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SOLUCIONARIO EDITATORIAL CUZCANO CEPRE UNI
2011 S nthe nthesis Gas Se Semina minar – Mar arita rit a Feed Feed Pretrea Pretr eatm tment ent November 2–4, 2011
Feed Gas Treatment
•
Steam HC Feed
HTS
u ur
S Coking Cl S Pu r i f i c at i o n
ro em components
Chlorides
Pr e Ref o r m er Primary Reformer
CO2 Reforming
S H2 HT CO Sh if if t LT CO Sh if if t
SynGas Seminar – Margarita – Nov 2-4,2011
CO 2 Removal Methanation
Page 2
Feed Gas Treatment
•
Steam HC Feed
HTS
u ur
S Coking Cl S Pu r i f i c at i o n
ro em components
Chlorides
Pr e Ref o r m er Primary Reformer
CO2 Reforming
S H2 HT CO Sh if if t LT CO Sh if if t
SynGas Seminar – Margarita – Nov 2-4,2011
CO 2 Removal Methanation
Page 2
Feed Gas Treatment
•
c va e ar on – adsorption of H 2S + organic S y ro esu ur za on
–
convert organic S to H 2S onver organ c c or es o
Chlo lori ride de Gua Guard rd – re remo move ve HCl HCl • Ch • nc x e – sor 2 Sulf lfur ur re remo mova vall • ActiSorb® G 1 – Su
SynGas Seminar – Margarita – Nov 2-4,2011
Page 3
Activated Carbon: C8-6 / C8ADVANTAGES
DISADVANTAGE
• Low Cost • Regenerable •
• Ca
Operation ffe ect ctiv ive e on Vir Virtu tua all • Eff all Sul ulfu furr Specie pecies s
SynGas Seminar – Margarita – Nov 2-4,2011
ac i t A f f ec t ed b Heavy Hyd ydro rocarbon carbons s
f or Fre • Need for
uent ue nt
Regeneration missions ions Contro ontroll • Emiss duri du ring ng Regene generatio ration n
Page 4
Lead-Lag Reactors Raw Natural Gas Feed
Regeneration Steam
Activated Carbon
• m ent temperature • Steam before initial use • Regenerate upflow with steam to vent (or hot NG/fuel )
on ro s eam ve oc y o preven < 0.5 ft/sec (SLV)
u
za on
regeneration may need to condense/capture regeneration steam and hydrocarbons
No oxygen in steam if above 400ºF (205ºC)
• No oxygen > 200ºF (95ºC) without steam
Activated Carbon - Operation
• u ur capac ty s re uce a ove • Typical operating cycle 7-14 days • Typical feeds: < 5 ppmv RSH
o
< 5 ppmv H2S
• Troublesome contaminants:
Heavy hydrocarbons can reduce capacity
CO2 (>5 %) can reduce capacity significantly
Water vapor can reduce capacity somewhat
Activated Carbon - Operation apac ty
etween
egenerat ons
SCF of Feed per Ft³ of C8-7
Sulfur Type H2S R-SH
ppm SCF/ft³ -
,
3-5
130,000
1-3
260,000
3-5
130,000
COS passes through Re en C cle de ends on
Activated Carbon - Problems
Surface Contamination
Heavy Hydrocarbon Buildup o
C5+ can reduce capacity 50%
o
Insufficient regeneration temperature
Increased Inlet Sulfur o Adsorbent o
capacity is fixed
Cycle length is inversely proportional to S content
3% H2O can reduce capacity 20-30%
Hi h inlet tem erature - > 125ºF 50ºC ca acit falls o
Feed Gas Treatment
•
c va e
ar on – a sorp on o
2
an organ c
• Hydrodesulfurization (HDS) –
conver organ c
o
Convert organic chlorides to HCl
2
• or e uar – remove • Zinc Oxide – Adsorb H2S • ActiSorb® G 1 – Sulfur removal
Hydrodesulfurization HDMax ® 200 Series
®
CoMo on Alumina
HDMax® Catalysts
Catalyst Wt % CoO Wt% NiO Wt% MoO3 Alumina Operating Temp ºF
HDMax 200 HDMax 30 4.5 --18.5 Balance 450-800 -
--4.9 20.0 Balance 450-800 -
• Converts all S species to H 2S – downstream H2S trap – owns ream rap • onver s spec es o • Hydrogenates olefins
HDMax® Reactions -
+
-
2
RSR’ + 2 H2
C4H4S + 4 H2
2
RH + R’H + H2S
RS-SR’ + 3 H2 COS + H2
+
RH + R’H + 2 H2S CO + H2S C4H10 + H2S
2
Olefins
RnH2n + H2
RnH2n+2 + Heat
Needed when > 0.5% olefins ΔT
= ~15-18ºF (8-10ºC) per 1% molar
HDMax® - Operation
• Temperature
Min-Max = 450-800ºF (230-425ºC) yp ca range = Limits risk of hydrocarbon cracking
• • Sulfiding
•H
-
,
Olefins in the feed – must be pre-sulfided
dro en Re uirement
Typical H2 = 4-7 psia (0.3-0.5 bara)
Olefins H2 = stoichiometric + 5-10% excess in the efflu
Sulfiding Reactions u
ng
CoO + 0.11H2 + 0.89H2S MoO3 + 2H2S 3NiO + H2 + 2H2S
CoS0.89 + H2 MoS2 + 3H2O Ni 3S2 + H2O
Desulfiding CoS0.89 + 0.89H2
Co + 0.89H2S
MoS2 + 2H2
Mo + 2H2S
Ni 3S2 + 2H2
2Ni + 2H2S
H2S to Sulfide CoO 1.00E+01 1.00E+00
0.1 Bar H2 Partial Pressure 1 Bar H2 Partial Pressure 5 Bar H2 Partial Pressure
.
-
1.00E-02 .
-
1.00E-04 1.00E-05 1.00E-06 1.00E-07 1.00E-08
10 Bar H2 Partial Pressure
H2S to Sulfide NiO 1.00E+03 0.1 Bar H2 Partial Pressure
1.00E+02
1 Bar H2 Partial Pressure 5 Bar H2 Partial Pressure 10 Bar H2 Partial Pressure
1.00E+01
.
1.00E-01
1.00E-02
1.00E-03
1.00E-04
H2S to Sulfide MoO 3 .
1.00E+00
0.1 Bar H2 Partial Pressure 1 Bar H2 Partial Pressure
1.00E-01
1.00E-02
1.00E-03
.
-
1.00E-05
1.00E-06
1.00E-07
10 Bar H2 Partial Pressure
HDS Special Consideration
Carbon laydown and ΔP buildup
Minimize H2 recycle – possibly < 1%
• • Shutdown
Maintain with inert gas (could be N2, H2, NG)
If Olefins in the feed, purge with inert gas during
Feed Gas Treatment
•
ct vate
ar on – a sorpt on o
2
S y ro esu ur za on
–
• convert organic S to H2S
• Chloride Guard – remove HCl –
2
• ActiSorb® G 1 – Sulfur removal
an organ
Cl Guard – ActiSorb® Cl 2
Alkali ≥ 6.5% LOI ≤ 7.0% Alumina Balance Density 45 lbs/ . g
ActiSorb® Cl 2
• or es are a very strong po son to t e ZnCl 2 + H2O • Reacts with ZnO: ZnO + 2HCl n
2
su
• Reaction
mes ~ Na2O + 2HCl
2NaCl + H2O
• Operating Temperature = 70-850ºF (20-450ºC) • Vapor Phase or Liquid Phase • Cl pickup = 8-10% wt. • Typically a layer on top of the ActiSorb® S 2
Feed Gas Treatment
•
ct vate
ar on – a sorpt on o
S y ro esu ur za on
–
• convert organic S to H2S
• Chloride Guard – remove HCl –
2
• ActiSorb® G 1 – Sulfur removal
2
an organ
Zinc Oxide – ActiSorb® S 2
ActiSorb® S 2 2
(g)
+ n
(s)
n
(s)
+
2
(v)
• An ADSORBENT, not a catalyst • ZnO is consumed by H2S containing gas • Not regenerable • Must be replaced when it no longer adsorbs Sulfu
• Typical performance 40-60 ppbv (Zn-ZnS equilibr • With Pre-Reformer recommend bottom layer of ActiSorb® 305 to achieve < 10 ppb
Component
ppmv
Temperature
Limited, Short-term Capacity for Organic Sulfurs
RSH / RS-SR'
< 10
>600ºF (315ºC)
RSR'
< < 10
> º º >750ºF (400ºC)
• For temporary, unavoidable circumstances •
ActiSorb® S 2 Capacity for H S Ambient e m u l o V r e P t g W ( p u k c i P r u l u S
Optimized
Sulfur Adsorption
• • Surface adsorption (gas diffusion) • Solid diffusion • Saturated
Axial Profile of Sulfur Level Satu rated
So lid Diffu s io n
Gas Diffu s io n
Fres h Cata
Saturated With S
ActiSorb® S 2 Capacity for H S Ambient e m u l o V r e P t g W ( p u k c i P r u l u S
Optimized
ZnO Optimization
•
er ormance resu ts rom:
Physical Integrity
ZnO Content – active ingredient
Density of finished product
Surface Area – better diffusion
High and Low Surface Area 5
4 Low Surface Area ZnO
2
1 High Surface Area ZnO 0 0
20
40
60
80
100
ZnO Problems
Surface contamination o
Cracking in the feed heater coil
o Affects o At
structure
>500ºF >260ºC can move downstream; corrosion
CO2 + ZnO
ZnCO3 (Zinc Carbonate)
o
Forms rapidly 200-500ºF (95-260ºC)
o
Weakens the physical structure
o
Reduces amount of Zn available to form ZnS
Comparing Adsorbents
System Design Choices – 1 Vessel Medium / High Temperature – Single Bed Cobalt Moly / ZnO Hydrogenation of Sulfur to H2S RAW GAS
•
vantages – Lowest initial cost system –
CoMo
and not sensitive to changes
• Disadvantages ZnO
– CoMo “ Thrown” Away – Lower Capacity than a 2-bed
PURIFIED GAS
– Plant must shut down to changeout
System Design Choices – Lead/Lag Medium / High Temperature – Dual Bed Cobalt Moly / ZnO Hydrogenation of Sulfur to H2S
• – Handles ALL sulfur species and not sensitive to changes CoMo
CoMo
ZnO
ZnO
– Increased Sulfur Capacity 50% –
ange
n
e
• Disadvantages –
“
”
– Increased Cost in vessels/material
un
System Design Choices: 3-Bed Medium / High Temperature – 3 Bed System Cobalt Moly / ZnO Hydrogenation of Sulfur to H2S
• – Handles ALL sulfur species
RAW GAS
– – Increased Sulfur Capacity ZnO o o
ZnO
– Change “ On the Run”
• Disadvantages – Highest Cost in
PURIFIED GAS
Feed Gas Treatment
•
ct vate
ar on – a sorpt on o
2
S y ro esu ur za on
–
• convert organic S to H2S
• Chloride Guard – remove HCl – • ActiSorb® G 1 – Sulfur removal
an organ
ActiSorb® G 1
and Sulfur Adsorption
ActiSorb® G 1 Cu
1.5% wt
Mo
3.5% wt
ZnO
Balance ²
Density
75-85 lbs/ft³ . - .
• Same ZnO lbs/ft³ as ActiSorb® S 2 ame
apac y
• HDS activity even after S saturation
System Design Choices: 1 Vessel Single Bed – Optimized use of Actisorb G-1
CoMo
-1 ZnO -
PURIFIED GAS
Option 1 - Lower Cost for CoMo required) p on - p o onge Life with fixed reactor volume (replace CoMo with G-1)
System Design Choices – Lead/Lag Dual Bed – Optimized use of Actisorb G-1 RAW GAS
pt on - ower ost or Same Time On-stream (no CoMo re uired
CoMo
CoMo
Option 2 - Up to 30-50% longe G-
ZnO
1
G-
ZnO
1
(replace CoMo with G-1)
System Design Choices: 3-Bed
3 Bed System – Actisorb G-1 The CoMo Vessel
RAW GAS
(new designs or replacement) ZnO G-1 CoMo
ZnO G-1
CO2 and COS
•
n
as some trou e w t H2S + CO2
an
2
n t e ee
COS + H2O
• Higher CO2 means higher COS • Small amount of H2O helps – COS hydrolysis COS + H2O
CO2 + H2S
• ActiSorb® G 1 can solve the problem
SynGas Seminar – Margarita – Nov 2-4,2011
Page 44
ActiSorb® G 1 and COS
•
t
o o
COS + H2 COS + H2O
o H2S + CO Hydrogenation H2S + CO2 Hydrolysis
• Leaving equilibrium COS • In ZnO H2S + ZnO
ZnS + H2O
• ActiSorb® G 1 has Hydrogenation/Hydrolysis to the bottom of the bed and continuous H 2S adsorption
• As H2S concentration decreases so does COS equilibrium
• With H2S concentration ~50 ppb, COS eq = ~0 SynGas Seminar – Margarita – Nov 2-4,2011
Page 45
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