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National Energy Technology Laboratory
Driving Innovation ♦ Delivering Results
Victor KusumaNational Energy Technology Laboratory, AECOM
NETL Carbon Capture Technology Review Meeting 2016
Automated Post-combustion Flue Gas Membrane Performance Testing Skidat the National Carbon Capture Center
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Outline
• The NETL Post-combustion Membrane Testing Skid (PCMS)• Lessons learned • Initial testing results• Ongoing testing• Future outlook
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Our home at the PC4 Bench Scale Facility
Image courtesy of Patrick Crossley and Justin Anthony, Southern Company Services
PCMS
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Our home at the PC4 Bench Scale Facility
Image courtesy of Patrick Crossley and Justin Anthony, Southern Company Services
PCMS
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Post-Combustion Membrane Testing Skid
• The proving ground for our most promising membranes• Compact footprint: can be moved as one unit• Fully automated operation: set and forget
– Designed for multiday/multiweek experiments for medium/long term testing
Feed chiller
Electricals/Electronics
Monitor
Membrane+Circulator
GC
Flow control
Gas linesFeed pump
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Post-Combustion Membrane Testing Skid
• Based on standard constant pressure membrane testing system– Mixed gas analysis using gas chromatograph– Pressurizes feed up to 30 psig, filters particulate matter, and dehumidifies
feed to avoid condensation– Accepts hollow fiber modules and flat sheet modules
Flue MFC
MFC
PT
Argon MFC
0-50 sccm*
0-50 sccm
0-50 sccm
PT
PTC
PTC
15-30 psia
Chiller
Pumped to~30 psig+7 µm filters
FI
GC
15-30 psiaPrimary membrane moduleWater bath temp. control
5-80 °C
to flue gas return~2 slm feed bypass
FI
HMT
HMT
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Software and automation
• Embedded Windows 7 rugged computer/DAQ with custom LabVIEW-based software
• Enables “setup, start and walk away” operation philosophy• Up to 5 pre-programmed pressure/flow steps• Automated GC injections for mixed gas analysis from either feed or sweep
John O’Connor
NI cDAQ-9132
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Membrane assembly
Flat sheet membrane assemblyHollow fiber membrane assembly
(Single strand)
Typical area: 0.6 to 2.7 cm2
Cross-current flowTypical length: 10 cmCounter-current flow
Membrane module
Feed
Retentate
Sweep
Permeate
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December 2015 campaign timeline
12/7/15 12/8/15 12/9/15 12/10/15 12/11/15 12/12/15
12/13/15 12/14/15 12/15/15 12/16/15 12/17/15 12/18/15
• Primary task: install and confirm PCMS operating properly– Extensive tests at NETL minimizes installation and shakedown time at NCCC
• Secondary task: test membranes (24-hour tests)– 7 membranes successfully tested: 4 hollow fibers, 3 dense flat sheet membranes
PCMS arrives@ NCCC
PCMS installation
GC bakeout
GC Cal
PDMS
HF-1
TFEPPZ HF-2
Cal
HF-3
HF-4
Film C
Unit 5 shutdown
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December 2015 feed characteristics
CO2, O2 and N2 feed compositions analyzed from retentate + permeate streams
PCMS-analyzed feed composition matches well with NCCC’s
Feed dewpoint depends on outside temperature (reduced by feed chiller to prevent condensation)
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Reference membrane: PDMS
H2O(g) permeability of PDMS: Metz, SJ; van de Ven, WJC; et al.: JMS 2005. 251, 29
• Commercial polydimethylsiloxane film
• Stable performance:– ~3300 barrer CO2– CO2/N2 around 8.5– O2/N2 around 1.9– All the above numbers
agree with lit. data• Insufficient flowrate to
measure water vapor permeability– Around 16k-18k barrer
H2O – much lower than literature ref. (40k)
– 10 sccm not enough to avoid conc. polarization
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Gen 1 mixed matrix coated hollow fibers
SIFSIX-2Cui: Nugent, P; et. al.: Nature 2013. 495, 80
SIFSIX-2Cui
PN
OCH2CF3
OCH2CF3 n
poly(bistrifluoroethoxy)phosphazene(TFE-PPZ)flat sheet TFE-PPZ/SIFSIX-2Cui (not tested at PCMS)
HF-1 (TFE-PPZ/30 wt% SIFSIX-2Cui coating)high surface porosity Torlon hollow fibers
Polymer
MOF
+Fiber
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Mixed matrix coated hollow fiber membranes
• PPZ/SIFSIX mixed matrix coated hollow fiber (HF-1)– Slight decline in all gas
permeance over 22h: CO2 from ~75 GPU to ~70 GPU
– Insufficient time to determine decline significance
All hollow fibers are assumed: length = 10 cm, outer diameter = 540 µm
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Summer 2016 campaign timeline
5 6 7 8
27 28 29
July
8
24 25 26 22 23
August September
• Three membranes planned this season– Focus on medium term tests (3-4 weeks) to gain operational
experience– Whenever available, test thin film hollow fiber composite membranes– One three-week test successfully concluded on a free-standing film– Ongoing testing on membrane #2
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PDMS re-run to verify operation
• Confirmed PCMS still working after 6 months downtime
• Confirmed CO2, O2, N2results against previous run
• Higher apparent H2O permeability (25k-28k barrer) with 50 sccmfeed flowrate
• Hourly sampling frequency
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Conclusions
• We have an operational membrane testing skid at NCCC– Versatile for testing different membrane formats– Short term testing gives data well corroborated with literature values
and/or other testing equipment at NETL– Sufficient feed flowrate is required to quantify water vapor permeance
accurately• Short term membrane performance at low humidity +
contaminants consistent with performance under dry, ideal conditions
• The PCMS can be operated unattended for longer periods of time– We have completed a three-week unattended test– The skid can tolerate several process upsets (e.g. temporary loss of feed
flue gas)– Gas chromatograph maintenance imposes the biggest limitation on testing
length
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Future plan
• Finish current testing season at NCCC– Up to two additional membranes to be tested
(4 week runs)– Upgrade feed flowrate capability to measure
water vapor permeance
• Design improvements– More efficient water vapor removal to
protect GC columns– Flow components to accommodate small
multi-fiber modules
• Continue developing membranes with focus on thin film composite hollow fiber membranes
Gen 1 coated HF (tested)
Gen 2 coated HF (in development)
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Acknowledgements
NETL• Justin Anthony• Bob Lambrecht• NCCC process engineers• Caddell construction crew
• Heather Juzwa• Mark Waksmonski• Yuan Lin
NCCC
Shimadzu Corp.
• Kevin Resnik• Dave Hopkinson• John O’Connor• Jeffrey Hash• Ron Hirsh• Ray Rokicki• Bill Walker• Rocky Stoneking• Rich Valdisera• Surendar Venna• Shan Wickramanayake• Ganpat Dahe • Ali Sekizkardes• Christina Myers
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This project was funded by the Department of Energy, National Energy Technology Laboratory, an agency of the United States Government, through a support contract with AECOM. Neither the United States Government nor any agency thereof, nor any of their employees, nor AECOM, nor any of their employees, makes any warranty, expressed 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.
Thank you for your attention!
This technical effort was performed in support of the National Energy Technology Laboratory’s ongoing research under the RES contract DE‐FE0004000.