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Evaporative Concentration of a Thermally Sensitive Chemical
Chen 4450 Process SafetyAuburn UniversityNovember 27, 2006
Guest SpeakerRobert D’Alessandro, P.E.Director of Process EngineeringDegussa Corporation
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Introduction
Five Main Principles of Inherently Safer Chemical Plants:
Limitation of Effects
Use equipment fit for its service
Webster: Existing in something as an inseparable element.
Synonyms: Innate, native, inbred, ingrained
Substitution
Use safer chemicals
Simplification
Use less complexity
An Integral Part Of
Attenuation or Moderation
Use the least hazardous conditions
Intensification or Minimization
Use less hazardous chemicals
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Lecture Objectives
Recognizing potential reactivity problems
Safety aspects of connected equipment
Safety instrumented systems
Adiabatic calorimeters for obtaining proper data
Gassy systems versus tempered systems
Vapor-liquid disengagement in vessels
Two-phase venting versus “all vapor” venting
Introduction to the following process safety related concepts:
Reactive System
Pressure Relief
ExampleEvaporative
Concentration of a
Thermally Sensitive ChemicalIntegrating process safety into process design
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Evaporative Concentration
Process Flow Diagram - RA 2nd Stage Concentration
Steam60 psig
Z-100Three Stage Steam
Jet Vacuum System
Chilled Water5 C
T
70 wt% RAFrom 1st StageConcentration
Steam150 psig
Process OffgasTo Thermal Oxidizer
90 wt% RATo Crystalazer Chilled Water
5 C
Process CondensateTo Treatment
Note 1: Barometric LegNote 2: Equilization LineNote 3: 3 Barometric Legs
P
L
L
RO
F
T
R-100
P-100
A-100X-100
V-101
P-101
X-101
83 C
70 C
15 C
20 C
20mmHgA
2,500 PPH
1,944 PPH
Cond.
250 PPH
806 PPH
10mmHgA
16.7psia
16.7psia
1 32
575,200Btu/hr
308,800Btu/hr
21.7 C
15.2 C
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Signs of Inherent Trouble
“70 wt% RA begins, at what the chemists describe as, a slow decomposition when temperatures exceed 120 °C.”
Be suspicious of “normal” laboratory data
“The chemists also noted some foaming when this slow decomposition occurred.”
Hints from Chemists or Operators
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Signs of Inherent Trouble
MSDS – Material Safety Data Sheet:Excellent source of general safety information
OSHA type data is good – hygiene, PPE, medical, fire fighting, etc.
Physical property data is usually good
“MSDS for 70 wt% RA also indicates this temperature limit.”
However, my experience indicates:Reactivity data is lacking and sometimes wrong
Better now then in the past, but still needs improvement
Better for common petrochemicals then for specialty chemicals
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Signs of Inherent Trouble
The hints from the chemists tell us that additional data is needed.
What kind of data?
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Laboratory Scale Data
Consider:A typical organic fluid at 80 °C in some container
Surrounded by still air at 20 °C
Factor 10,840
Bottom Line = Heat Loss
Small Scale Has It
Large Scale Doesn’t
?? WHY ??
Laboratory Heat LossEquipment Btu / Hour / Lb
Test Tube10 ml
Beaker100 ml
Cooling Rate°C / Minute
0.09
0.06
542
341
Full Scale Heat LossEquipment Btu / Hour / Lb
Reactor660 gallons
Reactor6600 gallons
0.048
0.004
4.6
0.05
Cooling Rate°C / Minute
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Surface Area to Volume Ratio
0.0
1.0
2.0
3.0
4.0
5.0
6.0
7.0
8.0
0.001 0.010 0.100 1.000 10.000 100.000 1000.000
Volume (Gallons)
Surf
ace
Are
a / V
olum
e (S
F/G
allo
n)
L / D = 1
L / D = 4
3.8 ml 38 ml 380 ml 3800 ml (S/V)Lab Scale >>> (S/V)Commercial Scale
Heat Generation ~ Volume of Contents
Heat Loss ~ Surface AreaSmall Scale Experiments Must
Eliminate Heat Loss
Surface AreaVolume Volume Ratio
10ml
100ml
1000gallons
5000gallons
124
57
2
1
10.5
4.9
0.145
0.085
Laboratory Scale Data
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Laboratory Scale Data
Two Forms of Heat LossBoth are magnified by large surface to volume ratios
Heat loss to the sample container caused by thermal capacity of test cell.
CapacityCarryingHeatSampleCapacityCarryingHeatSystem
≡Φ Phi Factor
tpftf
pbb
tpftf
pbbtpftf
CmCm
CmCmCm
+=+
≡Φ 1
If ThenTUAQ Δ=
Heat loss to surroundings caused by temperature difference .
0=ΔT 0=Q
Decrease Test Cell Mass
Increase Sample Mass
Commercial Vessel Phi Factor = 1.05 to 1.10Goal for Small
Scale Equipment
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Adiabatic Calorimeters
ARC – Accelerating Rate Calorimeter
Invented by D.I. Townsend at Dow Chemical in the late 1970s
Solved the ΔT problem
But not the thermal inertia problemHeavy Wall Test Cell
Containment T
Sample T
Heating Elements
Containment Vessel
Can not track very fast reactions
Very sensitive at low reaction rates
Still has important applications
High Thermal Inertia Adiabatic Calorimeter
Phi Factor: 2.0 ≤ Φ ≤ 4.0
Heavy wall test cell
Built to withstand internal pressure
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Adiabatic CalorimetersLow Thermal Inertia Adiabatic Calorimeters
Invented by DIERS in the early 1980s
Solved the ΔT problem
Solved the thermal inertia problem
Can track very fast reactions
Not sensitive at low reaction rates
Phi Factor: 1.05 ≤ Φ ≤ 1.15
Thin wall test cell
Pressure compensation prevents test cell rupture
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Adiabatic CalorimetersLow Thermal Inertia Adiabatic Calorimeters
Containment vessel isolation ball valve
Containment Vessel Pressure Transducer
Test Cell Pressure Transducer
“Super”Magnetic Stirrer
Auxiliary Fill Line
Rupture Disk(1900 psig)
3-Way ValveFilling Test Cell
or Pressure Equalization
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Adiabatic CalorimetersLow Thermal Inertia Adiabatic Calorimeters
Thin Walled Low Thermal Inertia Test Cell
Insulation for Maintaining Adiabatic Conditions
A View of the InsidePressure Containment
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
The type of data that is needed is now known!
The experiment must now be specified.
Evaporative Concentration
Data from a Low Thermal Inertia Adiabatic Calorimeters
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Tempered Versus Gassy SystemsTempered Liquid Phase Systems:
T & P related directly to each other via the vapor pressure of components
In Open Systems:Heat generation or addition causes vaporization of components
Vaporization provides liquid phase cooling
When vapor removal is sufficient, T (and P) stops increasing
In Closed Systems:Essentially no vaporization occurs
Pressure increases in step with increasing temperature
Examples of Tempered Systems:Styrene polymerization
Methanol vessel under fire
Blowdown of a vessel containing liquid propane
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Tempered Versus Gassy SystemsGassy Liquid Phase Systems:
Non-condensable gases are present or formed by reaction
T & P are not simply related by the vapor pressure of the components
In Open Systems:Heat generation or addition does not cause vaporization
Cooling effects from vaporization do not occur
Instead, the sensible heat content (temperature) of the liquid increases
Examples of Gassy Systems:Decomposition of some organic peroxides
Decomposition of some polymers
Blow-down of a subcooled liquid containing dissolved gas
In Closed Systems:Pressure increases almost without bounds
Rossonic Acid Decomposition
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Experimental Specification
Testing 90 wt% RA in a Low Thermal Inertia Adiabatic Calorimeter:Stainless Steel Open Test Cell
Containment Backpressure = 300 psig
Charge = 90 g (Fill ~ 75%) (Phi Factor ~ 1.1)
Hold at 70 °C
Test Normal Operating Condition
Heat (4 °C Increments) and
Search (5 minute holds)
Until self-heating is observed
Convert to adiabatic mode
Allow test cell to self cool
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Adiabatic Calorimeter Data
Temperature Versus Time
50
75
100
125
150
175
200
225
250
0 2000 4000 6000 8000 10000 12000 14000
Time (seconds)
Tem
pera
ture
(C)
Heat & Search
Normal Operating Condition
Self-Heating Detected
∆T ~ 120 °C
Adiabatic Operation
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Adiabatic Calorimeter Data
Pressure Versus Time
250
275
300
325
350
375
400
425
0 2000 4000 6000 8000 10000 12000 14000
Time (seconds)
Pres
sure
(psi
a)
Containment Pressure
Self-Heating Detected
Pressure Rise ~ 90 psiClosed Test Cell ~ 12,000 psi
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Adiabatic Calorimeter Data
Self Heat Rate Versus Recipricol Temperature
0.01
0.10
1.00
10.00
100.00
-3.0 -2.9 -2.8 -2.7 -2.6 -2.5 -2.4 -2.3 -2.2 -2.1 -2.0 -1.9 -1.8 -1.7 -1.6 -1.5
Recipricol Temperature
Self
Hea
t Rat
e (C
/min
)
110 C
94 C
Heat & Search
Based on Lab Data
Onset Temperature
Maximum Self-Heat Rate 80 °C/minute
Second Reaction
ArrheniusKinetics
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Adiabatic Calorimeter Data
Pressure Rise Rate Versus Recipricol Temperature
0.01
0.10
1.00
10.00
100.00
1000.00
-2.6 -2.5 -2.4 -2.3 -2.2 -2.1 -2.0 -1.9
Recipricol Temperature
Pres
sure
Ris
e R
ate
(psi
/min
)
Maximum Pressure Rise Rate
180 psi/minute
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Now the proper data is known and available!
So lets examine the Auburnite design concept
Evaporative Concentration
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Evaporative Concentration
Process Flow Diagram - RA 2nd Stage Concentration
Steam60 psig
Z-100Three Stage Steam
Jet Vacuum System
Chilled Water5 C
T
70 wt% RAFrom 1st StageConcentration
Steam150 psig
Process OffgasTo Thermal Oxidizer
90 wt% RATo Crystalazer Chilled Water
5 C
Process CondensateTo Treatment
Note 1: Barometric LegNote 2: Equilization LineNote 3: 3 Barometric Legs
P
L
L
RO
F
T
R-100
P-100
A-100X-100
V-101
P-101
X-101
83 C
70 C
15 C
20 C
20mmHgA
2,500 PPH
1,944 PPH
Cond.
250 PPH
806 PPH
10mmHgA
16.7psia
16.7psia
1 32
575,200Btu/hr
308,800Btu/hr
21.7 C
15.2 C
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Evaporative Concentration
Jacket Jacketor or
Total Working Tubes Tubes
R-100 2nd Stage ConcentratorPressure Vessel
476 gallons
395 gallons 4'0" ID x 4'0" TT 30 psig & FV 100 psig & FV
316L Stainless
Steel
316L Stainless Steel
A-1002nd Stage Concentrator Agitator
Pitched Blade Turbine NA NA
2 - 18" Impellers 50 RPM x 5 HP NA NA
316L Stainless
SteelNA
X-1002nd Stage Concentrator Overhead
Shell & Tube Exchanger NA NA 630,000 Btu/hr 30 psig & FV 100 psig & FV
Carbon Steel Carbon Steel
P-1002nd Stage Concentrator Bottoms Pump
Centrufugal NA NA 10 GPM x 50' TDH 100 psig NA316
Stainless Steel
NA
Z-1002nd Stage Concentrator Vacuum System
Steam Jets & Direct Contact Condensers
NA NA 15 PPH @ 10 mmHgA 3 Stages 200 psig & FV NACarbon Steel NA
V-1012nd Stage Concentrator Distillate Receiver
Pressure Vessel
264 gallons
172 gallons 3'0" ID x 4'0" TT 15 psig & FV NA
Carbon Steel NA
X-1012nd Stage Concentrator Distillate Receiver
Shell & Tube Exchanger NA NA 340,000 Btu/hr 100 psig & FV 100 psig & FV
Carbon Steel Carbon Steel
P-1012nd Stage Concentrator Distillate Receiver
Centrifugal NA NA 60 GPM x 100' TDH 100 psig NADuctile
Iron NA
Characteristics Shell ShellVolume
Service TypeItem
N
umbe
r Design PressureEquipment List - 2nd Stage Concentration
Materials of Construction
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Evaporative Concentration
Steam60 psig
T
70 wt% RAFrom 1st StageConcentration
90 wt% RATo Crystalazer
L
RO
F
T
R-100
P-100
A-100
83 C
70 C
20mmHgA
2,500 PPH
1,944 PPH
Cond.
70 C556 PPH
Water Vaporto OverheadCondenser
Saturated Steam @ 60 psig
Temperature = 153 °C
Onset Temperature = 94 °C
This doesn’t look good!
Inventory ~ 395 gallons
Mass ~3,300 pounds
Wetted Area ~ 62 ft2
Normal Operating T = 70 °C
Onset Temperature = 94 °C
Close, but OK
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Evaporative Concentration
Steam60 psig
T
70 wt% RAFrom 1st StageConcentration
90 wt% RATo Crystalazer
L
RO
F
T
R-100
P-100
A-100
83 C
70 C
20mmHgA
2,500 PPH
1,944 PPH
Cond.
70 C556 PPH
Water Vaporto OverheadCondenser
Quick Calculation
Perry’s Handbook
For stainless steel, jacketed vessels with organics and condensing steam
OHT Coefficient = 50 -150 Btu/h/sf/F
U ∆T T condBtu/h/sf/F °C °C
80 62 132100 50 120120 42 112
( ) ( )
UAQTTUAQ
ftAhBtu
lbBtuhlbQ
=Δ⇒Δ=
=
==
22.62/000,559
/1005/556
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Evaporative Concentration
Inventory Concerns:Inventory is relatively large for such a potentially energetic material.
Reducing inventory doesn’t work…………. Why?
Wall Temperature Concerns:Inside wall temperature is probably higher than decomposition onset T
No choice at the required capacity with the current configuration
Single Failure Upset Cases of Concern:Loss of agitation
Failed open steam valveResults in Increasing wall temperature
Are there any others?
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Evaporative Concentration
Multiple Sequential Failure Upset Cases of Concern:Loss of cooling + stuck open steam valve
Loss of vacuum + stuck open steam valve
Failed closed pressure valve + stuck open steam valve
And others!
CONCLUSIONS:An uncontrolled exothermic decomposition appears plausible
The concentrator relief device should be sized for this case
Fortunately, the necessary data is available!
But should sizing be based on “all vapor” venting or two-phase flow?
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Why Does Two-Phase Venting Occur
Results of Water Blowdown Experiments:
Final Liquid Volume
For “All Vapor” Venting
485 Gallons
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Why Does Two-Phase Venting Occur
Valve Opens
Pressure Falls
If Rate of Bubble Generation is High Enough Liquid Swells to the Top of the Vessel
Liquid Swell Caused by Volume Generation
Not Liquid Entrainment
Highly Dependent on Physical Characteristics of Components
Volumetric Generation
LiquidSwell
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Rossonic Acid Decomposition
Volumetric Generation of Non-Condensable Gas
Evaporative Concentration
“The chemists also noted some foaming when this slow decomposition occurred.”
Remember this clue!
Concentrator Fill ~ 83 %
CONCLUSION: Design for Two-Phase Flow
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Larger Relief Devices Are NeededWhen Two-Phase Flow OccursVolume Balance Concept – Closed System
Gas Generating
Exothermic Reaction
T & P
Increase
Wouldn’t It Be NiceVOLUME
GENERATIONRATE
VOLUMEEXPANSION
RATE=
CONSTANT
PRESSURE
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Larger Relief Devices Are NeededWhen Two-Phase Flow OccursVolume Balance Concept – Open System
A More Realistic
System
VOLUMEGENERATION
RATE
VOLUMEDISCHARGE
RATE=
CONSTANT
PRESSURE
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Larger Relief Devices Are NeededWhen Two-Phase Flow OccursVolume Balance Concept – Open System
Definition of a Successful Emergency Relief Device:
Provides a balance between volume generation and volume dissipation
For the “Worst Credible” case conditions
At a pressure no greater than the maximum allowable pressure
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Larger Relief Devices Are NeededWhen Two-Phase Flow OccursVolume Balance Concept
Vg = Volume Generation Rate = Volume Discharge Rate = Vd
⎭⎬⎫
⎩⎨⎧
====ρρρGAGAWVV dg
Mass Flow Through Relief Device
Two-Phase Density
Two-Phase Mass Flux
Relief Device X-Sectional Area
2
3
3
2
ftsft
ftlbfts
lbG
==⎭⎬⎫
⎩⎨⎧ρVolumetric Flux =
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Larger Relief Devices Are NeededWhen Two-Phase Flow OccursVolume Balance Concept Saturated Hexane at 320 °F & 132.8 psia
Two Phase Density
0
10
20
30
40
0.0 0.2 0.4 0.6 0.8 1.0
Inlet Void Fraction
Two
Phas
e D
ensi
ty (l
b/cf
)
Increasing Vapor Content
Critical Mass Flux
500
600
700
800
900
0.0 0.2 0.4 0.6 0.8 1.0
Inlet Void Fraction
Crit
ical
Mas
s Fl
ux (l
b/sf
/s)
Increasing Vapor Content
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Larger Relief Devices Are NeededWhen Two-Phase Flow Occurs
0
50
100
150
200
250
300
350
400
450
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
Inlet Void Fraction
Volu
met
ric F
lux
(cf/s
/sf)
ALL LIQUID ALL VAPOR
⎭⎬⎫
⎩⎨⎧
====ρρρGAGAWVV dg
Volume Balance Concept Saturated Hexane at 320 °F & 132.8 psia
Increasing Vapor Content
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Simple Ideal Vent Sizing Results
Inside Diameter = 4’0” T-T Length = 4’0” Total Volume = 475 gallons
Fill Volumes = 428 gallons (90 %), 333 gallons (70 %), 238 gallons (50 %)
Design Pressure (DP) = 50, 75, 100, 150 psig
Maximum Pressure = (1.1) DP (10% accumulation)
Maximum Pressure Rise Rate = 180 psi per minute
Consider the following cases:
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Simple Ideal Vent Sizing Results
Concentrator475 Gallon Vessel
0
50
100
150
200
250
300
350
400
450
25 50 75 100 125 150 175
Design Pressure (Psig)
Vent
Are
a (S
q In
)
Fill Ratio = 90%
Fill Ratio = 70%
Fill Ratio = 50%
~ 12” Vent
~ 23” Vent
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
A large vent is required due to two-phase flow
Can two-phase flow be avoided?
Evaporative Concentration
Yes
By allowing enough room for vapor disengagement
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Vessel DisengagementBubbly Flow Regime
Co = 1.2
0.00
0.10
0.20
0.30
0.40
0.50
0.60
0.70
0.80
0.90
1.00
0.1 1.0 10.0 100.0
Dimensionless Superficial Vapor Velocity
Vess
el A
vera
ge V
oid
Frac
tion
Onset/Disengagement Boundary
Vessel Condition
Vapor Venting Region
Two Phase Venting Region
Inside Diameter = 4’0”
T-T Length = 4’0”
Total Volume = 475 gallons
DP = 50 psig & FV
Disengagement
Maximum Fill ~ 17 %
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Evaporative Concentration
With less inventory, how can the heat needed for the normal evaporation be added?
Decrease the concentrator inventory
Avoid two-phase flow
Size the relief device for “all vapor” venting
Basis for New Concentrator Design Concept
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
New Concentrator Design
Inside Diameter = 4’0”
T-T Length = 5’0”
Total Volume = 535 gallons
DP = 50 psig & FV
DT = 500°F 70 wt% RA
Emergency Water
Water Vapor
90 wt% RA
20 mmHg
70°C
LC On Upstream Vessel
5 psig Saturated
Steam
Tube Side
Condensation
Conditions
11.5 psia
93°C
Pumping
TrapSide View Top View
Baffles
Working Volume = 70 gallons
Maximum Volume = 100 gallons
Relief Device = 6” PSE based on vapor flow only
Minimization, Moderation, Limitation of Effects
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Is This Enough?
Shutdown Based On:
Redundant High Level
Redundant Process Temperature
Redundant Tube Side Steam Pressure
Quench water addition triggered by high process temperature only.
Shutdown
Feed & Steam
Safety Instrumented Systems (SIS) - Interlocks
Independent of the Basic Process Control System (BPCS)
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Concentrator – Top View
Emergency Vent Line
Normal Vent Line
Car Seal Open
Full Port Block Valve
Rupture Disk
(hidden)
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Concentrator – Bottom View
Process Outlet Pipe
Steam
Condensate Line
Stab-In
Tube Bundle
SIS Redundant
Temperature
Transmitters
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Concentrator – Bottom View
SIS Redundant Level Switches
Process Outlet Pipe
BPCS Level Transmitter
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
What Could Have Been Done Differently?
Conduct a high phi factor calorimeter test to better understand reaction mechanism.
Conduct calorimeter tests to determine if the reaction system tempers at the maximum allowable working pressure of the vessel.
Conduct a blowdown test to obtain a better feeling for disengagement dynamics.
Use more sophisticated tools to analyze the possibility of utilizing smaller vent sizes.
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Alternate Schemes to Consider
Falling Film EvaporatorA very good alternative
Usually have low heat transfer coefficients
Probably more expensive then vessel/tube bundle combination
Agitated Thin Film EvaporatorNot the best for low viscosity liquids
Considerably more expensive then vessel/tube bundle combination
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Connected Equipment
Jacket Jacketor or
Total Working Tubes Tubes
R-100 2nd Stage ConcentratorPressure Vessel
476 gallons
395 gallons 4'0" ID x 4'0" TT 30 psig & FV 100 psig & FV
316L Stainless
Steel
316L Stainless Steel
A-1002nd Stage Concentrator Agitator
Pitched Blade Turbine NA NA
2 - 18" Impellers 50 RPM x 5 HP NA NA
316L Stainless
SteelNA
X-1002nd Stage Concentrator Overhead
Shell & Tube Exchanger NA NA 630,000 Btu/hr 30 psig & FV 100 psig & FV
Carbon Steel Carbon Steel
P-1002nd Stage Concentrator Bottoms Pump
Centrufugal NA NA 10 GPM x 50' TDH 100 psig NA316
Stainless Steel
NA
Z-1002nd Stage Concentrator Vacuum System
Steam Jets & Direct Contact Condensers
NA NA 15 PPH @ 10 mmHgA 3 Stages 200 psig & FV NACarbon Steel NA
V-1012nd Stage Concentrator Distillate Receiver
Pressure Vessel
264 gallons
172 gallons 3'0" ID x 4'0" TT 15 psig & FV NA
Carbon Steel NA
X-1012nd Stage Concentrator Distillate Receiver
Shell & Tube Exchanger NA NA 340,000 Btu/hr 100 psig & FV 100 psig & FV
Carbon Steel Carbon Steel
P-1012nd Stage Concentrator Distillate Receiver
Centrifugal NA NA 60 GPM x 100' TDH 100 psig NADuctile
Iron NA
Characteristics Shell ShellVolume
Service TypeItem
N
umbe
r Design PressureEquipment List - 2nd Stage Concentration
Materials of Construction
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Summary
Critical information often comes from inconspicuous place.
Keep your eyes and ears wide open!!
Guessing is unacceptable
In God we trust, everyone else bring the right data!!
Avoid two-phase emergency venting where possible
Its always easier to ride your bicycle down-hill
Be weary of lab scale data when exothermic reactions are involved.
Scale-up is usually not included in a chemistry curriculum!!
A safety concept can not be realized without having the proper data
Don’t go skydiving without reading the parachute instructions
Chemistry knowledge is a key ingredient for process safety.
Don’t sell your Morrison & Boyd on eBay!!
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Summary
What can happen, will happen.
Remember Murphy’s Law.
Keep the “stuff” in the pipes
Once you start skidding, you are out of control.
Integrate the safety concept and the process design
Avoid problems by changing the basic process and/or equipment
Pressure relief should be the last line of defense
But not the only line of defense.
Use the right equipment.
Don’t try to fix your car without the right tools.
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Closing Remarks
Contact Information – Call or Write Anytime !!
Email: [email protected] (best method)
Phone: 251-443-2420 (I travel allot, so be patient)
Address:
Robert D’Alessandro
Degussa Corporation
4301 Degussa Road
Theodore, AL 36590-0606
I will be glad to help in anyway I can !!
mailto:[email protected]
Auburn University Chen 4450 Process Safety Robert D‘Alessandro, P.E.
Closing Remarks
Thank you !!
Auburn University
Professor Chambers, Professor Eden, and Professor Roberts
Degussa Corporation
Professor Riemenschneider, Dr. Kemnade
Students in Chen 4450
Evaporative Concentration of a Thermally Sensitive Chemical IntroductionLecture ObjectivesEvaporative ConcentrationSigns of Inherent TroubleSigns of Inherent TroubleSigns of Inherent TroubleLaboratory Scale Data Laboratory Scale Data Laboratory Scale Data Adiabatic CalorimetersAdiabatic CalorimetersAdiabatic CalorimetersAdiabatic CalorimetersEvaporative ConcentrationTempered Versus Gassy SystemsTempered Versus Gassy SystemsExperimental SpecificationAdiabatic Calorimeter DataAdiabatic Calorimeter DataAdiabatic Calorimeter DataAdiabatic Calorimeter DataEvaporative ConcentrationEvaporative ConcentrationEvaporative ConcentrationEvaporative ConcentrationEvaporative ConcentrationEvaporative ConcentrationEvaporative ConcentrationWhy Does Two-Phase Venting OccurWhy Does Two-Phase Venting OccurEvaporative ConcentrationLarger Relief Devices Are Needed�When Two-Phase Flow OccursLarger Relief Devices Are Needed�When Two-Phase Flow OccursLarger Relief Devices Are Needed�When Two-Phase Flow OccursLarger Relief Devices Are Needed�When Two-Phase Flow OccursLarger Relief Devices Are Needed�When Two-Phase Flow OccursLarger Relief Devices Are Needed�When Two-Phase Flow OccursSimple Ideal Vent Sizing ResultsSimple Ideal Vent Sizing ResultsEvaporative ConcentrationVessel DisengagementEvaporative ConcentrationNew Concentrator DesignIs This Enough? Concentrator – Top ViewConcentrator – Bottom ViewConcentrator – Bottom ViewWhat Could Have �Been Done Differently? Alternate Schemes to Consider Connected EquipmentSummarySummaryClosing RemarksClosing Remarks