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CO2 Capture by Cold Membrane Operation with Actual Power Plant Flue Gas (FE0013163)
August 22, 2017A. Augustine, T. Chaubey, R. Gagliano, S. Kulkarni, S. Fu,
D. Hasse, T. Li, D. Kratzer, M. Bennett, M. | R&DJ.-M. Gauthier, R. Hutchinson, W. Wheeler, R. Warwick | MEDAL
2017 NETL CO2 Capture Technology Project Review Meeting:
Bench Scale Testing of Next Generation Hollow Fiber Membrane Modules (FE0026422)
Air Liquide, world leader in gases for industry, health and the environmentResearch & Development2
Air Liquide & MEDAL
Air Liquide: world leader in industrial and medical gases
68,000 employees
$19 billion sales (2016)
NG Sweetening EOR NG Trimming Fuel Gas
H2 applications / markets
CO2 applications / markets
N2 applications / markets
Biogas
OBIGGSMaritime
Food & BevUB Oil Drilling
CB Inerting
Chemical Synthesis
Air Liquide Advanced Separations, MEDAL
CO2 Capture /CO2 Sourcing
Refinery Off-gas Streams
Air Liquide, world leader in gases for industry, health and the environmentResearch & Development3
Background: Cold Membrane Process
Energy integration / savings:• Residue expansion, direct coupling with compression• Pumping of liquid CO2
• Boiler feed water (BFW) sufficient for entire power plant steam cycle
Drawbacks:• High membrane capital cost• Energy intensive
Air Liquide, world leader in gases for industry, health and the environmentResearch & Development4
Commercial PI-1, RTCommercial PI-1 @ - 45°CPI-2 Fiber, RTPI-2 Fiber @ -45°C
Background: Novel PI-2 Membrane Material
PI-1 standard product• 1,000’s of modules per year, dozens of applications• Performance improves at low temperature
PI-2 novel material• Permeation properties near Robeson* upper bound• Spinnable• Performance at NCCCover 500+ hours
*Robeson, J. Membr. Sci. 2008(320), 390-
Air Liquide, world leader in gases for industry, health and the environmentResearch & Development5
Commercial PI-1, RTCommercial PI-1 @ - 45°CPI-2 Fiber, RTPI-2 Fiber @ -45°C
Background: Novel PI-2 Membrane Material
PI-1 standard product• 1,000’s of modules per year, dozens of applications• Performance improves at low temperature
PI-2 novel material• Permeation properties near Robeson* upper bound• Spinnable• Performance at NCCCover 500+ hours
*Robeson, J. Membr. Sci. 2008(320), 390-
12” OD x 34” LFeed: 3,300 Nm3/h
(0.6 MWe eq.)18% CO2, 200 psig, -45°C
Residue: <1.8% CO2(~190 psig)
Permeate: >58% CO2(~1 psig)
(1 module, projected performance)
Air Liquide, world leader in gases for industry, health and the environmentResearch & Development6
NETL Project Manager: José FigueroaProject Team:
Air Liquide R&D – Sudhir Kulkarni, Trapti Chaubey, David Hasse, Ted Li, Madhava Kosuri, Shilu Fu, Jiefu Ma, Monaca McNall, Jacob Brumback, Dean Kratzer, Michael Bennett, Judy Huss, Dennis Calvetti, Robert Sokola, Gerard Gagliano, Jean-Pierre Tranier, Robert Gagliano, David Edwards, Deborah Hutchinson, Yang Jiang, Ian Moskowitz
MEDAL/ALAS - Karl Beers, Jean-Marie Gauthier, Alfredo Velasco, Dana Husnay, Ed Sanders
E&C – Mike Turney, Paul Terrien
Parsons - Brad Knutson, Surajit Amrit, Jay Hellinger, Tom Moe, Louis Wheat
Test partner – National Carbon Capture Center
DE-FE0013163 DOE AL
Cost Share $5.12MM $1.28MMTotal Budget $6.4MM
Project Organization: DOE/NETL Awards
DE-FE0026422 DOE AL
Cost Share $3.00MM $0.97MMTotal Budget $3.97MM
Oct-2013
Apr-2017
Oct-2015
Dec-2018
• Improve commercial bundle performance• Early development PI-2• Field-test at NCCC
• Develop PI-2 to 4” OD, bench scale and test• Develop to commercial scale• Field-test at NCCC
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Membrane
Skid 1Skid 3
Skid 2
Agenda
Technology & Project Overview
NCCC Testing (FE0013163)Membrane testingAnalytical campaign
PI-2 Scale-up (FE0026422)Manufacturing development
and testingAcid gas contaminants
Next StepsPI-2 scale-up to 6” sizeBack to NCCC
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Process Flow Diagram - NCCC
Liquid Ring Blower
Oil Flooded Compressor
Power Plant
LP treatment HP treatment
Feed Gas -49°F, 200 psig
1” PI-2 Bundle
2x12” PI-1 Bundles (series or parallel)
Permeate: 60+% CO2
Retentate: 2% CO2
Flue Gas
Retentate
Permeate
HeatExchanger
Air Liquide, world leader in gases for industry, health and the environmentResearch & Development9 Not used at full scale
Process Flow Diagram - NCCC
Liquid Ring Blower
Oil Flooded Compressor
Power Plant
LP treatment HP treatment
Feed Gas -49°F, 200 psig
1” PI-2 Bundle
2x12” PI-1 Bundles (series or parallel)
Permeate: 60+% CO2
Retentate: 2% CO2
Flue Gas
Retentate
Permeate
HeatExchanger
Air Liquide, world leader in gases for industry, health and the environmentResearch & Development10
DRTC TEAM AT NCCC: Oct-2015
Air Liquide, world leader in gases for industry, health and the environmentResearch & Development11
10
20
30
40
50
60
0
2
4
6
8
10
50% 60% 70% 80% 90% 100%
CO2/
N2
Sele
ctiv
ity
Nor
mal
ized
CO2
Perm
eanc
e
% CO2 Capture
CO2 Permeance
CO2 Permeance (with Sweep)
Selectivity
Selectivity (with Sweep)
1” PI-2 Bundle Parametric Testing at NCCC
1” PI-2 bundle has non-ideal flow, no impact of sweep
Ideal Selectivity
Ideal Permeance
Air Liquide, world leader in gases for industry, health and the environmentResearch & Development12
10
20
30
40
50
60
0
2
4
6
8
10
50% 60% 70% 80% 90% 100%
CO2/
N2
Sele
ctiv
ity
Nor
mal
ized
CO2
Perm
eanc
e
% CO2 Capture
CO2 Permeance
CO2 Permeance (with Sweep)
Selectivity
Selectivity (with Sweep)
1” PI-2 Bundle Parametric Testing at NCCC
1” PI-2 bundle has non-ideal flow, no impact of sweep
Ideal Selectivity
Ideal Permeance
TEA PI-2 Case 2Performance
TEA PI-2 Case 1Performance
Air Liquide, world leader in gases for industry, health and the environmentResearch & Development13
0
1
2
3
4
5
6
7
1" PI-1 12" PI-1 6" PI-1 1" PI-2
Nor
mal
ized
CO2
Perm
eanc
e
0
10
20
30
40
50
60
70
80
90
100
1" PI-1 12" PI-1 6" PI-1 1" PI-2
CO2/
N2
Sele
ctiv
ity
12” PI-1 vs PI-2 Bundle Performance
610 Nm3/h
240 Nm3/h
2,500 Nm3/hto
3,300 Nm3/h
Extra
pola
ted
to 1
2”
Purity = 64% 71%69% 61%
Higher productivity →Lower CAPEX
Higher purity →Lower OPEX
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Analytical Campaign to Track Impurities
*Results of Arsenic are all below detection limit
Low pressurecondensate
Inlet Dryerbeds
CompFeed
Blower
Activated Al
CompOutletFlue
GasCold
membrane
Gas sampling pointLiquid sampling point
Compressor
High pressurecondensate
MembraneFeed
Powerplant
CO2
N2
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Analytical Campaign to Track Impurities
CO2
Low pressurecondensate
Dryerbeds
Activated Al
Flue Gas
Cold membrane
Gas sampling pointLiquid sampling point
N2
High pressurecondensate
Powerplant
0
50
100
150
200
250
300
350
400
5:55 6:05 6:24 6:34 6:44
Conc
entr
atio
n (p
pm)
Time (PM)
NO2 (ppm)
NO (ppm)
Start dryer bed regeneration
Impurities are mitigated in pre-treatment, undetectable after the activated alumina bed.
Blower Compressor
InletCompFeed
CompOutlet
MembraneFeed
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Techno-Economic Analysis
Cold Membrane (PI-1) Projected PI-2
Case 12 (Amine) Cold Membrane (PI-1) PI-2Power Plant Cost (MM$) 1,366 1,305 1,326CO2 Capture System (MM$) 593 357 254Total Plant Cost (MM$) 1,959 1,662 1,580CO2 Capture Cost ($/tonne) 55 40 – 45* 38 – 42*
PI-2: big cost reduction on membranes
* Cost range is based on sensitivity analysis
Air Liquide, world leader in gases for industry, health and the environmentResearch & Development17
Membrane
Skid 1Skid 3
Skid 2
Agenda
Technology & Project Overview
NCCC Testing (FE0013163)Membrane testingAnalytical campaign
PI-2 Scale-up (FE0026422)Manufacturing development
and testingAcid gas contaminants
Next StepsPI-2 scale-up to 6” sizeBack to NCCC
Air Liquide, world leader in gases for industry, health and the environmentResearch & Development18
OD (in) Length(ft)
Fiber Count Spinning Device
Fabrication Technique
Mini permeator 0.25 - 0.5”1.6’
<1000 1-hole lab unit
Hand
Permeator 1” 1 – 5xSkein
12-hole“DSU”
Skein module 2.5”
2.8’
15 – 20xR&D prototypebundle 2.5 - 4” 15 – 20x
Forming6” bundle (commercial) 6” 50 – 90x 24/36-hole
production unit12” bundle
(commercial) 12” >200x
Manufacturing Development
Spinning Equipment (DSU)
Spinning
Forming EquipmentFiber Processing / HandlingWashing Drying Bobbin
winding Tube-sheet forming MachiningPost-spin handling
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PI-2 fiber synthesized on the DSU
Periodic samples for quality control:
• Fiber performance was consistent and agreed with previous lab-scale results
• Fiber “formed” into two prototype bundles
Sample # Normalized CO2 Perm*
CO2/N2Select*
Fiber ID
1 24.6 27.82 22.0 313 26.9 284 20.6 265 24.9 356 17.6 27
Average 22.8 29.1Std Dev 11.6% 14.7% 3.6%
Fiber Synthesis & Bundle Forming
*Normalized to 12” PI-1 bundle performance, ambient temperature
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4” Prototype Bundle Performance
• Similar performance confirms manufacturing reproducibility
Bundles 03 and 04: 18% CO2/N2, 14.8 bar, -45°C
• Permeance and selectivity exceeding targets for 90% recovery
*Normalized to 12” PI-1 bundle performance
Minimumpermeance
Minimumselectivity
90%
reco
very
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5060708090100110120130140
04080
120160200240280320360
60% 70% 80% 90%
CO2
Perm
eate
Pur
ity (%
)
Feed
Flow
Nm
3 /h
CO2 Recovery
Feed Flow (P = 1.5 psig)Feed Flow (P = 6.5 psig)CO2 Purity (P = 1.5 psig)CO2 Purity (P = 6.5 psig)
4” Prototype Bundle Performance
• Performance improvement by process design (low permeate pressure, matches large scale conditions)
Bundle PI-2_04
• CO2 purity improvement leads to lower recycle flow, lower specific energy
Full scale conditions: 18% CO2/N2 feed, 200 psig, -45°C, 1.5 psig permeate
Success criteria:90 Nm3/h feed flow, 90% CO2 recovery, 58% permeate purity
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0
10
20
30
40
50
60
70
80
90
100
0 2 4 6 8 10 12
CO2/
N2
Sele
ctiv
ity
Normalized CO2 Permeance
PI-2 Intrinsic Fiber
PI-1, 12" (FE0013163)(performance
normalizedbased on PI-1)
1" PI-2(90% Rec,
FE0013163)
Target performance
region
1" PI-2(70% Rec)
4” Prototype Bundle Performance
• Significant improvement by using ‘forming’ method in scale-up
• Lessons learned resulting in further performance gains
1) Epoxy application for tubesheet
2) Post-treatment solution concentration
3) Outer wrap layer positioning
4) Optimize fiber ODLower CAPEX
Low
er O
PEX
Success criteria:90 Nm3/h feed flow, 90% CO2 recovery, 58% permeate purity
Air Liquide, world leader in gases for industry, health and the environmentResearch & Development23
0
10
20
30
40
50
60
70
80
90
100
0 2 4 6 8 10 12
CO2/
N2
Sele
ctiv
ity
Normalized CO2 Permeance
PI-2 Intrinsic Fiber
PI-1, 12" (FE0013163)(performance
normalizedbased on PI-1)
1" PI-2(90% Rec,
FE0013163)
Target performance
region
1" PI-2(70% Rec)
0
10
20
30
40
50
60
70
80
90
100
0 2 4 6 8 10 12
CO2/
N2
Sele
ctiv
ity
Normalized CO2 Permeance
PI-2 Intrinsic Fiber
PI-1, 12" (FE0013163)(performance
normalizedbased on PI-1)
1" PI-2(90% Rec,
FE0013163)
Target performance
region
4" PI-2_02
4" PI-2_03
4" PI-2_01(rep)
1" PI-2(70% Rec)
4" PI-2_03 & 04
4" PI-2_01
4” Prototype Bundle Performance
• Significant improvement by using ‘forming’ method in scale-up
• Lessons learned resulting in further performance gains
1) Epoxy application for tubesheet
2) Post-treatment solution concentration
3) Outer wrap layer positioning
4) Optimize fiber ODLower CAPEX
Low
er O
PEX
Success criteria:90 Nm3/h feed flow, 90% CO2 recovery, 58% permeate purity
Air Liquide, world leader in gases for industry, health and the environmentResearch & Development24
Fiber Manufacturing Cost Analysis
FE00
1316
3 TE
A
What are relative merits of cost-saving approaches?
• Best value is composite formulation
• With low polymer price monolith fiber yields CO2 capture cost savings
• Pursuing both approaches
FE00
1316
3 TE
A
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Acid Gas Contaminant Testing
0
2
4
6
8
10
12
14
0 100 200 300 400 500 600 700
CO2
Perm
eanc
e [P
CO2/
P CO
2,PI
-1,0
]Time On Stream [hours]
PI-2 (Form A)PI-2 (Form B)PI-1
18% CO2 (bal N2)200 psig, -45°C
18% CO2, 100 ppmv NO, 100 ppmv SO2 (bal N2)
200 psig, -45°C
0
50
100
150
200
250
0 100 200 300 400 500 600 700
CO2/
N2
Sele
ctiv
ity
Time On Stream [hours]
18% CO2, 100 ppmv NO, 100 ppmv SO2 (bal N2)
200 psig, -45°C
100 ppm NO & 100 ppm SO2
• PI-2 fiber permeance and selectivity tolerant towards NO and SO2
• Typical levels in flue gas after FGD: 1 – 5 ppm SO2, 50 ppm NO
Effect of acid gas contaminants on PI-2 fiber: ¼” mini modules, tested with synthetic gas mixtures, temperature controlled by lab refrigerator
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0
20
40
60
80
100
400 600 800 1000 1200 1400 1600
CO2/
N2
Sele
ctiv
ity
Time On Stream [hours]
Acid Gas Contaminant Testing
0
2
4
6
8
10
12
14
400 600 800 1000 1200 1400 1600
CO2
Perm
eanc
e [P
CO2/
P CO
2,PI
-1,0
]
Time On Stream [hours]
PI-2 (Form A)
PI-2 (Form A, duplicate)
18% CO2 (bal N2)200 psig, -45°C
Changed feed system
20 ppmv NO2 50 ppmv NO2
100
ppm
vN
O2
100 ppm NO2 (not shown)
• Nearly complete loss of permeance due to 100 ppm NO2!
• Cause was identified as solvent effect of gas on fiber micro-structure
20 – 50 ppm NO2
• Minor decline in permeance due to 20-50 ppm NO2
• Represents SCR failure case, 1 – 3 ppm NO2 typical from 0.3 MWe field-test unit
• Long-term exposure to 5 ppm:No problem
• Short-term exposure to 50 ppm:No problem
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Membrane
Skid 1Skid 3
Skid 2
Agenda
Technology & Project Overview
NCCC Testing (FE0013163)Membrane testingAnalytical campaign
PI-2 Scale-up (FE0026422)Manufacturing development
and testingAcid gas contaminants
Next StepsPI-2 scale-up to 6” sizeBack to NCCC
Air Liquide, world leader in gases for industry, health and the environmentResearch & Development28
Commercial PI-2 bundle preparationPolymer procurement scaled up to 5 lb (2.5 kg) scale) Fiber spun on DSU for full 6” bundle fabrication (>90% yield)QC testing: 24 - 30 times PI-1 permeance, 30 CO2/N2 selectivity (room temperature, post-treated) - excellent performance, best batch yet!Bundle formed, QC by air test: performance was in line with previous 4” bundles
First 6” Commercial Bundle
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Manufacturing several 6” bundles (6 – 8), test on 0.1 MWe skid in Newark, DE
Field-test at NCCC, 0.3 MWe scaleFirst test window: November 2017!
Techno-economic analysis for PI-2Updated manufacturing cost
Performance from field testing
Novel process designs considered
Next Steps
0.3 MWe Field-Test Unit at NCCC, Pilot Bay 3(DE-FE0013163)
Budget Period 2: July 2017 to December 2018
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US DOE: José Figueroa, Sheldon FunkNCCC: Frank Morton, Tony WuAir Liquide: Rob Gagliano, Shilu Fu, Sudhir Kulkarni, Dave Hasse, Mike Bennett, Dean Kratzer, Jean-Marie Gauthier
Some material in this presentation is based on work supported by the Department of Energy National Energy Technology Laboratory under Award Number DE-FE0004278 (completed), DE-FE0013163 (completed), and DE-FE0026422.
“This report was prepared as an account of work sponsored by an agency of the United States Government. Neither the United States Government nor any agency thereof, nor any of their employees, makes any warranty, express or implied, or assumes any legal liability or responsibility for the accuracy, completeness, or usefulness of any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights. Reference herein to any specific commercial product, process, or service by trade name, trademark, manufacturer, or otherwise does not necessarily constitute or imply its endorsement, recommendation, or favoring by the United States Government or any agency thereof. The views and opinions of authors expressed herein do not necessarily state or reflect those of the United States Government or any agency thereof.”
Acknowledgments / Disclaimer
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