PureEthanolPhysicalProperties
G =

P MW
RT

( 1 atm ) 18.02
G =

g
mol

L atm
( 373.15 K )
(0.08206 mol
K )

V F = 0.075

m
s

g
g
=0.5885 =5.89 104
L
c m3

( 0.955.89 104 )
4

5.89 10

=3.01

m
s

Floodingvelocitycalculationatthetopofthedistillationcolumn:

( 1atm ) 46.07
G =

g
mol

L atm
( 351.55 K )
(0.08206 mol
K )

g
g
=1.597 =1.597 103
L
c m3

m
V F = 0.059
s

( 0.7891.597 103 )
3

1.597 10

=1.31

m
s

SteamFlowRates:
Steamflowratecalculationusinganenergybalancearoundthereboilerat50%flooding:
msteam =

H vap ,ethanol V top

H vap , steam

Where:

fA G V F
V
=
top

MW

msteam =

Therefore:
Where:

f=FractionofFlooding(unitless)
A=ColumnArea(cm2)
G=DensityofEthanolVapor(g/cm3)
VF=FloodingVelocity(cm/s)
MW=MolecularWeightofEthanol(g/mol)

9674
m steam =

msteam =0.432

H vap ,ethanol f A G V F
H vap , steam MW

cal
cm
2
2
3 g
0.5 7.5 c m 1.597 10
131
3
gmol
s
cm
kg s
1.081
cal
g
mol min
9718
46.07
gmol
mol

kg
min

AverageMolecularWeight:

AverageMolecularWeightcalculationofthefeedstream:
x

W ij
M

M W feed =

Where:
x ij=mass fraction of component istream j

[|

||

0.32 g ethanol mo l ehtanol

0.68 gwater mol water
M W feed =
+
g feed
46.07 g ethanol
gfeed
18.02 gwater

AverageMolarFlowRate:
AverageMolarFlowRatecalculationofthefeedstream:
j 1

n j=m j ( M W )

Where:

n j=mol ar flow rate of stream j

j=mass flow rate of stream j
m

n feed=

35 kg feed kgmo l feed

kgmo l feed
=1.56
min 22.38 kg feed
min

AverageMoleFraction:
AverageMoleFractioncalculationofthefeedstream:

|]

=22.38

gfeed
mo l feed

W ij
M
j
i ( i1 ]

j
Wi
M
j
i ( i1 ]

W ij
M

y ij=

yE =

(|

0.32k gethanol kgmo l ethanol

k g feed
46.07 k g ethanol

|)(

22.38

k g feed
kgmol ethanol
=0.16
kgmo l feed
kgmol feed