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Idaho National Engineering and Environmental Laboratory

Absorption of CO2by AqueousDiethanolamine Solutions in aVortex Tube Gas-LiquidContactor and Separator

Participants:

INEEL: Daniel S. Wendt,

(208-526-3996, [email protected])

Michael G. Mc Kellar(208-526-1346, [email protected])

Anna K. Podgorney

Douglas E. Stacey

Terry D. TurnerConocoPhillips Canada:

Kevin T. Raterman

May 6, 2003Supported by U.S. DOE (DESupported by U.S. DOE (DE--AC07AC07--99ID13727)99ID13727)

ParticipantsPoster PresentationsPlenary SessionsTechnical SessionsMain Menu

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Project Objectives: Low capital cost due to compact, simple design

High CO2capture efficiency high efficiency mass transfer

reduced solvent regeneration requirements

Operationally flexible

turn-down & scale-up with parallel design

easily accommodates variable flow rates and gas

compositions

low maintenance/portable configuration Works equally well for physical / chemical absorbents

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Jet type absorbers highly efficientReactor Type kl a ( s-1 x 100)

Packed tower 7

Sieve plate 40

Venturi reactor 25

Bubble column 24

Impinging jet 122

(Herskowits et. al.)

High Shear Jet Absorber

highly turbulent... large interfacial

area for mass transfer

multiple jets impingement zonecreates secondary drop breakup / greater area for mass transfer

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High Efficiency Absorption. acid gas separation Co-inject chemical or physical absorbent

COCO22 + 2R+ 2R22NHNH RR22NCOONCOO-- + R+ R22NHNH22++

RR22NCOONCOO-- + H+ H22OO RR22NH + HCONH + HCO33

--

R designatesR designatesCC22HH44--OHOH

Mass transfer rate ~ f(interfacial area, film thickness) Vortex tube

high differential gas-liquid acceleration - small drops

high turbulence - small film thickness GOAL achieve near equilibrium acid gas loading

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Vortex Tube with Liquid Separator

Lorey, et. al., 1998

Cool

Gas

Outlet

8 atm2 C

Gas Inlet

12.6 atm

9 CHot Gas Outlet

8.6 atm

7 C

Liquid

Outlet

J-T Temperature = 5 C

Joule-Thomson expansion

near sonic to supersonic velocity

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Scaled Contactor Process-wellhead (~Mscfd) to full gas plant (~MMscfd)-distributed engine (~Mscfd) to centralized power plant (~MMscfd)

Flash

Feed CO2 MixCO2

CO2

StripperAbsorbent

Clean Gas

Parallel VortexContactors

(Heat Regeneration if needed)Simple Process Schematic

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Vortex Contactor

Separator TubeSeparator TubeNozzleNozzle

Boroscope / Throttle

Vortex ContactorVortex Contactor

Gas Exit

Liquid inlet

Gas Inlet

Liquid Exit

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Contactor Prototype

60 SLPM @ 100 psia inlet

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Gas - Liquid Loading Tests

Achieve >95% gas-liquid separation for

stoichiometric loading of a 15% volume CO2mixture

Design parameters

vortex inlet

tube design

tapered & slotted stepped with holes

tube length

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Stepped tube design exceedsgas/liquid separation target

0

10

20

30

40

50

60

70

80

90

100

0 200 400 600 800 1000

Inlet Liquid Flow Rate (cm3/minute)

Gas/Liq

uidSeparationEfficiency

(%)

0

5

10

15

20

25

30

35

40

45

Liqui

d/GasRatio(massbasis)

Separation Efficiency

Liquid/Gas Ratio

Inlet Pressure @ 100 psia

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Stepped tube design exceedsgas/liquid separation target

0

100

200

300

400

500

600

700

800

0 200 400 600 800 1000


Liqu

idOutletFlow

(cm3/min)

0

5

10

15

20

25

30

35

40

45

Liquid/GasRatio(ma

ssbasis)

liquid side

gas side

L/G

Inlet Pressure @ 100 psia

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CO2/DEA Baseline Test Apparatus

CO2supply

N2supply

Reg Reg

CO2 FlowController

N2 FlowController

P

T

T P

Gas

Chromato-graph

P

P

Flowmeter

Liquid

T

Exit HighFlow

Exit LowFlow

TescomCheck Valve

Tescom

Liquid Pump

LiquidCollect-

ionVessel

LiquidCoalescer

VacuumPump

Hood

Atmosphere

Atmosphere

Vortex Tube

Air InletPress.

Air Inlet

Temp.

Hot AirOutletTemp.

Hot ExitPress.

LiquidOutletTemp

LiquidInlet

Press.

ExitPress.

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CO2/DEA Baseline Testing Operation

Operating Parameters

100-500 cm3

/min liquid flow rate 15-50 wt% liquid DEA composition

80-200 psig inlet gas pressure

5-15 mol% inlet gas CO2composition

25-75 slpm inlet gas flow rate (dependent variable)

Solvent loading and CO2capture efficiency unsatisfactory in

baseline testing

Diagnostic testing indicated increased residence time required process modifications necessary

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Process Modifications Modifications to process hardware

increase gas-liquid contact time capacity to adjust the gas-liquid contactor geometric configuration

maintain ability to control the inlet gas pressure and CO2 : DEA

feed stream mole ratio

Modifications to process operating parameters

75-350 cm3/min liquid flow rate

30 wt% liquid DEA composition

70 slpm inlet gas flow rate 10 mol% inlet gas CO2composition

170-250 psig inlet gas pressure (dependent variable)

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Baseline and Modified Process

Configurations

CO2supply

N2supply

Reg Reg

CO2 FlowController

N2 FlowController

P

T

T P

Gas

Chromato-graph

P

P

Flowmeter

Liquid

T

Exit HighFlow

Exit LowFlow

TescomCheck Valve

Tescom

Liquid Pump

LiquidCollect-

ionVessel

LiquidCoalescer

VacuumPump

Hood

Atmosphere

Atmosphere

Vortex Tube

Air InletPress.

Air Inlet

Temp.

Hot AirOutletTemp.

Hot ExitPress.

LiquidOutletTemp

LiquidInlet

Press.

ExitPress.

CO2

supply

N2

supply

Reg Reg

CO2 Flow

Controller

N2 FlowController

P

T

T P

GasChromato-

graph

P

P

Flowmeter

LiquidSupply

T

Exit HighFlow

Exit LowFlow

Check Valve

Liquid Pump

LiquidCollect-

ionVessel

LiquidCoalescer

VacuumPump

Hood

Atmosphere

Atmosphere

Air InletPress.

Air InletTemp.

Hot Air

OutletTemp.

Hot Exit

Press.

LiquidOutlet

Temp

LiquidInlet

Press.

ExitPress.

Contactor

TescomBack Press.Regulator

TescomBack Press.

Regulator

Modified

Contactor/

Separator

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Inlet gas pressure as a function ofliquid flow rateFouling is caused by deposits accumulating in the vortex tube nozzles

0

50

100

150

200

250

300

0 50 100 150 200 250 300 350


InletGasPress

ure(psia)

0

50

100

150

200

250

300

0 50 100 150 200 250 300 350

Inlet Liquid Flow Rate (cm 3/minute)

InletGasPress

ure(psia)

No Nozzle Fouling Nozzle Fouling Present

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CO2capture efficiency as functionof liquid flow rate

0%

10%

20%

30%

40%

50%

60%

70%

80%

90%

100%

0 50 100 150 200 250 300 350 400 450 500 550 600


CO

2CaptureEfficien

cy(%)

Modified Configuration 1









Mo dified Co nfiguration 10



30 wt%DEA, 10%C O2, 90 p sig

15wt%DEA, 10%CO2, 90 psig

30 wt%DEA, 10%C O2, MAX p sig

50wt%DEA, 10%C O2, 100 ps ig

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CO2capture efficiency as functionof liquid flow rate (no fouling)

0%

10%

20%

30%

40%

50%

60%

70%

80%

90%

100%

0 50 100 150 200 250 300 350 400 450 500 550 600

Inlet Liquid Flow Rate (cm 3/minute )

CO

2CaptureEfficien

cy(%)





Mo dified Co nfigurat ion 11

Mo dified Co nfigurat ion 12

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CO2capture efficiency as functionof liquid flow rate (fouling present)

0%

10%

20%

30%

40%

50%

60%

70%

80%

90%

100%

0 50 100 150 200 250 300 350 400 450 500 550 600


CO

2CaptureEfficiency(%)

Mo dified C onfiguration 3






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Solvent loading as function ofliquid flow rate

0.00

0.05

0.10

0.15

0.20

0.25

0.30

0.35

0.40

0.45

0.50

0 50 100 150 200 250 300 350 400 450 500 550 600


SolventLoading[moleCO

2/moleDEA] Modified Configurat ion 1

Modified Configurat ion 2








Modifie d Conf igura t ion 10

Modifie d Configura t ion 11

Modifie d Configura t ion 12

30wt % DEA, 10% CO2, 9 0 psig

15wt% DEA, 10% CO2, 90 psig

30wt % DEA, 10% CO2, MAX psig

50wt% DEA, 10% CO2, 100 psig

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Solvent loading as function ofliquid flow rate (no fouling)

0.00

0.05

0.10

0.15

0.20

0.25

0.30

0.35

0.40

0.45

0.50

0 50 100 150 200 250 300 350 400 450 500 550 600


Solvent

Loading[moleCO

2/moleDEA]







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Solvent loading as function ofliquid flow rate (fouling present)

0.00

0.05

0.10

0.15

0.20

0.25

0.30

0.35

0.40

0.45

0.50

0 50 100 150 200 250 300 350 400 450 500 550 600


Solvent

Loading[moleCO

2/moleDEA]

Modified Configuration 3Modified Configuration 4





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Conclusions Gas/Liquid separation efficiencies in excess of 95%

Non-optimized vortex tube testing has resulted incarbon dioxide capture efficiencies of up to 86%

Solvent loading as high as 0.49 moles CO2/mole

DEA

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Future Research/Applications Process hardware optimization

Scaled contactor and separator Additional solvents

Additional CO2applications

H2S

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References Herskowits,D.; Herskowits,V.; Stephan, K .; Tamir. A.: Characterization of a two-phase

impinging jet absorber. II. Absorption with chemical reaction of CO2 in NaOH solutions.

Chem. Eng. Science 45 (1990) 1281-1287

Lorey, M., Steinle, J., Thomas, K. 1998. Industrial Application of Vortex Tube Separation

Technology Utilizing the Ranque-Hilsch Effect, presented at the 1998 SPE European

Petroleum Conference, The Hague, Netherlands, October 20-22.

Chakma, A., Chornet, E., Overend, R. P., and Dawson, W. H., Absorption of CO2by

Aqueous Diethanolamine (DEA) Solutions in a High Shear Jet Absorber, The Canadian

Journal of Chemical Engineering, Volume 68, August 1990. Lee, J. I., Otto, F. D., and Mather, A. E., Solubility of Carbon Dioxide in Aqueous

Diethanolamine Solutions at High Pressures, Journal of Chemical and Engineering Data,

Vol. 17, No. 4, 1972.

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