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SulfaTreat, a Business Unit of MI L.L.C. A Smith/Schlumberger Company
Thomas G. Braga Manager, Research and Development
© 2004 Copyright MI L.L.C.
Who is SulfaTreat?
A World Leader in H 2 S Removal for More than a Decade Today there are over 1,000 SulfaTreat installations worldwide in more than 20 countries. Almost 3 trillion cubic feet of gas is processed by SulfaTreat annually.
© 2004 Copyright MI L.L.C.
SulfaTreat Technology
Gas Flowrate, MMscfd Gas Flowrate, MMscfd
0.2 TPD sulfur
25 TPD sulfur
Amine/Claus
SulfaTreat Direct Oxidation SulfaTreat Direct Oxidation
[H2S
]
SulfaTreat
© 2004 Copyright MI L.L.C.
What is SulfaTreat?
SulfaTreat is a dry, freeflowing iron oxide based media that selectively removes H 2 S and some light mercaptans from vapor and liquid streams.
SulfaTreat is environmentally nonhazardous and safe in unreacted and reacted forms.
SulfaTreat has uniform shape and size between 4 and 40 mesh.
SulfaTreat has a density of 70 lbs/ft 3
SulfaTreat is available in 50 lb and 2000 lb bags.
© 2004 Copyright MI L.L.C.
SulfaTreat Products
Product suitable for low pressure applications and odor control SulfaTreat 410 HP
Faster reaction rates in water saturated gas streams Gas streams with >80 percent relative humidity Removal of some ethyl and methyl mercaptans
SulfaTreat HP
Similar to Standard product with up to 3 x bed life SulfaTreat XLP
Standard product SulfaTreat
© 2004 Copyright MI L.L.C.
SulfaTreat Quality
§Using SPC methodology, SulfaTreat is manufactured to be “in control” and “capable”.
SulfaTreat (410)
dP = 0.084e 0.247(% fines)
R 2 = 0.931
0.0
0.5
1.0
1.5
2.0
2.5
0.0 2.0 4.0 6.0 8.0 10.0 12.0 14.0
% fines (30 mesh) dP
, psi / ' m
edia (@
1 cfm
lab un
it)
EPS dP model
© 2004 Copyright MI L.L.C.
Why is SulfaTreat Safe?
SulfaTreat begins as a safe and stable compound that is environmentally non hazardous . It reacts with H 2 S to form “pyrite”, also stable compound.
SulfaTreat meets EPA guidelines for classification as nonhazardous waste.
© 2004 Copyright MI L.L.C.
Environmental Impact
Spent media samples of representative applications were collected and tested. l Total Metals Method 6010B: Hg, As, Pb, Se, Ba, Cd, Cr, Ag
l TCLP Method 6010B: Hg, As, Pb, Se, Ba, Cd, Cr, Ag
l Volatile Organics Method 8260B
© 2004 Copyright MI L.L.C.
Environmental Impact
"The chemical analyses of these representative samples have shown that in no instance has the spent media absorbed enough material and subsequently released it upon undergoing the “hazardous metals test” or VOC test to be deemed hazardous waste, as defined by the U.S. Environmental Protection Agency. Many states have their own limitations, frequently lower than that of the federal government, that must be adhered to when disposal of a material occurs and this must be investigated in each case in order to ensure compliance. However, the levels obtained by independent analysis thus far are well below currently existing state levels."
© 2004 Copyright MI L.L.C.
How is SulfaTreat Used?
The SulfaTreat System should be placed upstream of dehydration.
© 2004 Copyright MI L.L.C.
What is a Lead/Lag System?
The Lead/Lag arrangement allows more efficient use of the SulfaTreat material with no interruption in unit service and greater process reliability.
© 2004 Copyright MI L.L.C.
TwoVessel LeadLag Mass Transfer Zone
1 2 3 4 1 2 3 4
Tower # 1 Tower # 2
Time Intervals Time Intervals
© 2004 Copyright MI L.L.C.
Lead/lag advantages
§ More efficient use of SulfaTreat § Buildin guard bed §No shutdown during changeout §Valve systems allows flexibility
© 2004 Copyright MI L.L.C.
SulfaTreat Products
Removes hydrogen sulfide and some light mercaptans from liquid hydrocarbons SulfaTreat HC
© 2004 Copyright MI L.L.C.
SulfaTreatHC Uses
gasoline • industrial water kerosene (non potable) NGL LNG LPG solvents
Treatment of clear light liquid hydrocarbons and water
© 2004 Copyright MI L.L.C.
Use Specifications
§ Reduction and conversion of aggressive sulfur contaminants to meet copper strip corrosion test for liquid fuels.
§ Liquid phase treatment for odor control and reduction of total sulfur content
© 2004 Copyright MI L.L.C.
Use Specifications
Copper Strip Tarnish Test ASTM D 13094 Most common goal of SulfaCleanHC Use Grade 1 criteria, 1A if necessary
© 2004 Copyright MI L.L.C.
Use Specifications
Odor Control §Commonly used in solvents § Industrial / Process water
Reduction of Total Sulfur Content “Removal” of mercaptans §Only methyl and ethyl mercaptans removed §50% reacted ; 50% converted to disulfides §Important in total S reduction
© 2004 Copyright MI L.L.C.
Market Analysis
Gas Flowrate, MMscfd Gas Flowrate, MMscfd
0.2 TPD sulfur
25 TPD sulfur
SulfaTreat
Amine/Claus
SulfaTreat Direct SulfaTreat Direct Oxidation Oxidation
© 2004 Copyright MI L.L.C.
SulfaTreatDO Partners
•Uses a proprietary, patented catalyst developed by TDA Research, Inc. •Engineering / Fabrication support from Westfield Engineering.
© 2004 Copyright MI L.L.C.
Direct Oxidation Process
•Catalytic oxidation of hydrogen sulfide to elemental sulfur and water.
•Under properly controlled conditions, little or no SO2 produced.
) ( 2 ) ( 8 ) ( 2 ) ( 2 8 1 5 . 0 g g
Catalyst TDA g g O H S O S H + → +
© 2004 Copyright MI L.L.C.
AIR
INLET GAS
SULFUR
Feed Preheater
Fuel/air Direct Oxidation Reactor
Sulfur Condenser
Flue gas
Liquid knockout
SulfaTreat
OUTLET GAS
Process Flow Diagram
1. Liquid is separated
2. Gas is heated to 350ºF & air injected if necessary
3. 8595% of H2S is catalyzed to gaseous sulfur
4. Gas is cooled to 200 to 250ºF to condense liquid sulfur
Sulfur Quench
5. Sulfur mist is removed
6. H 2 S is polished.
© 2004 Copyright MI L.L.C.
Catalyst Development
•Laboratory bench scale testing •Field bench scale testing •Field full scale Pilot Test
The commercial catalyst has been developed and tested under the following conditions.
© 2004 Copyright MI L.L.C.
1,200+ hour continuous operation: l Gas Source: Associated gas l Flow Rate: up to 710 Nm 3 /hr l Operating Conditions ü 0.8% H 2 S ü 20% methane ü 15% ethane ü 10% propane ü Balance CO 2 ü >2300 ppm BTEX ü ~100 ppm mercaptans ü 400 lbs/day of sulfur
Pilot Test
Heater Reactor Condenser
© 2004 Copyright MI L.L.C.
Full Scale Pilot Test Actual Unit
Sulfur condenser
Reactor
Electric heater attaches here
Flare line
Gas inlet not attached in this photo
Sulfur storage pots
Sulfur condenser
Reactor
Electric heater attaches here
Flare line
Gas inlet not attached in this photo
Sulfur storage pots
© 2004 Copyright MI L.L.C.
Full Scale Pilot Test Unit Process Conditions – Reaction Temperature
90
92
94
96
98
100
180 185 190 195 200 205 210
Temperature ( C)
H S con
version (%
)
80
84
88
92
96
100
S se
lectivity
(%)
© 2004 Copyright MI L.L.C.
Full Scale Pilot Test Unit Process Conditions – Sulfur Dew Point
0 50 100 150 200 250 0.000
0.001
0.002
0.003
0.004
0.005
0.006
0.007
0.008 File: C:\STEVE GEBHARD\SG_ PROJECTS\SULFUR projects\WHITING FIELD TEST\sulfurDP.OGI
C
kmol
Temperature
S
S8(g) S6(g) S2(g)
S7(g) S5(g)
© 2004 Copyright MI L.L.C.
Pilot Test Results Gas Chromatography Analysis
• 88 % removal of H2S • 80 % removal of mercaptans • No change in hydrocarbon content
Component Mol% (inlet) Mol% (outlet) Component Mol% (inlet) Mol% (outlet) H2S 0.8000 0.095 cyclohexane 0.17 0.14 N2 1.6 2.9 nheptane 0.09 0.07
CH4 17.7 17.8 methylcyclohexane 0.05 0.04 CO2 58.6 58.7 toluene 0.02 0.01
Ethane 8.7 8.6 noctane 0.005 0.003 Propane 6.5 6.3 ethyl benzene 0.003 0.002
isobutane 0.98 0.92 p and m xylene 0.003 0.003 nbutane 2.38 2.32 oxylene 0.0007 0.0004
isopentane 0.74 0.71 nnonane 0.0022 npentane 0.77 0.75
cyclopentane 0.01 0.01 Mercaptans (ppm) 101.00 20 2methylpentane 0.15 0.14 3methylpentane 0.13 0.12 Specific gravity
(air =1 ) 0.45
nhexane 0.27 0.24 Gross BTU/CF dry 731.00 methylcyclopentane 0.14 0.12 Gross BTU/CF wet 718.00
benzene 0.21 0.17
© 2004 Copyright MI L.L.C.
Applications
§Two units scheduled for commissioning in 1 st Quarter 2006