CATALYTIC OXIDATION TECHNOLOGY TRANSFER PROGRAMJohnson Matthey CatalyK6 Sample 400 Cells/in2. CATOX...
Transcript of CATALYTIC OXIDATION TECHNOLOGY TRANSFER PROGRAMJohnson Matthey CatalyK6 Sample 400 Cells/in2. CATOX...
CATOX CBR Filtration Team Technology Transfer Program (TTP)
Dr. Alex Balboa
Mr. Michael Parham
Research and Technology Directorate
Edgewood Chemical Biological Center
US Army, Research Development and Engineering Command
CATALYTIC OXIDATION TECHNOLOGY TRANSFER
PROGRAM
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1. REPORT DATE 16 NOV 2004
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4. TITLE AND SUBTITLE Catalytic Oxidation Technology Transfer Program
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Standard Form 298 (Rev. 8-98) Prescribed by ANSI Std Z39-18
CATOX CBR Filtration Team Technology Transfer Program (TTP)
• Design, construct and evaluate a catalytic air purification system for collective protection applications
– Demonstrate Broader Protection of Catalytic versus Single Pass Filtration Technology
– Optimize Power, Weight and Size of Catalytic Process
Overall Objective
CATOX CBR Filtration Team Technology Transfer Program (TTP)
-Incorporate commercial/newly developed catalysts for chemical, biological and TICs destruction (leverage w/
Advanced Adsorbents Program)
-Establish design relationships for predicting system size and energy requirements for potential applications
CATOX Reactor
Post-Treatment Abatement
CO2
Air
CWA
TIC
Heat ExchangerH2O
Approach
CATOX CBR Filtration Team Technology Transfer Program (TTP)
DARPA Investment ECBC/INDUSTRY
COLLABORATIONTECHNOLOGY READINESS LEVELS
LAB-SCALE TESTING
(COMPONENT)
SYSTEM-SCALE TESTING
- evaluation of commercial catalysts
- identification and evaluation of acid gas abatement strategies
- evaluation and optimization of catalyst system components- integration of system components
- determine size and energy requirements of scalable AP system
Program Leverage
CATOX CBR Filtration Team Technology Transfer Program (TTP)
– Objectives
• Technology maturity level/Technology readiness level
• Applicability/relevance to DoD CB Defense Acquisition Program
• Potential to mature for evaluation in field environment
• Availability of other funding to leverage Technology Transition investment
• Availability to government of data bases, methodology details, and design concepts
DARPA Investment
CATOX CBR Filtration Team Technology Transfer Program (TTP)
Chemical delivery sensitivities
• Single pass filters have their capacity defined in terms of CT (conc x time).
• This is a misleading indicator for CATOX.• CATOX challenges must be as close to the application’s
threat to account for performance sensitivities to:– # of attacks– Dosage per attack– Peak concentration– Frequency of attacks
• CATOX systems can succeed or fail for a given CT if any of these variables are changed.
CATOX CBR Filtration Team Technology Transfer Program (TTP)
Current filter technology • limited capacity for agents that are removed by chemical reaction and/or weakly
adsorbed• minimal protection versus several of the toxic industrial chemicals (TICs)• prolonged environmental exposure has been shown to reduce the capacity of these
filters for agents that are removed by chemical reaction
Catalytic oxidationAn alternative air purification technology
(1) broad and universal protection against the chem-bio threat, (2) reduced logistics due to long operational life,(3) greatly increased capacity for CB agents and TICs compared to current NBC
collective protection technologies and (4) lower energy costs relative to other regenerative filtration technologies. (5) Catalytic oxidation is a destructive technology, converting CB agents and TICs to
CO2 (catalysts exist that are capable of decomposing nitrogen-containing compounds with minimum NOx formation), H2O and haloacids (should halogens be associated with the parent compound).
Benefits
CATOX CBR Filtration Team Technology Transfer Program (TTP)
Issues Toxic By-productsCatalyst StabilityEnergyPost treatment
State of the ArtHigh activity Stable catalystsNOx, acid retentionImproved acid abatement technologies
• Mitigation of reaction product emissions• Maximize heat recovery to minimize energy
utilization
Challenges
CATOX CBR Filtration Team Technology Transfer Program (TTP)
Material Development
Downselect (light-off curves and selectivity)
-Incorporate commercial/newly developed catalysts for chemical, biological and TICs destruction
CATOX CBR Filtration Team Technology Transfer Program (TTP)
Monolithic Bed Catalyst Suppliers
Manufacturer Catalyst Designation Cell Density
Engelhard Corporation Engelhard Catalyst 200 Cells/in2
United Emissions Catalyst NB001-73-01 200 Cells/in2
United Emissions Catalyst NB001-73-02 200 Cells/in2
Sud Chemie Prototech LS02-03145 400 Cells/in2
Sud Chemie Prototech Misc-03144 400 Cells/in2
Guild Associates No-NOx 400 Cells/in2
Guild Associates 3X 400 Cells/in2
Johnson Matthey CatalyK6 Sample 400 Cells/in2
CATOX CBR Filtration Team Technology Transfer Program (TTP)
Catalyst oxidation of CO
by catalytic materials under
low and high humidity conditions(materials
improvement)
Lab-scale results
• good indicator of catalyst
activity (very clean parent and
byproduct)• poor effective
filtration by current NBC
systems
0 %
2 0 %
4 0 %
6 0 %
8 0 %
1 0 0 %
0 5 0 1 0 0 1 5 0 2 0 0 2 5 0 3 0 0
T e m pe rature , oC
Con
vers
ion,
%
U EC -0 1 C a ta ly s tEng e lha rd C a ta ly s tN o -N O x C a ta ly s tS C P-0 1 C a ta ly s tJ M C a ta lK 6 S a mpleU EC -0 2 C a ta ly s t3 X Ca ta ly s tS PS M IS C -0 3 1 4 4 N o -N O x plus 3 X
M on ol i thG H S V = 9,00 0[C O ] = 2,0 00 m g/m 3
(16 50 ppm ))[H 2O ] = 4.1 % vo l u m e
0 %
2 0 %
4 0 %
6 0 %
8 0 %
1 0 0 %
0 5 0 1 0 0 1 5 0 2 0 0 2 5 0 3 0 0
T e m pe rature , oC
Con
vers
ion,
%
U EC -01 C ata lys tEnge lhard C ata lys tSC P-03145 C ata lys tN O -N O x C ata lys tJM C ata lK 6 SampleU EC -02 C ata lys t3X Cata lystSC P M ISC -03144 C ata lys tN o-N O x plus 3X
M o no l i thG HS V = 9 ,0 00[C O ] = 2 ,00 0 m g /m 3
(1 65 0 ppm ))[H 2O ] = 0 .34 % vo l u m e
CATOX CBR Filtration Team Technology Transfer Program (TTP)
Schematic representationof catalytic reactor
Thermocouples
Gas Inlet
Inlet Flange
Packing
Frit
Catalyst
Gas Outlet
Gas Inlet
Inlet Flange
Packing
Frit
Catalyst
Gas Outlet
CATOX CBR Filtration Team Technology Transfer Program (TTP)
0%
20%
40%
60%
80%
100%
150 200 250 300 350 400
Temperature, oC
Con
vers
ion,
%
UEC-01 CatalystNO-NOx CatalystEngelhard CatalystSCP LS02-03145JM CatalK6 SampleUEC-02 Catalyst3X CatalystSCP MISC-03144No-NOx plus 3X
MonolithGHSV = 9,000[NH3] = 2,000 mg/m3
(2,650 ppm)[H2O] = 0.34% volume
Dry NH3 tests
CATOX CBR Filtration Team Technology Transfer Program (TTP)
Humid NH3 tests
0%
20%
40%
60%
80%
100%
150 200 250 300 350 400
Temperature, oC
Con
vers
ion,
%
UEC-01 CatalystNO-NOx CatalyatEngelhard CatalystSCP LS02-03145JM CatalK6 SampleUEC-02 Catalyst3X CatalystSCP MISC-03144No-NOx Plus 3X, Layered
GHSV = 9,000[NH3] = 2,000 mg/m3
(2,650 ppm)[H2O] = 4.1% volume
CATOX CBR Filtration Team Technology Transfer Program (TTP)
1
10
100
1000
200 220 240 260 280 300 320 340 360 380 400
Temperature, oC
[NO
x], p
pm
UEC-01 CatalystNo-NOx CatalystSCP LS02-03145Engelhard CatalystJM CatalK6 SampleUEC-02 Catalyst3X CatalystSCP MISC-03144No-NOx plus 3X
5 ppm NO2 Effluent NIOSH Requirement
GHSV = 9,000[NH3] = 2,000 mg/m3
(2,650 ppm)[H2O] = 0.34% volume
25 ppm NO Effluent NIOSH Requirement
30 ppm NO2 Effluent CHPPM MEG Guidelines
9 ppm NO Effluent CHPPM MEG Guidelines
Selectivity (NOx): NH3 tests (dry)
CATOX CBR Filtration Team Technology Transfer Program (TTP)
1
10
100
1000
200 220 240 260 280 300 320 340 360 380 400
Temperature, oC
[NO
x], p
pm
UEC CatalystNo-NOx CatalystSCP LS02-03145Engelhard CatalystJM CatalK6 SampleUEC-02 Catalyst3X CatalystSCP MISC-03144No-NOx Plus 3X, Layered
5 ppm NO2 Effluent NIOSH Requirement
GHSV = 9,000[NH3] = 2,000 mg/m3
(2,650 ppm)[H2O] = 4.1% volume
25 ppm NO Effluent NIOSH Requirement
30 ppm NO2 Effluent CHPPM MEG Guidelines
9 ppm NO Effluent CHPPM MEG Guidelines
Selectivity (NOx): NH3 tests (humid)
CATOX CBR Filtration Team Technology Transfer Program (TTP)
0
200
400
600
800
1000
200 220 240 260 280 300 320 340 360 380 400
Temperature, oC
[NO
x], p
pm
UEC-1 CatalystNo-NOx CatalystSCP :S02-03145Engelhard CatalystJM CatalK6 SampleUEC-2 Catalyst3X CatalystSCP MISC-03144No-NOx plus 3X
GHSV = 9,000[NH3] = 2,000 mg/m3
(2,650 ppm)[H2O] = 0.34% volume
Selectivity (N2O): NH3 tests (dry)
CATOX CBR Filtration Team Technology Transfer Program (TTP)
Selectivity (N2O): NH3 tests (humid)
0
200
400
600
800
1000
200 220 240 260 280 300 320 340 360 380 400
Temperature, oC
[NO
x], p
pm
UEC CatalystNo-NOx CatalystSCP LS02-03145Engelhard CatalystJM CatalK6 SampleUEC-02 Catalyst3X CatalystSCP MISC-03144NO-NOx plus 3X, Layered
GHSV = 9,000[NH3] = 2,000 mg/m3
(2,650 ppm)[H2O] = 4.1% volume
CATOX CBR Filtration Team Technology Transfer Program (TTP)
Dry C3F6 tests
0%
20%
40%
60%
80%
100%
100 150 200 250 300 350 400 450 500
Temperature, oC
Conv
ersio
n, %
UEC-01 CatalystEngelhard Catalyst3X CatalystUEC-02 CatalystSCP-01 CatalystSCP-02 CatalystJM CatalK6 Sample3X Plus No-NOx CatalystGuild NO-NOx
GHSV = 9,000
[C3F6] = 2,000 mg/m3
(300 ppm)[H2O] = 0.34%
CATOX CBR Filtration Team Technology Transfer Program (TTP)
Humid C3F6 tests
0%
20%
40%
60%
80%
100%
100 150 200 250 300 350 400 450 500
Temperature, oC
Conv
ersio
n, %
UEC-01 CatalystEngelhard Catalyst3X CatalystUEC-02 CatalystSCP-01 CatalystSCP-02 CatalystJM CatalK6 Sample3X Plus No-NOx CatalystGuild No-NOx
GHSV = 9,000
[C3F6] = 2,000 mg/m3
(300 ppm)[H2O] = 4.1%
Table showing T95?
CATOX CBR Filtration Team Technology Transfer Program (TTP)
Catalyst PerformanceCatalyst performance summary information
Catalyst Design Lim. Temperature2 Ammonia Ammonia Chemical1 [NOx]3 [N2O]3
Guild No-NOx C3F6 T > 500°C > 500 ppm > 300 ppm
Guild No-NOx Plus 3X C3F6 350°C 15 ppm 160 ppm
Guild 3X C3F6 310°C 400 ppm 550 ppm
Engelhard #164217005 C3F6 440°C > 1,000 ppm ~ 300 ppm
UEC NB001-73-001 C3F6 T > 500°C > 1,000 ppm ~ 300 ppm
UEC NB001-73-002 C3F6 T > 500°C > 1,000 ppm ~ 300 ppm
SCP LS02-03145 C3F6 450°C > 1,000 ppm ~ 300 ppm
SCP MISC-03144 C3F6 450°C > 1,000 ppm ~ 300 ppm
JM CatalyK6 Sample C3F6 T > 500°C > 1,000 ppm ~ 300 ppm 1Chemical requiring greatest temperature to achieve 99% destruction 2Temperature required to achieve 99% destruction of design limiting chemical 3NOx or N2O concentration formed during destruction of NH3 at temperature
CATOX CBR Filtration Team Technology Transfer Program (TTP)
Catalyst Bed
Heater/Precooler
ContaminatedAir In
CleanAir Out
PostTreatmentFilter
AmbientAir Out
Fan
Fan
Targeted for:FCS ApplicationScalable for building protectionTransportable shelters (JECP)
NBC Subsystem Summary
CATOX CBR Filtration Team Technology Transfer Program (TTP)
Ammonia (HC): Feed TemperatureECBC 50 SCFM CATOX UNIT
Feed Conditions
0
10
20
30
40
50
60
70
80
90
100
0 500 1000 1500 2000 2500 3000 3500 4000 4500 5000
Time (min)
Tem
pera
ture
(C)
TC 10 - Water NozzleTC 11 - Chemical NozzleDew Point @ 4.2 psig
CATOX CBR Filtration Team Technology Transfer Program (TTP)
ATD Experimental Design
• 6 x 2000 mg/m3 x 10 minutes (CT = 120,000 mg-min/m3)
• 6 x 200 mg/m3 x 100 minutes (CT = 120,000 mg-min/m3)
______________________________
CT = 240,000 mg-min/m3
(under 2.5% water (volume) and 50 cfm)
CATOX CBR Filtration Team Technology Transfer Program (TTP)
ECBC 50 SCFM CATOX UNITNH3-HW-BHc Ammonia Feed Chart 5-6-04
6 x 10 minute pulse
0
500
1000
1500
2000
2500
0 50 100 150 200 250 300 350 400 450
Time (min)
Am
mon
ia (m
g/m
3)
A1 - Feed (Pre-Heater)
A3 - Feed (Post Heater)
Ammonia (HC): Feed Concentrations
CATOX CBR Filtration Team Technology Transfer Program (TTP)
Ammonia (HC): TemperatureECBC 50 SCFM CATOX UNIT
Temperature Plot
0
50
100
150
200
250
300
350
0 50 100 150 200 250 300 350 400 450 500
Time (min)
Tem
pera
ture
(C)
TC 1 - Feed
TC 2 - HeatEx HotOut
TC 3 - Heater Out
TC 4 - MAP Inlet
TC 5 - MAP Outlet
TC 6 - PTF Outlet
TC 7 - HeatEx HotIn
TC 8 - HeatEx ColdOut
TC 9 - Guard PTFInlet
CATOX CBR Filtration Team Technology Transfer Program (TTP)
ECBC 50 SCFM CATOX UNITAnalog Signal Chart
0
5
10
15
20
25
30
35
235 245 255 265 275 285 295 305 315 325
Time (min)
Am
mon
ia (m
g/m
3)
A4 - Post MAP A5 - Post PTF
Ammonia (HC); Parent compound
CATOX CBR Filtration Team Technology Transfer Program (TTP)
Ammonia (HC): By-productsECBC 50 SCFM CATOX UNIT
Analog Signal Chart
0
50
100
150
200
250
300
350
400
450
500
235 245 255 265 275 285 295 305 315 325
Time (min)
NO
x co
ncen
trat
ion
(ppm
)
NOX 2 Post MAP
NOX 3 Post PTF
CATOX CBR Filtration Team Technology Transfer Program (TTP)
ECBC 50 SCFM CATOX UNITFeed Conditions
0
10
20
30
40
50
60
70
80
90
100
0 100 200 300 400 500 600
Time (min)
Tem
pera
ture
(C)
TC 10 - Water NozzleTC 11 - Chemical NozzleDew Point @ 4.2 psig
Ammonia (LC): Feed Temperature
CATOX CBR Filtration Team Technology Transfer Program (TTP)
ECBC 50 SCFM CATOX UNITNH3-HW-BLc P3-5Feed Chart 5-10-04
0
20
40
60
80
100
120
140
160
180
200
0 100 200 300 400 500 600
Time (min)
Am
mon
ia (m
g/m
3)
A1 - Feed
A3 - Feed
Ammonia (LC): Feed Concentrations
CATOX CBR Filtration Team Technology Transfer Program (TTP)
ECBC 50 SCFM CATOX UNITTemperature Plot
0
50
100
150
200
250
300
350
0 100 200 300 400 500 600
Time (min)
Tem
pera
ture
(C)
TC 1 - Feed
TC 2 - HeatEx HotOut
TC 3 - Heater Out
TC 4 - MAP Inlet
TC 5 - MAP Outlet
TC 6 - PTF Outlet
TC 7 - HeatEx HotIn
TC 8 - HeatEx ColdOut
TC 9 - Guard PTFInlet
Ammonia (LC): Temperature
CATOX CBR Filtration Team Technology Transfer Program (TTP)
ECBC 50 SCFM CATOX UNITNH3-HW-BLc P3-5
Effluent Chart (NH3) 5-10-04
0
5
10
15
20
25
30
35
40
45
50
0 100 200 300 400 500 600
Time (min)
Am
mon
ia (m
g/m
3)
A4 - Post MAP
A5 - Post PTF
Ammonia calibration +/- 50% below 12 mg/m3
Ammonia (LC): Parent
CATOX CBR Filtration Team Technology Transfer Program (TTP)
ECBC 50 SCFM CATOX UNITTemperature Plot
EO-HW-BHc 6-18-04
0
50
100
150
200
250
300
0 10 20 30 40 50 60 70 80
Time (min)
Tem
pera
ture
(C)
TC 1 - Feed
TC 2 - HeatEx HotOut
TC 3 - Heater Out
TC 4 - MAP Inlet
TC 5 - MAP Outlet
TC 6 - PTF Outlet
TC 7 - HeatEx HotIn
TC 8 - HeatEx ColdOut
TC 9 - Guard PTFInlet
Ethylene Oxide (HC): Temperature
CATOX CBR Filtration Team Technology Transfer Program (TTP)
Ethylene Oxide (HC): Feed ConcentrationsECBC 50 SCFM CATOX UNIT
EO-HW-BHc 6-18-04EO Feed - CO2 Effluent
0
200
400
600
800
1000
1200
1400
1600
1800
2000
0 10 20 30 40 50 60 70 80
Time (min)
Con
cent
ratio
n (p
pm)
A1 - EO Feed
A4- CO2 Effluent
CATOX CBR Filtration Team Technology Transfer Program (TTP)
Ethylene Oxide (HC): By-productsECBC 50 SCFM CATOX UNIT
EO-HW-BHc 6-18-04EO - CO Effluent
0
1
2
3
4
5
6
7
8
9
0 10 20 30 40 50 60 70 80
Time (min)
Con
cent
ratio
n (p
pm)
A4 - CO Effluent
A4 - EO Effluent (FID)
CATOX CBR Filtration Team Technology Transfer Program (TTP)
ECBC 50 SCFM CATOX UNITTemperature Plot
0
50
100
150
200
250
300
0 20 40 60 80 100 120 140
Time (min)
Tem
pera
ture
(C)
TC 1 - Feed
TC 2 - HeatEx HotOut
TC 3 - Heater Out
TC 4 - MAP Inlet
TC 5 - MAP Outlet
TC 6 - PTF Outlet
TC 7 - HeatEx HotIn
TC 8 - HeatEx ColdOut
TC 9 - Guard PTFInlet
Formalin (LC)
CATOX CBR Filtration Team Technology Transfer Program (TTP)
ECBC 50 SCFM CATOX UNITHCHO-HW-DLc 7-14-04
A1 - HCHO A4 - CO2
0
100
200
300
400
500
600
700
800
900
0 20 40 60 80 100 120 140
Time (min)
Con
cent
ratio
n (p
pm)
A4 - CO2 (ppm)
A1 - HCHO (ppm)
Formalin (LC)
CATOX CBR Filtration Team Technology Transfer Program (TTP)
ECBC 50 SCFM CATOX UNITHCHO-HW-DLc 7-14-04
A3 - CO2 A4 - CO A4 - HCHO A5 - HCHO
0
10
20
30
40
50
60
70
80
90
100
0 20 40 60 80 100 120 140
Time (min)
Con
cent
ratio
n (p
pm)
A4 - CO (ppm) A4 - HCHO (ppm)
A5 - HCHO (ppm) A3 - CO2 (ppm)
Formalin (LC)
CATOX CBR Filtration Team Technology Transfer Program (TTP)
Chemicals tested:Carbon Monoxide
AmmoniaEthylene Oxide
FormalinChemical underway:
AcetonitrileChemicals left:
ChloroformCKCS2
Nitric AcidCEES
HFHFP
DMMP
CATOX CBR Filtration Team Technology Transfer Program (TTP)
Power and weight optimization
In a fielded system, one catalyst bed operating at one flow rate and one operating temperature will be employed.
Field conditions impacting CATOX
C a t O x D e m o n s tra t o r I m p a c t o f A ir f lo w o n A v e r a g e P o w e r D e m a n d
[ 8 0 % H X e f f , 5 0 S C F M a i r f l o w , 2 5 0 C C a t a l y s t T e m p e r a t u r e , 8 1 0 0 W M a x P o w e r D e m a n d , 8 0 k g Th e r m a l M a s s ]
0
5 0 0
1 0 0 0
1 5 0 0
2 0 0 0
2 5 0 0
3 0 0 0
3 5 0 0
4 0 0 0
4 5 0 0
5 0 0 0
5 5 0 0
6 0 0 0
0 2 5 5 0 7 5 1 0 0 1 2 5 1 5 0 1 7 5 2 0 0 2 2 5 2 5 0
A ir f l o w (S C F M )
Ave
rage
Pow
er D
eman
d (W
)
C a t O x D e m o n s t r a t o rM C P E ( M 4 8 )C a t a ly s t T e m p e r a t u r e R e d u c t io n o f 2 5 C a n d 5 % I n c r e a s e in H e a t E xc h a n g e r E f f ic ie n c y
Sy s t e mO p t i m i z a t i o n
CATOX CBR Filtration Team Technology Transfer Program (TTP)
Improvement of SubcomponentsNext Generation PTS
Catalyst Improvements
Heat Exchanger (greater 90% heat recovery efficiency
Modular System
Lighter, Smaller Overall Footprint
CATOX CBR Filtration Team Technology Transfer Program (TTP)
AcknowledgementsJoseph Rossin, Ph.D., Guild Associates
Russell W. Johnson, Ph.D., Honeywell, Inc.
Peter M. Michalakos, Ph.D., Honeywell, Inc.
Brian Elmiger, Honeywell, Inc.