IAPG Natural Gas Congress

Molecular Sieves:is your regeneration

procedure optimized?
CECA VETEK
Author Peter Meyer
Presenter Bob Davenport
 Why optimize the regeneration procedure?

A non optimized regeneration procedure can harm the

molecular sieves and reduce significantly their life time
New unit: if the regeneration gas is recycled the
recycled water content has to be taken in account, if
the regeneration gas flow rate is too short the unit will
not work
Knowing how to optimize the procedure can help
debottlenecking a unit

IAPG 2008
 Regeneration: how does it work?

cap PSA

cap TSA

Industrial
units

IAPG 2008
 TSA Regeneration: how does it work?

This presentation will focus on Natural Gas Drying

regenerated by Thermal Swing Adsorption (TSA).

Regeneration procedure:
1) Switch including possibly pressure change (depress.)
2) Heating (Purge? Two step heating? Heating ramp?)
3) Cooling (dry/wet gas?)
4) Switch including possibly pressure change (repress.)

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 Regeneration: parameters

Heating step: how much heat?

- Heat up the molecular sieves
- Heat up the vessel (internal/external insulation)
- Remove water
- Push out desorbed water

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 Regeneration: temperature influence

Quantity of
regeneration
gas

Minimum!! Regeneration temperature

The quantity of regeneration gas depends on the inlet temperature during the
heating. Below a minimum temperature the water dew point spec could not
be reached (too high residual water content), the maximum temperature
depends on the type of molecular sieve.

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 Regeneration: uncomplete regeneration

Adsorption
time

Adsorption cycles

A sudden decrease of adsorption time is the sign for a bad

regeneration (accumulation of water) happens very
often shortly after start up, possibility to recover sieves

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 Regeneration: uncomplete regeneration

Temperature
Regeneration time

Make sure to have a plateau at the outlet during heating.

Make sure to have a small temperature difference between
inlet and outlet during heating.

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 Regeneration: Maximum temperature

3A: 230C (446F) for saturated gases, up to 260C

(500F) for unsaturated gases

4A: normally 250C (482F), up to 290C (554F) with

precautions

For information

5A/13X: 300C (572F) in case of sweetening, but if

there is NO water on the sieves

IAPG 2008
 Regeneration: pressure influence
More regeneration gas (quantity) is needed if the regeneration
pressure is at a high pressure.
Two cases for pressure range:
Low pressure heating limited
The regeneration gas has to bring in the energy for heating and
desorption (regeneration temperature above boiling temperature
of water at regeneration pressure)
High pressure stripping limited
The regeneration gas has additionally to strip off (push out) the
desorbed water.

The limit between both is around 30-35 bars. Example: a

regeneration at 60 bar (870 psia) may require perhaps
25% more regeneration gas quantity.

IAPG 2008
 CASE STUDY

3 adsorber system, 2 in
adsorption, 1 in regeneration
500 MMSCFD, 60 bar (870
psia), 30C (86F),
Saturated gas, 4A molecular
sieve,
Adsorption time 16 hrs,
Regeneration recycled (air
cooler sat. @ 55C (131F),
30 bar (435 psia))

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 CASE STUDY

Case 1: Regeneration at 250C, 482F and 30 bar, 435 psia

Case 2: Regeneration at 250C, 482F and 60 bar, 870 psia

Case 3: Regeneration at 290C, 555F and 60 bar, 870 psia

Case 4: Regeneration optimization to minimize hydrothermal

damage and improve molecular sieves performance.
(Case 5: Correction of case 2 supposing only case 1 flow rate
available, internal heat insulation)

Fixed: pressure drop during adsorption, no stand-by time.

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 CASE 1

Case 1:
100% FR1
Regeneration
at 250C,
482F and 30
bar, 435 psia
Procedure
Depress 15 min
Heating
100% FP Cooling
Repress 15 min
Case 1
7 hrs 30 min
Vessel diameter : 100% available
Adsorbent weight : 100%

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 CASE 2

Case 2:
115% FR1
Regeneration
at 250C,
482F and 60
bar, 870 psia
Procedure
Depress 0 min
Heater /
Heating
Compressor -
100% FP Cooling
Capacity ??
Case 2 Repress 0 min
Vessel diameter : 100% 8 hrs 00 min
Adsorbent weight : 104% available

Regengasquantity : 123% 30 min more

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 CASE 3

Case 3:
108% FR1
Regeneration
at 290C,
482F and 60
bar, 870 psia
Procedure
Depress 0 min
Steel: max.
design Heating
100% FP temperature ?? Cooling
Case 3 Repress 0 min
Vessel diameter : 100% 8 hrs 00 min
Adsorbent weight : 102% available

Regengasquantity : 115%

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 CASE STUDY

MS Quantity Regengas Regengas

quantity Flow rate
CASE 1 100% 100% 100% FR1
CASE 2 104% 123% 115% FR1
CASE 3 102% 115% 108% FR1
Case 1: Regeneration at 250C, 482F and 30 bar, 435 psia
Case 2: Regeneration at 250C, 482F and 60 bar, 870 psia
Case 3: Regeneration at 290C, 555F and 60 bar, 870 psia
(possibility to reach lower dew point)
Case 4: ???

HYDROTHERMAL DAMAGING

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 Hydrothermal damaging

End of Adsorption

ETAT FINAL DE LA COLONNE(ADSORPTION), Q_H2O

18

16

14

12

quantit adsorbe (g/100g)

10

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 Hydrothermal damaging
Start of Heating

Cold saturated
section

140 Bed Temperature ramp up

120

100

80

TC

60

40

20
Srie1

0 S1
elaps
ed
time
bed length min

Heated section

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 Hydrothermal damaging

Heating proceeds ...

Cold Saturated
Section

Steam Fog B ed T empe r a tur e r a mp up

Formation 14 0

12 0

10 0

80

T C

60

S rie2
40

20

0 S1

elapsed

tim
e m
in

bed l en gt h

Hot Section

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 Hydrothermal damaging
Water Retro-condensation
during Heating
Water Droplets

Condensation Zone
R etro condes ed Water in the B ed during heating

1.0

0.9

0.8

0.7

0.6

0.5

0.4

0.3

0.2

Crust and Lumps

0.1

0.0
0 .2 4

0 .4 8

0 .7 2

0 .9 6

1 .4 4

1 .6 8

2 .1 6
1 .9 2

3 .1 2
2 .6 4

2 .8 8

3 .3 6

3 .8 4

4 .0 8

4 .3 2
1 .2

4 .5 6

5 .2 8
2 .4

5 .0 4

5 .5 2

5 .7 6
3 .6

4 .8

be d l engt h

formation
REFLUX
14 0

B e d T empe r a tur e r amp up

12 0

10 0

80

TC

60

S r ie2
40

20

0 S1
elapsed

Vaporization Zone
t ime

min

bed l en gt h

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 CASE 4

Case 4:
115% FR1
Regeneration
at 290C,
482F and 60
bar, 870 psia
Procedure
Depress 0 min
30 min intermediate
100% FP heating

Case 4 Heating

Vessel diameter : 100% Cooling

Adsorbent weight : 102% Repress 0 min

Regengasquantity : 123% 7 hrs 30 min

available
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 CASE STUDY

MS Quantity Regengas Regen flow rate

Quantity
CASE 1 100% 100% 100% FR1
CASE 2 104% 123% 115% FR1
CASE 3 102% 115% 108% FR1
CASE 4 102% 123% 115% FR1
Case 1: Regeneration at 250C, 482F and 30 bar, 435 psia
Case 2: Regeneration at 250C, 482F and 60 bar, 870 psia
Case 3: Regeneration at 290C, 555F and 60 bar, 870 psia
Case 4: Regeneration at 290C, 555F and 60 bar, 870 psia, interm. heating

Advantage of case 4: lower water dew point at outlet.

IAPG 2008
 CASE STUDY

MS Quantity Regengas Regen flow rate

quantity
CASE 1 100% 100% 100% FR1
CASE 2 104% 123% 115% FR1
CASE 3 102% 115% 108% FR1
CASE 4 102% 123% 115% FR1
Case 1: Regeneration at 250C, 482F and 30 bar, 435 psia
Case 2: Regeneration at 250C, 482F and 60 bar, 870 psia
Case 3: Regeneration at 290C, 555F and 60 bar, 870 psia
Case 4: Regeneration at 290C, 555F and 60 bar, 870 psia, interm. heating
Case 5: keep regeneration gas flow rate and MS height of case 2, internal heat
insulation , diameter 3.5 m, increase feed flow rate, decrease adsorption
time

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 CASE 5 (versus case 2)

Case 2:
100% FR2
Regeneration
at 250C,
482F and 60
bar, 870 psia
Procedure
Depress 0 min

Pressure drop Heating

140% FP 0.7 bar Cooling
Case 2 (233%) Repress 0 min
Vessel diameter : 94.6% 4 hrs 30 min
Adsorbent weight : 88% available

Regengasquantity : 61% Adsorption 9 hrs

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 CASE STUDY

MS Quantity Regengas Regen flow rate

quantity
CASE 2 100% 100% 100% FR2
CASE 5 88% 61% 100% FR2

Internal insulation, 3.7m 3.5 m internal diameter

Higher feed flow rate : 140%

Higher pressure drop during adsorption : 233%
Adsorption time down from 16hrs to 9hrs (shorter life time)

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 How to prevent hydrothermal damaging?

Hydrothermal damaging happens when liquid water is present on the

molecular sieves at high temperature:

One should try to change the regeneration procedure in order to

prevent desorption of water when the molsieve bed is not yet
heated up almost homogenously thus limiting water condensation
at top layers
intermediate heating step + higher regeneration gas flow rate

IAPG 2008
 How to prevent hydrothermal damaging?
Instantanious w ater flow
Inlet heating temperature
600 6000

500
temperature (F)

5000
Regeneration

400
4000

300 Original
3000
200
2000
100
0 1000

0 50 100 150 200 250 0

0 50 100 150 200 250
Heating time (min) R e ge ne r a t i on t i me ( mi n)

Tem perature at adsorber outlet

Original procedure: 300

250

- int. temperature too high, 200

too much water desorbed 150

- plateau of outlet
100

50
temperature showing water 0
re-vaporization 0 50 100
T i me (mi n)
150 200 250

IAPG 2008
 How to prevent hydrothermal damaging?
Instantaneous w ater flow
Inlet heating temperature
600 7000

500 6000
temperature (F)
Regeneration

400 5000
Original
300 4000
CECA
3000
200
2000
100
1000
0
0 50 100 150 200 250 0
0 50 100 150 200 250
Heating time (min) T i me (mi n)

Tem perature at adsorber outlet

New procedure: 300

250

- int. temperature lower 200

- smoother increase of outlet 150

100
temperature 50

0
0 50 100 150 200 250
T i me (mi n)

IAPG 2008
 How to prevent hydrothermal damaging?

Comparison for water maximum

200

150

100
Original w ater
CECA w ater 50
Original Temperature
CECA Temperature 0
0.00 1.00 2.00 3.00 4.00 5.00
Vessel from bottom to top

IAPG 2008
 Conclusion

When looking at your molecular sieve unit and its

regeneration procedure:
- Dont underestimate the pressure influence on the
regeneration gas quantity
- Think about hydrothermal damaging
- Optimization does not cost a lot but lengthens the life
time of the molecular sieves

Dont hesitate to ask the nice and knowledgeable guys

from CECA to help you.
THANK YOU!

IAPG 2008