2017 NETL CO2 Capture Technology Project Review Meeting Library/Events/2017/co2 capture/2... ·...

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


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


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-


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)


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


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


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


DRTC TEAM AT NCCC: Oct-2015


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


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


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


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


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


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


Membrane

Skid 1Skid 3

Skid 2

Agenda







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


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


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


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)


• 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


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)


• 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



0

10

20

30

40

50

60

70

80

90

100

0 2 4 6 8 10 12

CO2/

N2

Sele

ctiv

ity





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





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


• 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



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


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


0

20

40

60

80

100

400 600 800 1000 1200 1400 1600

CO2/

N2

Sele

ctiv

ity


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

]


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


Membrane

Skid 1Skid 3

Skid 2

Agenda







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


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


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


Research & Development

Opening new ways

THANK YOU FOR YOUR ATTENTION

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