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. It was compiled by process experts from several major oil and gas processing companies and independent consultants. It is based on their collective experiences relating to operating guidelines for H2S/CO2 amine systems. The intent is to help the industry better understand and operate their amine plants with the goals of improved environmental compliance, improved reliability, reduced operating costs, and improved sulfur plant operation. In putting this document together, a number of assumptions were made. Some of the key assumptions, particularly in the “action” section, include:
• Plant equipment functions as designed and is correctly designed. • All instrument readings (flows, temperatures, and pressures) are correct;
“repair instruments” is not included as a listed action.
• Amine quality is within established limits.
We have described how to operate a generic amine unit that we believe to be typical of those in the industry. The reader may have to adjust the information presented here where his operation or amine unit is atypical. In preparing these practices we have used one set of terminology, recognizing that other terminology is used in the industry. Examples include: Regenerator – stripper, reactifier, tower, still, still tower Absorber – treater, contactor, scrubber Disclaimer It should be noted there is no operational guarantee implied with the data or procedures presented in this manual. They are intended to be used as guidelines against which to measure or evaluate specific amine unit operations.
Amine Best Practices Group
TABLE OF CONTENTS
Page PROCESS FLOW DIAGRAM Typical Amine System………………………………………… 3 EQUIPMENT 1. Feed Preparation…………………………….................... 4 2. Overhead KO Drum…………………………………….. 7 3. LPG-Amine Coalescer…………………………………... 8 4. Gas Absorber…………………………………………..... 9 5. LPG Contactor…………………………………………... 14 6. Rich Amine Flash Drum………………………………… 17 7. Rich Amine Pump………………………………………. 20 8. Lean-Rich Exchanger……………………….................... 21 9. Regenerator……………………………………………… 23 10. Regenerator Overhead Condenser……………………..... 29 11. Reflux Drum…………………………………………….. 30 12. Reflux Pump…………………………………………….. 31 13. Lean Amine Pump……………………………………..... 34 14. Lean Amine Coolers…………………………………….. 35 15. Regenerator Reboiler…………………………………..... 37 16. Amine Filter……………………………………………... 39 17. Amine Carbon Treater…………………………………... 42 18. Carbon Treater After Filter……………………………… 45 19. Amine Surge Tank…………………………..................... 46 20. DGA Reclaimer………………………………………..... 48 21. Amine Reclaimer………………………………………... 51 22. NH3 Scrubber………………………………..................... 53 SPECIAL ISSUES Amine Condition………………………………………............. 55 Caustic Neutralization…………………………………............ 60 Water Balance…………………………………………............. 61 Foaming……………………………………………………….. 62 Ammonia………………………………………………………. 63
Amine Best Practices Group
TYPICAL AMINE SYSTEM
TO FUEL OH CONDENSER OH KO DRUM 10 2 REGENERATOR LEAN/RICH EXCHANGERS GAS ABSORBER
NH3 SCRUBBER (OPTIONAL)
22 SOUR WATER
11 4 RAW GAS FEED PREP 1 15 FLASH GAS TO FUEL 6 7 LEAN AMINE PUMP 13 14 LEAN AMINE TRIM COOLERS 8 9
REFLUX DRUM 12
REFLUX PUMP REBOILER
RECLAIMER 20 21
RICH AMINE FLASH DRUM
CARBON TREATER AMINE AFTER FILTER FILTER 18 17 16
RICH AMINE PUMP
LPG-AMINE COALESCER WATER
AMINE SURGE TANK LPG
LPG CONTACTOR (ABSORBER)
Amine Best Practices Group
Clean or replace dirty element. It is difficult to size the apparatus for slug protection and the need is determined by an analysis of the upstream system considering the tendency of the source to carryover. acids ammonia or particulates.1. Liquid is bled to the sour water system. Coker. or Vacuum Unit that may contain cyanides. high liquid loadings Reduced throughput. at alarm or upset < 0. A pump may be added if significant carryover is expected. Amine Best Practices Group Page 4 05/23/07 . The goal of any of these alternatives is to prevent the introduction of hydrocarbons. The Inlet Knockout Drum functions to catch entrained hydrocarbon liquids and occasional slugs. open bypass Hydrocarbon contamination leading to foaming Filter material carried into amine equipment Confirm board and field instruments in agreement. A Filter-Separator is frequently used to remove liquids and solids from gas streams. Replace elements. HC contamination leading to foaming Drain liquid boot more frequently (manual drain). board. What about adding aerosol coalescing separation?? A water wash drum is a trayed column recommended for gas streams from an FCC. Continual rise Particle accumulation. FEED GAS PRETREATMENT For gas feeds. corrosion. filter-separators or a water wash drum or column. Filter Separator Pressure Drop • • • • Normal Range: Instrument: Status Check: Deviation: Cause: Consequence: Action: • Deviation: Cause: Consequence: Action: < 2 psi Differential pressure gages (field) Differential pressure transmitter/recorder/alarm (board) Field. Close bypass.1 psi reading Torn elements. A circulating water stream removes these contaminants. Check level instruments (auto drain). commonly applied apparatus includes knockout drums. Sour water stripper feed is commonly used as make-up because the ammonia is a good buffer and this minimizes refinery sour water. once/shift (round). Check for separation efficiency in upstream equipment. acids or other contaminants into the contactor to help prevent foaming. and other upsets.
or other level sensor / transmitter / readout / alarm Field. higher than normal liquid influx Hydrocarbon contamination of amine leading to foaming Control upstream upsets Increase manual drain frequency Check level control valve • Deviation: Cause: Consequence: Action: 05/23/07 Amine Best Practices Group Page 5 . level control failure (high) on upstream equipment. reduced throughput Control upset in upstream unit. 50% +/. torn element Hydrocarbon contamination of amine leading to foaming. d/p cell. manual drain valve leaks.25% (board or field level instrument) Gage glass. faulty level control/control valve. Clean or replace dirty element. liquid/solid fouling Blind-off leading to relief or compressor problems HC contamination of amine leading to foaming. FEED GAS PRETREATMENT .cont • Deviation: Cause: Consequence: Sudden increases Upstream upset. at alarm or upset No level ever shows Bypassing. start once/shift (round) Board.1. gas release to unprotected vessels or atmosphere Close bypass Check valves for leaks Replace element Gradual level increase Infrequent manual draining. float. Action: Liquid Levels • • • • Normal Range: Instrument: Status Check: Deviation: Cause: Consequence: Action: Level in gage glass (field). Drain liquid buildup.
high and low level alarms Every round and at alarm Low Water carryover. ammonia. control failure Breakthrough of contaminants to amine contactor (cyanides. particulates. check source of makeup water and restore High Excess makeup water. FEED GAS PRETREATMENT .cont Water Wash Drum Circulation Rate • • • • Normal Range: Instrument: Status Check: Deviation: Cause: Consequence: Action: 5 . check tower level Water Wash Drum Level • • • • Normal Range: Instrumentation: Status Check: Deviation: Cause: Consequence: Action: • Deviation: Cause: Consequence: Action: Design normal liquid level +/. loss of makeup water Loss of circulating water Check downstream KO pot for water. acids. restart or start spare.ft.1.5% Level gauge. increase purge rate 05/23/07 Amine Best Practices Group Page 6 . hydrocarbon carryover Loss of treating Check upstream source for problems. Flow controller On alarm at sign of upset Low Pump failure. loss of suction. organics) Check pump.10 gpm/sq.
Level • • Normal Range: Instrument: Empty to just visible Level gauge (sight glass) High level alarm in critical service Automatic level control valve in "wet" service Level to be visually checked on every round and vessel drained as needed. POTS An overhead knockout drum may be installed to pick up amine carryover. OVERHEAD K.O.hydrocarbon to a slops system Amine to the amine system Check operation of upstream equipment • Status check: • Deviation: Cause: Consequence: Action: 05/23/07 Amine Best Practices Group Page 7 . If foaming is expected. If alarm is provided.2. This requirement is a function of contactor design and the perceived likelihood of entrainment of foaming. in response to it High Upset in upstream equipment If not stopped. a water spray to collapse the foam may be appropriate. liquid will carry over and contaminate downstream processes Drain liquid .
but a coalescer-separator is generally recommended to recover chronically entrained droplets.3. in response to it High Upset in upstream contactor If not stopped. Recovery is further maximized by the upstream injection of recycle water which is typically limited to 5 wt-% amine. If alarm is provided. hydrocarbon will carry under and contaminate the regenerator Check drain valve • Status Check: • Deviation: Cause: Consequence: Action: • Deviation: Cause: Consequence: Action: 05/23/07 Amine Best Practices Group Page 8 . liquid will carry over and contaminate downstream processes Drain liquid to the amine system Check operation of upstream equipment Low Drain valve open or passing If not stopped. LPG-AMINE COALESCER With liquid hydrocarbon contactors. A simple knockout drum may be acceptable if the expectation is that the only significant carryover of amine will be as slugs. carryover of amine is a common occurrence. Level • • Normal Range: Instrument: Visible interface Level gauge (sight glass) High level alarm in critical service Automatic level control valve in "wet" service Level to be visually checked on every round and vessel drained as needed.
check feed gas for entrained HC’s Amine Best Practices Group Page 9 • • Status check: Deviation: Cause: Consequence: Action: • Deviation: Cause: Consequence: Action: • Deviation: Cause: Consequence: Action: 05/23/07 . contamination) Sudden increase. capacity limit Cleanout. Adequate separation space is required at the top and mist pads are frequently used. typically containing about 20 trays or equivalent. Differential Pressure • • Normal Range: Instrument: 0. poor efficiency. Tower material is steel. and is an absolute necessity for MEA systems.2 psi/tray Continuous recorder w/alarm. general plant upset Add antifoam (discriminately). identify root cause (e. flooding Poor efficiency. Design pressures of the contactor and associated KO pots normally match the gas source design pressure so that the contactor does not require overpressure relief capacity for full gas flow at blocked discharge.0. Note: By locating the lower d/p cell tap at roughly the same elevation as the top sight glass connection. check relative gas/amine temperatures to determine likelihood of HC condensation. reduce gas and/or liquid rates. it doubles as an independent high-level alarm. condensation may not be an issue and it may be preferable to minimize the lean amine temperature (to 80°F) in order to maximize fuel gas cleanup. However. to avoid foaming due to HC condensation where the gas is saturated. off-spec treated gas Mechanical repair Gradual increase Possible fouling Flooding. if the gas is not saturated or any heavy (C6+) HCs are not surface active. 316 or 410SS. erratic action Foaming.4. At alarm or sign of upset Consistently low Possible tray damage Poor efficiency.1 . Common industry practice is to maintain lean amine temperatures 10-15°F hotter than the raw gas feed to the absorber.g. corrosion. liquid carryover. Stress relieving (post weld heat treatment) is preferred for all amine vessels. GAS ABSORBER The Gas Absorber (or Contactor) is a typical counter flow gas-liquid contactor equipped with trays or with random or structured packing. off-spec treated gas. trays are typically 304.
supplement feed gas with recycle or clean gas if warranted High Upstream process change Increased amine demand.cont Feed Gas Flow Rate • • • • Normal range: Instrument: Status check: Deviation: Cause: Consequence: Action: • Deviation: Cause: Consequence: Action: Amine Flow Rate • • • • Normal range: Instrument: Status check: Deviation: Cause: Consequence: Action: • Deviation: Cause: Consequence: Action: 05/23/07 Site specific Continuous recorder At sign of upset or change in process conditions Low Upstream process change Reduced amine demand.4. possible jet flooding Increase amine flow As necessary to achieve on-spec treated gas within rich amine loading targets Controller w/alarm At alarm or sign of upset Low Change in controller status or supply pressure Potential reduction in acid gas recovery Adjust conditions determining rate High Change in controller status or supply pressure Increased utility consumption Adjust conditions determining rate Amine Best Practices Group Page 10 . GAS ABSORBER . potential reduction in mass transfer due to weeping Reduce amine flow.
4. with potential downstream condensation and resultant corrosion/fouling Increase lean amine cooling Amine Best Practices Group Page 11 Action: 05/23/07 . or increase amine flow rate to improve heat balance Lean Amine Temperature • • • • Normal range: Instrument: Status check: Deviation: Cause: Consequence: Action: • Deviation: Cause: Consequence: 90-130°F Indicator Once/round or at sign of upset Low Change in upstream process and/or ambient condition Potentially reduced acid gas removal from high viscosity or low rate of reaction Reduce lean amine cooling or supply heat High Change in upstream process and/or ambient conditions Potentially reduced acid gas removal due to poor equilibrium at high absorber temperatures Excessive moisture in treated gas. GAS ABSORBER .cont Feed Gas Temperature • • • • Normal range: Instrument: Status check: Deviation: Cause: Consequence: Action: • Deviation: Cause: Consequence: Action: 80-120°F Indicator Once/round or at sign of upset Low Change in upstream process and/or ambient conditions Reduced acid gas recovery in extreme cases Increase temperature of feed gas and/or amine High Change in upstream process and/or ambient conditions Potentially reduced acid gas recovery Decrease feed gas temperature.
GAS ABSORBER . Relative H2S loss is significantly increased by high contactor pressures. LPG entrainment and excessive (> 0. corrosion Increase amine circulation rate Amine Best Practices Group Page 12 Lean amine at least 10°F hotter than feed gas.4. Potential H2S release Site-specific.5) mole loadings. where gas is HCsaturated Indicators on individual streams Once/round or at sign of upset Low Change in upstream process and/or ambient conditions Condensation of HCs. potentially resulting in foaming and/or emulsification Increase lean amine temperature • • • Hazard: Status Check: Deviation: Cause: Consequence: Action: • Deviation: Cause: Consequence: Action: 05/23/07 . ranging from once/shift to weekly Low Overcirculation Excessive utility consumption Reduce amine circulation rate High Undercirculation Reduced acid gas removal.cont Lean Amine / Feed Gas Temperature Differential • • • • Normal range: Instrument: Status check: Deviation: Cause: Consequence: Action: Rich Amine Loading • • Normal range: Analysis: Caution: Maximum within target (see Appendix for typical rich amine loadings). contingent on satisfactory gas cleanup Spot lab sample Samples exposed to air or allowed to weather may not yield accurate results.
GAS ABSORBER . inadequate stripping. amine rate. temperature or quality Contractual/environmental non-compliance Adjust process conditions as warranted 05/23/07 Amine Best Practices Group Page 13 .4. foaming.cont H2S in Treated Gas • • • • • Normal range: Instrument: Analysis: Status check: Deviation: Cause: Consequence: Action: 10-50 ppm Optional online analyzer Length-of-stain tube Once/round or at sign of upset High One or more of following: flooding.
The flow of the discontinuous phase is from bottom to top and trays must be designed accordingly. configuration. LPG CONTACTOR The LPG Contactor (Absorber) is similar in most respects to the gas contactor with regard to materials. add antifoam Low Upstream flow rate changes None Lower lean amine rate • Instrument: • • Status check: Deviation: Cause: Consequence: Action: • Deviation: Cause: Consequence: Action: 05/23/07 Amine Best Practices Group Page 14 . The operating pressure/bubble point temperature relationship must be considered and it may be necessary for amine temperature to be below liquid hydrocarbon temperature to assure that localized vaporization of hydrocarbon does not occur. 2. These essential differences must be kept in mind: 1. Once/shift or upon upset or alarm High Upstream flow rate changes Process upset Sour product Emulsion formation at interface Amine carryover to downstream process Find cause of problem. Minimum recommended is flow rate indication. The rate is dependent on upstream devices such as level control or flow control from storage. Hydrocarbon Flow • Normal Range: Hydrocarbon flow direction is upward through the contactor. it is recommended that amine be the continuous phase. Recording instrumentation should be considered and provides indication of instability and upset conditions. Flow rate can vary from design rate down to 20-30% depending on refinery requirements.5. with the interface above the packing or trays. and design pressure considerations. There is a liquid-liquid interface to deal with. 3.
Once/shift or on alarm and indication of problems Low Improper set point Sour product Adjust amine flow to design rates High Improper set point Loss of interface control. Once/shift or on indication of problems High Improper amine cooling. flows are relatively low and may remain fixed without regard to economic considerations. LPG CONTACTOR – cont Amine Flow Rate • Normal Range: Amine flow rate should be adjusted at design flow rate and rich loadings. Some heat of reaction occurs and contributes to the temperature of the system.5. improper phase separation. Rates may be varied to match hydrocarbon loads if required. Normal temperature ranges from 100°F to 130°F. hydrocarbon feed temperature and rich amine temperature. amine carryover Adjust cooling to get amine to proper temperature Amine Best Practices Group Page 15 • • • Instrument: Status check: Deviation: Cause: Consequence: Action: 05/23/07 . Recording instrumentation should be considered. Minimum recommended is flow rate indication. upstream HC processing problems Sour product. amine losses Adjust amine flow to design rates • • • Instrument: Status check: Deviation: Cause: Consequence: Action: • Deviation: Cause: Consequence: Action: Temperature • Normal Range: Temperature is a function of the hydrocarbon temperature since it is normally the major flow component. Higher temperatures tend to break emulsions and assist interface control but hinder absorption and create bubble point problems. Normally. Bubble point of the hydrocarbon must be considered. Recommended lean amine temperature.
hydrocarbon undercarry or amine losses Look for upstream hydrocarbon or amine control problems. Operation near bubble point conditions must be avoided. pressure indication on hydrocarbon overhead Recorder recommended Once/shift or on upset Surges Hydrocarbon or amine control problem. loss of amine. LPG CONTACTOR – cont • Deviation: Cause: Consequence: Action: Low Improper amine cooling. loss of amine. sour product Bypass cooler to heat up amine Pressure • Normal Range: The minimum pressure is a function of the liquid hydrocarbon composition to be treated and the temperatures anticipated in the contactor. Consider level controllers resetting flow controllers. sour product. amine carryover Raise set point to recommended minimum Raise pressure set point or lower temperature • Instrument: • • Status check: Deviation: Cause: Consequence: Action: • Deviation: Cause: Consequence: Action: 05/23/07 Amine Best Practices Group Page 16 . partial vaporization of hydrocarbon.5. upstream HC processing problems Loss of interface control due to emulsions. Low Improper set point Loss of interface control. Recommended is RVP of the hydrocarbon plus 50 psi unless the operating temperature causes the vapor pressure at conditions to be much higher. feed composition change Loss of interface control. hydrocarbon flow may stop. Normal control is by a backpressure control system on the contactor overhead system. As a minimum.
as H2S levels are typically on the order of several %. although pressures as high as 90 psig . clean up amine.are not uncommon. Pressure • • • • Normal operating range: (1) High pressure (no rich amine pump): 45-65 psig (2) Low pressure (with rich amine pump): 0-25 psig Instrumentation: Status Check: Deviation: Cause: Consequence: Action: • Deviation: Cause: Consequence: Action: • Deviation: Cause: Consequence: Action: Pressure controller If amine foaming is observed High Excessive hydrocarbon in rich amine Regenerator foaming. add antifoam. At low pressure. Flash gas at less than fuel gas header pressure can be disposed of to the vapor recovery system. Level instrument design must consider the potential for accumulation of liquid HC layers of varying densities.6. skim hydrocarbon from flash drum Low System venting to atmosphere or relief system May not get into the regenerator Find leak Negative pressure Relief stack draft causing a vacuum on the system Air may be drawn into flash drum and contaminate the amine or cause an explosive mixture Adjust relief system pressure to hold positive pressure on drum 05/23/07 Amine Best Practices Group Page 17 . incinerator or heater firebox – usually subject to amine scrubbing. SRU upset or fouling Correct absorber operation. Materials are as for the Gas and LPG Contactors. flare. a rich amine pump is required. FLASH DRUM The Rich Amine Flash Drum provides for the venting of flashed light hydrocarbons and separation of liquid hydrocarbons ranging from LPG to gas oil. It is recommended that the flash drum be operated at a pressure of 15 psig or less. Stilling wells are required for liquid feed to avoid continual turbulent mixing of liquid hydrocarbon with amine.
low and high level alarms At or changing level High Water leaking into system. clean up amine. add antifoam. imbalance in amine flows Amine carryover into gas system. SRU upset Increase skim rate. absorbers returning amine inventory. Check amine strength.6. check gas and liquid absorber operation for hydrocarbon carryunder 05/23/07 Amine Best Practices Group Page 18 . foaming in regenerator (SRU upset) Correct absorber operation. skim hydrocarbon from flash drum Hydrocarbon Level • • • • Normal operating range: 0-5% level above amine Instrumentation: Status Check: Deviation: Cause: Consequence: Action: Amine Level • • • • Normal operating range: 40-75% when flash drum is system's surge capacity Instrumentation: Status Check: Deviation: Cause: Consequence: Action: Level recorder. Sight glass Once per round or regenerator foaming problems High Insufficient skimming Amine foaming. FLASH DRUM – cont Flash Gas Rate • • • • Normal operating range: Depends on absorber pressure and feed composition Instrumentation: Status Check: Deviation: Cause: Consequence: Action: Flow indicator and/or pressure controller At alarm or sign of upset High Hydrocarbon carryover from absorber Foaming and reduced acid gas absorption (possible violation). absorber level problem. diluting amine strength Remove some amine from plant.
6. Flash gas or liquid hydrocarbon carryover in rich amine to regenerator due to low residence time for gas or liquid hydrocarbon separation (SRU upset) Add amine or condensate to plant. absorber upset and holding up or losing amine. foaming in absorbers or regenerators. FLASH DRUM – cont • Deviation: Cause: Low Dehydrating amine system. or system losses. find leak or loss Consequence: Action: 05/23/07 Amine Best Practices Group Page 19 .
Mechanical seals are required of a quality to contain rich amine. required for low pressure flash drum operation may be to API or ANSI specifications.7. Pump materials include steel or stainless steel case and chrome or chrome-nickel stainless intervals. 05/23/07 Amine Best Practices Group Page 20 . Pump cases and seals must be designed for the relieving conditions of the flash drum. RICH AMINE PUMP The Rich Amine Pump(s). but must consider the following: 1. 2. a potentially toxic fluid. plus pump differential pressure.
the rich side pressure can be designed for Flash Drum design pressure plus Lean Amine Pump differential. a 10 degree change from “normal” value should be investigated Control-board mounted on final rich amine. at about ambient temperature. As with all equipment. tube sheets. temperature. Rich Outlet Temperature • • • • Normal Range: Instrument: Status Check: Deviation: Cause: Consequence: Action: • Deviation: Cause: Consequence: Action: Will vary with system design and current operation. 18-8 stainless tubes are recommended with stress relieved steel for the shell. Lean side design depends on location but should at least match Regenerator design pressure. For shell-and-tube units. exchanging Regenerator bottoms at reboiler temperature against rich amine feed to the Regenerator.8. Both shell-and-tube and plate-and-frame exchangers have been used. and channels. If the Rich Amine Flash Drum relief valve provides rich side protection. typical 5-10 psig Local pressure gauges Recorded as part of heat transfer monitoring or at capacity limitation 05/23/07 Amine Best Practices Group Page 21 . possibly bypass hot lean amine flows Low Exchanger fouling Poor stripping in regenerator and/or increased reboiler steam demand Check all temperatures for poor performance (fouling). LEAN/RICH EXCHANGERS The Lean-Rich Exchanger is a heat conservation device. clean exchangers Pressure • • • Normal Range: Instrument: Status Check: Design. to preheat the feed. local temperature indicators Once per round Heat transfer coefficients calculated monthly High rich amine temperature Low fuel rate Flashing and corrosion in exchangers and regenerator inlet piping Check amine flows. design pressures must consider actual maximum system pressure.
cont • Deviation: Cause: Consequence: High Fouling.8. LEAN/RICH EXCHANGERS . equipment failure Reduced circulation Reduced heat transfer High lean amine temperature and low regenerator feed preheat Locate the point of high pressure drop Action: 05/23/07 Amine Best Practices Group Page 22 .
install reflux purge and clean water makeup to control corrosion. hydrocarbon contamination Relief. REGENERATOR The Regenerator is usually a trayed tower. although packed towers are occasionally used. flooded vessel. at alarm or upset Low or decreasing pressure Failed pressure controller. Reflux Drum Pressure • • • • Normal Range: Instrument: Status Check: Deviation: Cause: Consequence: Action: 5-15 psig Pressure gage (field). loss of containment Upset of or shutdown of downstream sulfur unit. once/shift(round). Not all of this is true in the gas patch. Trays of 410SS or 18-8SS are used successfully. reduced heat input. decreased throughput. increased lean loadings. board. unit shutdown Determine cause for loss of feed or heating medium. loss of reboiler heat source. blocked outlet line. Capacity in the bottom may be provided for surge (common in tail gas treater systems) or surge may be external (preferred in primary systems). The feed nozzle is usually of 18-8SS or is lined with an 18-8 SS sleeve. failed pressure controller.9. transmitter/recorder alarm (board) Field. The tower shell is of steel (516-60 or 516-70) and is stress relieved. downstream unit shutdown or upset accelerate amine degradation Reduce feed Reduce reboiler duty Drain hydrocarbons from flash drum Raise reflux temperature Steam out liquid gas product Drain hydrocarbon liquid from reflux drum Shutdown and clean overhead line Amine Best Practices Group Page 23 • Deviation: Cause: Consequence: Action: 05/23/07 . excessive reboiler duty. unit shutdown. Minimize velocities by optimizing steam consumption High or rising pressure Downstream unit problems. Design pressure is based on system protection requirements and potential over pressure sources. Feed is below a rectifying section and above the stripping section. release to atmosphere. loss of feed.
unit shutdown. once/shift(round). foaming and excessive entrainment. meter/ transmitter/recorder/alarm (prefer to have flow control reset by upstream drum level) Field. transmitter/recorder/alarm (board) Field. reduced throughput Reduce feed Reduce reboiler duty Drain hydrocarbons from flash drum Steam overhead line Drain hydrocarbons from reflux drum Shutdown and clean overhead line Action: Rich Amine Feed Rate • • Normal Range: Instrument: System dependent Field. flow control failure. board. orifices filters. loss of cooling media Upset of downstream sulfur unit. local flow indicator/ controller. board. Amine Best Practices Group Page 24 • • Status Check: Deviation: Cause: Consequence: Action: 05/23/07 . at alarm or upset Sudden loss of flow Loss of flash drum or contactor levels. plugging from corrosion products or salts. relief. condenser fouled on the cooling media side. Check contactor level control and flows. board. at alarm or upset High or Rising Pressure Condenser fouled and plugged on the process side. high regenerator pressure Loss of throughput. loss of treating capability. SRU upset Check rich flash drum level control. increased lean loadings. acceleration of amine degradation. REGENERATOR – cont Top Pressure For Conventional Condenser/Drum Overhead Systems • • • • Normal Range: Instrument: Status Check: Deviation: Cause: Consequence: 5-15 psig (set primarily by downstream sulfur unit) Gage (field).9. once/shift(round). Check rich amine feed circuit for plugging in valves. or exchangers. check for hydrocarbons to regenerator. Remove heat stable salt anions and sodium Remove degradation products (reclaim).
Lean loadings vary from 0. equipment draining). board. at alarm or upset Sudden loss of flow Loss of feed. board. meter/transmitter/ recorder alarm (should coordinate into downstream sulfur unit control scheme) Field. loss of containment.9. plugged overhead line. pressure controller failure. downstream unit shutdown. tower internals malfunction Loss of throughput. loss of reboiler heat input. Steam out or otherwise heat overhead line. Check for maintenance activity (filter changes. Check for contactor foaming or upset. local flow indicator. REGENERATOR – cont • Deviation: Cause: Consequence: Action: Gradual decline in flow Declining rich amine flash drum level resetting flow. upset/shutdown of downstream sulfur unit Skim rich amine flash/reflux drums for hydrocarbon Change carbon filter • • Status Check: Deviation: Cause: Consequence: Action: • Deviation: Cause: Consequence: Action: Lean Loading • • Normal Range: Instrument: 05/23/07 Amine and acid gas dependent. foaming. leaks or open drains Loss of throughput. Acid Gas Product Rate • • Normal Range: Instrument: System dependent Field. raise reflux or pumparound return temperature. Balance reflux purges and makeup water rates. tower internals malfunction Amine carryover. unit shutdown Restore feed. relief.002 to 0. once/shift(round).1 mol acid gas/mol amine Laboratory test Amine Best Practices Group Page 25 . plugging from corrosion products or salts. loss of treating capability Balance flows in and out of system. loss of treating capability. Sudden increase in flow Hydrocarbon intrusion into regenerator. Restore reboiler heating media.
Special consideration: In H2S-containing systems.25% Field. residual H2S tends to oxidize to thiosulfate when exposed to air. board. REGENERATOR – cont • Status Check: Laboratory. Level-Trol or d/p cell with local indicator Board. over-circulation. excessive corrosion Increase reboiler heat input. loss of reboiler heat input Check controller. fouled lean/rich exchangers. d/p cell or float/transmitter/recorder/alarm Field. lean circulation pump failure/shutdown. Lean loading exceeds spec/treated gases and liquids fail to meet spec. Caution must be taken in sampling and sample handling. once/day to once/week. • Deviation: Cause: Consequence: Action: Bottom Level • • • • Normal Range: Instrument: Status Check: Deviation: Cause: Consequence: Field. Change carbon filter Action: 05/23/07 Amine Best Practices Group Page 26 . once/shift. loss of feed. Increase amine strength. Remove heat stable salt anions and sodium. Check for loss of feed.9. foaming Bottoms pump failure. gage glass. at alarm or upset Sudden loss of level Control failure. fouled reboiler. Insufficient reboiler heat input caused by: insufficient heating media supply. Skim flash drum and reflux drums for hydrocarbons. Check sodium level. in sight glass. loss of regenerator level Leaking lean/rich exchangers when rich amine exceeds lean amine pressure Caustic contamination Off-spec products. loss of circulation causing off-spec products. Clean fouled exchangers. Decrease circulation. Check for signs of hydrocarbon incursion. board 50% +/. rapid pressure-up.
Excessive particle accumulation caused by poor filtration. high heat stable salt anion content. at alarm or upset Little or no pressure drop Loss of feed. Reduce feed rate. loss of reboiler heating media. Skim rich amine flash drum and reflux drum for hydrocarbon. hydrocarbon intrusion from flash drum. Reduce heat input Gradual buildup or sudden permanent buildup Buildup of corrosion products causing tray plugging. damage. insufficient heat input leading to excessive lean loadings. tower internals malfunction Amine and/or hydrocarbon carryover into downstream sulfur unit. tray blowout. increased filter pore size to control filter replacement cost. high lean loadings leading to off-spec products. tray blowout Determine composition of reflux. add antifoam until pressure drop is normal. filter placement. d/p cell/transmitter/recorder/alarm Field. or flow. under-circulation leading to excessive rich loadings. once/shift(round). REGENERATOR – cont Tower Pressure Drop • • • • Normal Range: Instrument: Status Check: Deviation: Cause: Consequence: Action: • Deviation: Cause: 0. if high in hydrocarbon increase purge. reboiler heat input fluctuations.05-0. if high in amine stop purge of reflux to stop amine loss. Excessive corrosion rates caused by high ammonia/amine concentrations in reflux. change if necessary. Ensure proper levels are maintained in rich flash and reflux drum. Test feed and bottoms for foaming tendency. accumulation of particles in rich amine flash drum Amine Best Practices Group Page 27 Consequence: Action: • Deviation: Cause: 05/23/07 . board. Monitor carbon filter. unit shutdown downstream sulfur unit shutdown Determine reason for loss of feed Determine reason for loss of heating media Occasional sudden rise then returning to normal Foaming. tower internals malfunction High lean loadings leading to off-spec products.2 psi/tray d/p gage (field). check level instruments Check reboiler heating medium control for fluctuating pressure. temperature. hydrocarbon refluxed to tower.9.
Reduce circulation. Raise reflux or pumparound return temperatures. increase corrosion rates throughout regenerator. Reduce reboiler duty. excess energy costs. Re-establish condenser/pumparound cooler cooling media. increased energy consumption. reflux level or pumparound flow control valve failure. Amine Best Practices Group Page 28 Consequence: Action: • Deviation: Cause: Consequence: Action: 05/23/07 . keep rich loadings at or below recommended levels Action: Top Temperature For Conventional Condenser/Drum Overhead Systems Or Pumparound Type System Pumparound Draw Temperature • • • • Normal Range: Instrument: Status Check: Deviation: Cause: 190-230°F Field. board. increase amine in reflux water by entrainment and/or vaporization.9. REGENERATOR – cont Consequence: Reduced throughput. too cold reflux or pumparound return temperatures. Raise condenser cooling media temperature High Too high heat input. excessive rich loadings. temperature gage. high lean loadings leading to off-spec products. once/shift(round). accelerate amine degradation. too low loadings Overtax overhead system leading to excess water loss and poor downstream sulfur unit feed. board. higher corrosion rates. reduced circulation leading to higher rich loadings. at alarm or upset Low Insufficient heat input. increased filtration costs and increased plugging Discontinue antifoam additions and change carbon filters to prevent antifoam buildup and foaming episodes Remove heat stable salt anions and sodium Remove amine degradation products (reclaimer) Shutdown and chemical or water wash tower Reduce filter pore size. thermocouple/transmitter/recorder/alarm Field. tower internals malfunction Increased lean loadings leading to off-spec products Raise reboiler heat input. loss of reflux or pumparound cooling media. Clean rich amine flash drum bottom Add additional filtration upstream of regenerator Keep lean loadings minimal.
REGENERATOR OH CONDENSER The Overhead Condenser may be either shell-and-tube or an aerial cooler. but usual steel construction is preferred.10. 05/23/07 Amine Best Practices Group Page 29 . A single pass exchanger with water on the tube side is usually selected for shell-and-tube. Amine side design pressure should match the Regenerator and the Condenser is typically protected by the Regenerator safety valve. Tube materials have frequently been dictated by water quality.
once/shift(round). board. Acid Gas Product/Reflux Temperature • • • • Normal Range: Instrument: Status Check: Deviation: Cause: 90-130° F Field. at alarm or upset Temperature reads below 90°F Too much cooling media. too cold cooling media. It is designed for pressure such that it can be protected by the Regenerator safety relief valve. Confirm instrument readings Cut cooling media rate or raise its temperature Raise reboiler heat input Consequence: Action: 05/23/07 Amine Best Practices Group Page 30 . REFLUX DRUM The Reflux Drum collects condensate from the Overhead Condenser and allows acid gas to separate and flow to the SRU. reflux level control problem. insufficient heat input. The Reflux Drum is carbon steel. and does not require stress relieving. temperature gage. It is sized to provide for vapor-liquid separation and for 5 minutes of Reflux Pump capacity holdup. pumparound temperature control problem Plugged overhead line with hydrates or NH3. board thermocouple/ transmitter/recorder/alarm Field.11.
loss of cooling media. excessive water to downstream sulfur unit. plugging. leaks. insufficient reboiler heat input. Mechanical seals must contain hazardous materials. Reflux ratio varies from 1 to 3 moles of reflux water to mole acid gas product. Reflux Rate • • Normal range: Instrument: Dependent on tower heat balance. plugging. loss of reboiler heating media. Controllers can be field or board mounted.12. Check/repair controller Raise reboiler heat input Clear plugging in reflux system • • Status Check: Deviation: Cause: Consequence: Action: • Deviation: Cause: Consequence: Action: 05/23/07 Amine Best Practices Group Page 31 . upset of air to acid gas ratio in Claus unit Check controller. Reflux rate controlled by reflux drum level in a conventional system. once/shift(round). REFLUX PUMP The Reflux Pump is a small ANSI or API pump. Casing pressure is designed for Regenerator pressure plus pump differential. pump problems High lean loadings leading to off-spec product. loss of levels reducing circulation and throughput. fouled or plugged overhead exchanger. Materials are steel with 400 or 300 series stainless steel impeller and internals or 300 series stainless steel case and internals. correct supply problem Determine if cooling media lost or restricted Reflux ratio too low Controller problems. insure correct valve trim and metallurgy Determine if feed lost. Field. board. at alarm or upset Loss of reflux Control failure. loss of feed. liquid carryover to downstream sulfur units. pump failure Increased amine strength leading to heat/mass transfer problems or pumping problems. correct upstream unit Determine if heating media lost.
Flowrate is also dependent on draw temperature. too large purge rates. increase in pressure which raises temperatures which accelerates corrosion. shutdown and repair condenser. too low tower top temperature setting.12. condenser leak Erratic amine strengths. leaking draw tray. plugged overhead lines Compute water balance and adjust purge/makeup rates Raise tower top temperature Analyze chloride level of amine. Flow Control reset by tower top temperature. REFLUX PUMP – cont Pumparound Rate (Special/Option) • Normal Range: Dependent on tower heat balance. Internal reflux ratios similar to the external reflux ratio for conventional overhead systems are maintained. loss of cooling media. Flowrate is normally reset by tower overhead temperature. board. draw tray level indicator/controller. low/high level/flow/ temperature alarms Field. • Instrument: • • Status Check: Deviation: Cause: Consequence: Action: • Deviation: Cause: Consequence: Action: 05/23/07 Amine Best Practices Group Page 32 . insufficient makeup water. increase in rich loadings. makeup water and purge water controls board or field mounted. erratic amine strengths Increase heat input to reboiler Increase lean circulation Restore cooling media flow Compute water balance and adjust purge/makeup Clean pumparound cooler Increase in pumparound flow Improper water balance. once/shift(round). coolant side of exchanger fouled Excess water to downstream sulfur unit. at alarm or upset Decline or loss of pumparound flow Loss or decline in heat input.
high ammonia levels in unwashed gases Accelerated overhead system corrosion. conductometric titration Once/week to Once/month depending on system Ammonia exceeds 1. overhead line plugging. reflux of H2S back to the stripping section of the regenerator. REFLUX PUMP – cont Ammonia Buildup • • • • Normal Range: Analytical Method: Status Check: Deviation: Cause: 0-1. excessive ammonia to SRU not designed for ammonia destruction Purge reflux/pumparound Consequence: Action: 05/23/07 Amine Best Practices Group Page 33 . high lean loadings leading to off-spec product. water wash systems upstream of contactors not operating or saturated.0 wt% Ion chromatography (IC).12.0 wt-% Low or no purge.
Pump materials include steel or stainless steel case and chrome or chrome-nickel stainless internals. in others they are lower pressure and supply booster pumps at individual Absorbers. 2. In some systems. pumps may be ANSI or API and must consider: 1. Accordingly. LEAN AMINE PUMP Lean Amine Pumps are usually downstream of the Lean-Rich Exchanger to keep NPSH requirements low. 05/23/07 Amine Best Practices Group Page 34 . Mechanical seals.13. these are high pressure pumps. Pressure protection level that defines casing rating.
stress relieving should be considered for all amines. Some refiners have used plate-and-frame exchangers if pressures are not excessive. usually designed as a single pass with amine on the tube side.14. In general. Temperature considerations as mentioned for the contactors may dictate lean amine cooler design or it may be dictated by coolant conditions. loss of cooling water Reduced H2S removal efficiency in downstream contactors. The recommended material in contact with the amine solution is steel. calculate heat transfer coefficients and clean exchangers. exchanger fouling. rapid loss of cooling may be an indication of mechanical problems. check cooling water supply. control board mounted on final lean amine temperature Lean amine temperature checked once per round or at alarm or upset. Outlet Temperature • • • Normal Range: Instrument: Status Check: 90-130°F (minimum 10°F hotter than sour fuel gas) Local temperature gauges. Low Cooler bypass closed. loss of heat to regenerator Condensation of hydrocarbons in absorbers Open cooler bypass Check regenerator bottoms temperature for deviation • Deviation: Cause: Consequence: Action: • Deviation: Cause: Consequence: Action: 05/23/07 Amine Best Practices Group Page 35 . Hydrocarbon vaporization in liquid/liquid contactors Close cooler bypass. Welded elements in contact with the amine must be stress relieved for MEA service. All other temperatures are checked weekly Heat transfer coefficients should be calculated monthly High Cooler bypass open. cooler amine (down to 80ºF) assures better performance. an aerial cooler or a combination. LEAN AMINE COOLERS The Lean Amine Cooler may be a shell-and-tube exchanger.
LEAN AMINE COOLERS – cont Pressure • • • • Normal Range: Instrument: Status Check: Deviation: Cause: Consequence: Action: Design. or at capacity limitation High Fouling.14. equipment failure Reduced circulation or high lean amine temperature leading to off-spec product. reduced heat transfer Locate the point of high pressure drop 05/23/07 Amine Best Practices Group Page 36 . 5-10 psig typical Local pressure gauges Recorded as part of heat transfer monitoring.
d. Steam is normally used as heat medium. once/(round). temperature gages. board. but tube wall temperature must be kept below some maximum for each amine. heat stable salt content. steam is on the tube side.15. Design pressure on the amine side must at least match the Regenerator. f. tray loadings. loss of containment High lean loadings leading to off-spec product. amine is on the tube side. Once through kettle. b. Once through vertical shell-and-tube. d. amine type and concentration) Field. Horizontal thermosiphon. steam side design is fixed by the steam system. emission of toxic gases to atmosphere Confirm initial and final state and flows of heating media and calculate duty to exchanger. REBOILER The Regenerator Reboiler may be: a. Tubes are usually of 316 SS although steel tubes are used successfully in some units. Vertical thermosiphon For a. Isolate leak. failure of reflux/ pumparound control leading to overcooling. For c and f. thermocouple/transmitter/ recorder/alarm Field. c. e. there are alternatives. fouling of reboiler or lean/rich exchangers due to excessive corrosion rates. Compute reboiler and lean/rich exchanger heat transfer coefficients to determine fouling. and e. Remove heat stable salts and anions. at alarm or upset Low Loss of reboiler heating media. Steel shells must be stress relieved. Conventional kettle. board. Reboiler Temperatures (In/Out) • • • • Normal Range: Instrument: Status Check: Deviation: Cause: 230-260° F (dependent upon tower pressure. Once through horizontal shell-and-tube. Clean exchangers if fouled. Compute required heat requirement and compare to available heat. b. Remove amine degradation products (reclaim) Consequence: Action: 05/23/07 Amine Best Practices Group Page 37 . Compute tower heat balance.
alarm Field. hydrocarbon incursion causing higher pressures. improper circulation of amine through reboiler. Dependent on amine type. Clean reboiler and/or lean/rich exchangers Consequence: Action: Reboiler Heat Input • Normal Range: 540-1350 BTU/gal amine solution (0. field or board mounted. REBOILER – cont • Deviation: Cause: High Tower overhead or acid gas product line plugged or pressure control problem. once/shift. stripping trays available. acceleration of amine degradation Clear overhead line pressure restrictions Confirm temperature and pressure of heating media. ratio of H2S to CO2 in rich. 50 psig stm). corrosion damage leading to reboiler failure. rich loading. strength. condensate system bottleneck Loss of treating capability. too high heat input.5 lb stm/gal amine. loss of supply. ammonia and amine concentration in the reflux. improper design of reboiler. decreased throughput. lean loading requirements. board.15.65-1. too hot heating media. and overhead pressure Flow controller with indicator/recorder. high heat stable salt anion and sodium content. adjust as needed Skim rich flash drum/reflux drum for hydrocarbons Decrease reboiler heat input Remove heat stable salt anions and sodium Remove amine degradation products (reclaim) Evaluate heat transfer equipment for coefficient and hydraulics. at alarm or upset Loss of heating media flow Controller failure. high amine degradation product levels Increased corrosion rates leading to filter plugging and equipment fouling and plugging. off-spec product Restore supply of heating media Lower condensate system pressure • • • Instrument: Status Check: Deviation: Cause: Consequences: Action: 05/23/07 Amine Best Practices Group Page 38 . heat to feed ratio controller.
Pressure Drop • • • • Normal Range: Instrument: Status Check: Deviation: Cause: Consequence: Design start of run up to design change pressure drop d/p gauge and/or pressure gauges Once per round Low Low flow. and designed to match the pressure of the absorbers or lean amine pump discharge conditions. Check piping for filter line-up Block-in filter and inspect media and internals (exact response filter media dependent) High Buildup of contaminants on filter media or failure of filter media Reduced filtration rate. In some systems. bag. failure of filter media or internals Contaminant buildup in the amine will lead to foaming.16. look for root cause of corrosion Action: • Deviation: Cause: Consequence: Action: 05/23/07 Amine Best Practices Group Page 39 . poor H2S removal and corrosion. sand. A 25% slipstream is the recommended minimum. Most systems apply lean slipstream cartridge or bag filters. stress relieved as for other steel elements. AMINE FILTER An amine filter is always required. precoat. etc. 20 micron is a reasonable maximum and 5 micron a reasonable minimum for filter element porosity. on the lean or the rich side of the system and may be cartridge. Filter cases are of steel. It may be full flow or slip stream. rich amine filtration is recommended. leading to foaming and fouling Change filter media. and special care must be taken to assure that elements can be removed safely. Filter media can migrate to other parts of the unit causing pressure drop and poor performance.
bypassed or damaged Foaming Equipment fouling Equipment failure (corrosion) Check filter pressure drop. if dirty charge media Verify/increase rate to filter Check amine at each contactor Test amine for corrosivity Consequence: Action: Length Of Run • • • • Normal Range: Instrument: Status Check: Deviation: Cause: Consequence: Action: Site specific Log of filter changes When an unusual pattern develops Short period between changes Increased contamination or corrosion. particulate) Reduced rate to particulate filter Contamination of amine (dirty fuel gas) Corrosion Filter media spent. AMINE FILTER – cont Amine Appearance • • • • Normal Range: Analysis: Status Check: Deviation: Cause: Clear (Pencil can be read across a pint jar) Visual inspection Once per shift Fail visual test (cloudy. or process upset Increased costs Check absorbers for unstable operation Check flash drum for excessive hydrocarbons Test amine for corrosivity Test amine for contaminants 05/23/07 Amine Best Practices Group Page 40 .16. inspect if low Check filter outlet sample. change if high.
16. AMINE FILTER – cont Flow Rate • • • • Normal: Instrument: Status Check: Deviation: Cause: Consequence: Action: Design rate Flow controller Monitor each round Low High filter pressure drop Filter bypassed Contaminated amine Verify filter line-up Change filter at high d/p 05/23/07 Amine Best Practices Group Page 41 .
it must be immediately downstream of the lean Amine Filter. Action: • Deviation: Cause: Consequence: Action: Note: 05/23/07 Amine Best Practices Group Page 42 . other testing may indicate end of useful life prior to pressure drop. Pressure Drop • • • • Normal Range: Instrumentation: Status Check: Deviation: Cause: Consequence: Design start of run up to design change delta pressure Delta pressure gauge and/or pressure gauges This is monitored each day Pressure drop low Filter is being bypassed Failure of internals Contaminant buildup in the amine will lead to foaming Poor H2S removal and corrosion Carbon filter media can migrate to other parts of the unit causing pressure drop and poor performance Check piping for filter line-up Block-in filter and inspect media and internals High Buildup of contaminants on carbon Pressure drop will back out flow resulting in less treating Block in and change carbon Pressure drop is not a good indicator of spent carbon. In general. CARBON TREATER The Amine Carbon Treater is optional and may be rich or lean. in general. It will. but not dissolved acids or salts. to be sure it does not become clogged with particulates. slipstream of full flow. enhance amine quality and system performance. A 10-20% slipstream is usually sufficient. or a dedicated filter. Steel construction with appropriate stress relieving is satisfactory. The Amine Carbon Treater will remove entrained hydrocarbons.17.
17. flash drums Test amine for contaminants 05/23/07 Amine Best Practices Group Page 43 . CARBON TREATER .reduce Check contactors for hydrocarbon source Check rich amine flash drum Check particulate filter delta p Consequence: Action: Carbon Usage • • • • Normal: Instrument: Status Check: Deviation: Cause: Action: Site specific Record of carbon addition When an unusual pattern develops Increased consumption Increased contamination Check contactors. foam test Visually checked each shift. particularly organic Excess antifoam Carbon bed is exhausted Reduced rate to carbon filters Foaming in regenerator and contactors Fouling of equipment Foam test carbon bed in and out Fail replace carbon Pass verify/increase rate to carbon filter Check antifoam addition rate high . foam test weekly (simple hand shake of the sample will give some indication) Fail visual foam test Run a formal foam test Failure of foam test Amine contamination.cont Filter Outlet Amine Condition • • • • Normal Range: Analysis: Status Check: Deviation: Action: • Deviation: Cause: Outlet sample less foaming tendency than inlet sample Visual check.
CARBON TREATER – cont Flow Rate • • • • Normal: Instrument: Status Check: Deviation: Cause: Consequence: Action: Design rate Local flow meter Monitored each round Low High filter pressure drop. filter bypassed Contaminated amine Verify filter line-up Change carbon at high pressure drop 05/23/07 Amine Best Practices Group Page 44 .17.
18. the Carbon Treater After Filter is a relatively course particulate filter to stop any carbon particles which break through. 05/23/07 Amine Best Practices Group Page 45 . in particularly. or. to prevent spread of carbon throughout the unit on failure of the carbon support structure. CARBON TREATER AFTER FILTER Recommended following the carbon treater. Materials and design pressure are as for other filters.
usually a vent to an incinerator or heater firebox is acceptable. Level – Routine Gauging • • • • Normal Range: Instrumentation: Status Check: Deviation: Cause: Consequence: Action: • Deviation: Cause: Consequence: Action: 20-80% Field level indicator Once per day or following transfer Loss of level High amine losses Increased operating cost Check for leaks. It may also be a pressure vessel. carryover from contactor or regenerator overhead Gain of level Possible amine dilution due to water leak Possible tank overflow Check amine strength – if low. Great care must be taken in venting such tanks. 05/23/07 Amine Best Practices Group Page 46 .19. look for water cooler leak or excessive water makeup. The tank may need steam coils or circulation means to assure that the solution viscosity does not increase in cold weather. an Amine Surge Tank is required. AMINE SURGE TANK In primary amine systems. It is usually an API tank with fuel gas or nitrogen blanket.
AMINE SURGE TANK . foaming. causing increased generation of heat stable salts and degradation of amine Adjust set point or check pressure controller 05/23/07 Amine Best Practices Group Page 47 .cont Blanketing – Pressure • • • • Normal Range: Instrumentation: Status Check: Deviation: Cause: Consequence: Action: • Deviation: Cause: Consequence Action: 1-2 inches of water Split-range pressure controller on inert gas makeup with flow indicator Operator check of setting High Set point adjustment incorrect or malfunctioning controller. check for hydrocarbon carryover from flash drum or absorber Low Set point adjustment incorrect or malfunctioning controller Air contamination of amine. light hydrocarbons in lean amine High usage of inert gas.19. SRU upset Adjust set point or check pressure controller.
20. DGA RECLAIMER
On primary amines (MEA, DGA) a Reclaimer is recommended to remove heat stable salts (HSS) and degradation products. It is usually a kettle with 316 SS tubes and provision for easy addition of caustic or soda ash. Reclaimers frequently contain spargers to pass steam directly through the residue sludge to assist in reacting caustic or soda ash. Steel shells must be stress relieved. Steam supply must be hot enough to vaporize the amine and is usually in the 150-250 psig range.
FEED RATE • • • • Normal range: Instrument: Status check: Deviation: Cause: Consequence: Action: • Deviation: Cause: Consequence: Action: Water Rate • • • • Normal range: Instrument: Status check: Deviation: Cause: Consequence: Action: As necessary to maintain desired temperature Controller Once/round or at sign of upset Low Controller malfunction High temperature (due to over concentration of amine) Adjust rate As necessary to maintain level (1-3% of Regenator feed) Optional indicator/recorder Once/round or at sign of upset Low Low demand due to low vaporization rate caused by fouling or high process temperature Low reclaiming rate Clean reclaimer or dilute amine High Instrument malfunction resulting in liquid carryover Low temperature, inadequate reclaiming Adjust conditions as necessary to maintain proper level
Amine Best Practices Group
20. DGA RECLAIMER – cont • Deviation: Cause: Consequence: Action: Steam Rate • • • • Normal range: Instrument: Status check: Deviation: Cause: Consequence: Action: • Deviation: Cause: Consequence: Action: Temperature • • • Normal range: Instrument: Deviation: Cause: Consequence: Action: • Deviation: Cause: Consequence: Action: 360-380°F Continuous recorder/controller Low Low amine concentration Low reclaiming rate Increase steam rate High High amine concentration Low heat transfer rate, low reclaiming rate, degradation Dilute the inventory by adding condensate to the reclaimer Site specific Continuous recorder Once/round or at sign of upset Low Reduced heat transfer rate due to fouling or high process temperature Low reclaiming rate Clean reclaimer or dilute amine High Low process temperature due to dilute amine Low reclaiming rate Increase amine concentration by dehydration High Controller malfunction Low temperature (due to dilution) Adjust rate
Amine Best Practices Group
20. DGA RECLAIMER – cont
Level • • • • Normal range: Instrument: Status check: Deviation: Cause: Consequence: Action: • Deviation: Cause: Consequence: Action: 40-60% DGA flow controller Once/shift or at sign of upset Low Instrument malfunction Low reclaiming rate Adjust feed rate High Instrument malfunction Potential liquid carryover with salt entrainment Reduce feed rate
NaOH Addition • • • • Normal range: Analysis: Status check: Deviation: Consequence: Action: • Deviation: Consequence: Action: Stoichiometric equivalent of heat stable salts Spot lab sample Weekly Below normal Potential corrosion, incomplete amine recovery Adjust addition rate as appropriate Above normal Potential caustic embrittlement Adjust addition rate as appropriate
Amine Best Practices Group
then reduce slightly. Displacer level controller. Increase steam flow until bumping or violent boiling is heard. Decrease steam flow until bumping or violent boiling is no longer heard. usually local Once per shift. carryover of salts into regenerator. gauge glass on reclaimer. High Improper setting. Bumping. adding caustic or soda ash.21. extended reclaiming run. They work by converting the amine salts to sodium salts. and boiling the amine away from the resulting salt solution. or controller malfunction. Low Improper setting. Feed Rate • • • Normal Range: Instrument: Status Check: Controlled to maintain level in reclaimer. Low boil up. The sludge in the reclaimer is dumped and the cycle can be repeated. while making up with lean MEA to hold levels. inability to clean up MEA. This continues until the temperature of the slowly concentrating salt solution in the reclaimer nears the thermal degradation temperature of the MEA. Steam Rate • • • • Normal Range: Instrument: Status Check: Deviation: Cause: Consequence: Action: • Deviation: Cause: Consequence: Action: Varies with size and design of unit. Set to provide reasonable boil up rate. without excessive bumping or carryover to regenerator. or controller malfunction. Sometimes live steam is injected into the reclaimer at the end of the run to strip out any remaining MEA. A batch consists of the following steps: filling the reclaimer with amine. Flow controller. adding steam to the bundle to boil off the water and volatile MEA. AMINE RECLAIMER Reclaimers are installed in MEA units to permit cleaning up amine contaminated with heat stable salts. Once per shift 05/23/07 Amine Best Practices Group Page 51 .
Thermal degradation of MEA. many have recorder.21. stop steam flow. slowly increasing during run as salt concentration in reclaimer increases.cont • Deviation: Cause: Consequence: Action: High level Improper set point or controller malfunction. AMINE RECLAIMER . poor amine quality. Re-adjust level. possible corrosion. Low level Improper set point or controller malfunction. Carryover of salts into regenerator. Low temperature Inadequate steam flow or pressure (below about 35 psig) or excessive amine flow. or. Slow or no reclaiming. pressure is problem reduce it as appropriate. Exposed tubes may cause thermal degradation of amine on hot tube surface. Re-adjust level. if steam. Every four hours. If temperature fails to increase during the run it may indicate carryover of salts to the regenerator. Local indicator. inability to clean up MEA. High temperature High steam pressure (above about 90 psig) or salt concentration in reclaimer too high. end of run is when 300°F temperature is reached. • Deviation: Cause: Consequence: Action: Temperature • • • • Normal Range: Instrument: Status Check: Deviation: Cause: 260-300°F. Increase steam rate or pressure. End the batch run. Reducing steam rate may help reduce carryover. Consequence: Action: • Deviation: Cause: Consequence: Action: 05/23/07 Amine Best Practices Group Page 52 . Inspect/replace demister and check level to reduce carryover.
NH3 SCRUBBER Acid gasses bearing excessive amounts of ammonia require special consideration to prevent line blockage and associated sulfur plant problems. Water wash systems to remove ammonia prior to feeding sulfur plant is common for these conditions. NH4HS corrosion Increase makeup rate Low Too high water makeup rate High operating cost Decrease makeup rate 05/23/07 Amine Best Practices Group Page 53 .22. Ammonia is removed with water purged from this unit and routed to the sour water stripper. Circulating Water Rate • • • • Normal Range: Instrumentation: Status Check: Deviation: Cause: Consequence: Action: 5-10 GPM/ft2 Flow controller with low flow alarm At alarm Low Possible plugging in scrubber Inadequate NH3 removal – SRU upset Cleanout NH3 Concentration Of Water • • • Normal Range: Instrumentation: Deviation: Cause: Consequence: Action: • Deviation: Cause: Consequence: Action: 0-1 wt% NH3 (high liquid velocities in your system may require lower NH3 concentration in order to keep corrosion rates down) Sample and lab analysis High Too low water makeup rate Inadequate NH3 removal resulting in SRU fouling.
22. due to low ambient temperatures and long runs of acid gas lines Decrease water makeup rate or cut back coolant rate 05/23/07 Amine Best Practices Group Page 54 . temperature indicator Once per round or at alarm High Increased NH3 to scrubber or not enough cooling Increased NH3 to SRU (plugging). increased water to SRU (lower efficiency) Increase water makeup or coolant rate Low Too much cooling Possible plugging of acid gas line from hydrate. NH3 SCRUBBER – cont Temperature • • • • Normal Range: Instrumentation: Status Check: Deviation: Cause: Consequence: Action: • Deviation: Cause: Consequence: Action: 80-120°F Temperature controller on circulating water cooler.
accumulation of heat stable salt anions. selectivity requirements. Change carbon filter if sample shows hydrocarbon layer or if cloudy. • Analysis Method: • • Status Check: Deviation: Cause: Consequence: Action: 05/23/07 Amine Best Practices Group Page 55 . automatic acid titration with potentiometric or conductometric readout (Caution: amines containing high amounts of sodium or organic acid anions will interfere with pH and color indicator titrations. laboratory error Loss of capacity. leaks. adjust water makeup Check for hydrocarbon incursion. Amine Strength. corrosion rate acceleration Run duplicate to verify lab work Check system water balance and make-up requirements. cost to replace lost inventory. Remove heat stable salt anions. or upset Low Dilution from excess make-up water. Ensure proper temperature for lean amine to each contactor. Amine should be near color free and void of particulate matter. Organic acid anions will titrate similarly to amines because they behave as weak bases at the endpoint of the amine titrations. waste water emissions violations. acid gases removed. treating requirements. sodium accumulation.Amine Condition Condition and proper care of the solvent is as important to successful operations as equipment maintenance and performance. and corrosion control parameters Acid titration using pH meter or color indicator. Check for foaming in individual contactors and regenerators and add antifoam only as needed. heat stable salt anion accumulation.) Once/shift to once/week depending on water balance. reduced throughput. Active Amine • Normal Range: Dependent on amine type. upset or routine losses. Skim rich flash drum/reflux drum for hydrocarbons.
aggravation of foaming. freeze up. reduction of heat and mass transfer capabilities. adjust water make-up. high organic acid anion content Loss of levels/level alarms. loss of capacity. declining flow to regenerator. high reboiler temperatures and amine decomposition Run duplicate sample to verify lab work.Amine Condition – cont • Deviation: Cause: Consequence: High Lack of make-up water. over addition. heat stable salt anion accumulation caused by contaminants in streams being treated Corrosion rate acceleration. additional filter costs. Adjust addition procedures Action: Amine Strength. Remove heat stable salt anions (“reclaim”). use conductometric titration method. • • Status Check: Deviation: Cause: Consequence: Action: 05/23/07 Amine Best Practices Group Page 56 . automatic titration using potentiometric or conductometric method (Caution: errors in the titration will occur as the lean loading of the sample increases) Once/week to once/shift depending on heat stable salt anion accumulation Inactive amine exceeds 10 % of total amine concentration Insufficient heat input into regenerator causing high lean loadings. pumping problems. Check system water balance and make-up requirements. Purge contaminated amine and makeup with fresh. (Caution: This guideline is only correct if no sodium is present. loss of containment. exchanger fouling. unit shutdown Water wash streams to be treated. equipment failure. plugging. Inactive Amine • • Normal Range: Analysis Method: 0-10 % of the active amine concentration.) Base titration using pH or color indicator. laboratory error.
8 wt % of solution Ion Chromatography Once/two weeks to once/month dependent on accumulation Heat stable salt anions exceed 0.g. formic acid. IC Once/two weeks to once/quarter dependent on accumulation of heat stable salt anions and metal contamination • Analytical Method: • Status Check: 05/23/07 Amine Best Practices Group Page 57 . Ion Chromatography (IC). Inductively Coupled Plasma (ICP). Metals Including Sodium • Normal Range: Sodium 0-0. oxalic acid). acetic acid. chlorides. Heat Stable Salt Anions • • • • Normal Range: Analysis Method: Status Check: Deviation: Cause: 0-0. HCN. HCl. all others below 100 ppm (except in metal passivation additive systems).8 wt% Contaminants in treated streams (e. phosphates.Amine Condition – cont Amine Quality. Sodium. SO2. Dissolved iron above 25 ppmw may be indicative of excessive corrosion. sulfates. nitrates) See inactive amine strength high deviation section Water wash streams to be treated Remove heat stable salt anions Reclaim Purge contaminated amine and make up with fresh Consequence: Action: Amine Quality.2 wt-%.g. O2. ICP. Atomic Absorption(AA). Iron and others. contaminants in the make-up water (e. Ion Selective Electrode(ISE).
silver nitrate titration (inaccurate due to silver-amine complexes) Once/two weeks to once/month dependent on accumulation • Monitoring Frequency: 05/23/07 Amine Best Practices Group Page 58 . high velocity. corrosion rate acceleration Remove heat stable salt anions and sodium Consequence: Action: • Deviation: Cause: Consequence: Action: Amine Quality. high heat stable salt anion content. Chlorides • • Normal Range: Analytical Methods: 0-1000 ppmw Ion chromatography (Caution: some IC anion methods will not distinguish formates from chlorides). and high H2S and/or CO2 concentrations See Inactive amine strength high deviation section Lower lean loadings by increasing reboiler heat input Reduce rich loadings by increasing circulation or amine strength Lower reboiler input to reduce velocity in reboiler piping and in overhead system Lower circulation to decrease rich amine velocities Purge ammonia from the regenerator reflux Remove heat stable salt anions and sodium Reduce pressure to lower regenerator temperatures Reduce lean amine temperatures to reduce corrosion in contactor bottoms Reclaim Purge contaminated amine and make up with fresh Charge equivalents of metals exceeds charge equivalents of heat stable salt anions Over-neutralization during caustic or soda ash addition High lean loadings leading to off-spec products.Amine Condition – cont • Deviation: Cause: Iron exceeds 25 ppmw Corrosion rate acceleration caused by high temperature.
DEA Formamide • • • • Normal Range: Analytical Methods: Status Check: Deviation: Unknown NMR. Suspended Solids • • • • Normal Range: Analysis Method: Status Check: Deviation: 0-100 ppmw. weight of filtered solids Visual check once/shift or day Solution is green or green with black particles. heat stable salt anions. reduced throughput. temperatures. poor quality make-up water Chloride stress cracking. The formation of the formamide takes up amine capacity by reacting the amine. solution is white to yellow with large black particles Break-up of carbon in carbon filter entering amine corrosion Plugging. pitting on reboiler tubes Remove heat stable salt anions Amine Quality. particles settle out after standing for long periods of time. and velocities Cause: Consequence: Action: Amine Quality. filtration. 05/23/07 Amine Best Practices Group Page 59 .Amine Condition – cont • Deviation: Cause: Consequence: Action: Chloride level exceeds 1000 ppmw HCl from reformer hydrogen or crude gases. cooling water leak. The only way known to break up the formamide is a catalytic process developed by Mobil Oil. go to smaller filter pore size Reduce corrosion rates by reducing acid gas concentrations. foaming Use correct carbon filter loading procedures. Use harder carbon. solution clear water-white to yellow to green Visual inspection. IR. Change particle filters. is turbid. The formate can be removed by heat stable salt anion removal techniques. GC-Mass Spec Not established None known The formamide comes from reaction of formate heat stable salt anions and the DEA.
on the other hand. NACE International. Aug-98. Mar 26-31. Oct-97. Rooney/Bacon/DuPart (Dow Chemical). Hydrocarbon Processing. Corrosion/95. Hydrocarbon Processing.” Liu/ Dean/Bosen (Union Carbide). unpublished studies suggest that caustic can effectively increase HSS levels by fixing the acid anions to the point of inhibiting their tendency to otherwise be regenerated in the regenerator. Mar-96. Cummings/Mecum (MPR Services). there was once a widely-held belief that it reduced corrosion by elevating the pH and suppressing ionization. continued to maintain that corrosivity is generally reduced by neutralization. “Neutralization Technology to Reduce Corrosion from Heat Stable Amine Salts. Union Carbide and Dow Chemical. Mecum/Veatch/Cummings (MPR Services). The views of both camps are typified by the following articles (among others): • • • • “Why Caustic Addition is Bad for Amine Systems”. Hydrocarbon Processing. In addition. “Effect of Heat Stable Salts on MDEA Solution Corrosivity”. 05/23/07 Amine Best Practices Group Page 60 . “Remove Heat Stable Salts for Better Amine Plant Performance”. and in fact is sometimes made worse. and Carbide went so far as to market an alternative to caustic called DHM. The consensus of the ABPG is that caustic should not be added. However. contradictory corrosion studies within the past 10 years have resulted in controversy. ConocoPhillips and MPR Services asserted that corrosivity of the HSS anions is not reduced by caustic. In addition. 1995.Caustic Neutralization “Neutralization” with caustic has long been practiced as an economical means of displacing bound amine from heat stable salts.
Service. and via the reflux NH3 purge and miscellaneous physical losses. steam can be injected into the regenerator. In the absence of a convenient source of condensate or demineralized water. 05/23/07 Amine Best Practices Group Page 61 . Makeup is usually accomplished by periodic manual adjustment basis inventory.Water Balance Water must be added to the amine system to replace that lost as vapor in the treated and acid gas streams. fouling and foaming. Makeup water should be condensate-quality. with determination of free amine strength at sufficient frequency to ensure operation within established limits. and even boiler feed. water should be avoided due to dissolved solids and treatment chemicals that can accumulate in the system to cause corrosion.
flotation. usage should be minimized for two reasons: • Antifoam is itself a surfactant.Foaming Minor foaming can adversely impact absorption and/or stripping efficiency. If occasional antifoam addition has been found necessary. only surfactant HC components – aromatics and soaps. but they stabilize it. In the event of tower instability. in particular – cause foaming. Excessive iron sulfide particles are also associated with foaming. which are readily evidenced by a hazy or milky appearance. Technically. thus reducing the carbon’s capacity to adsorb the organics typically responsible for foaming. Regenerator foaming is often caused by such HC buildup in the reflux. Silicone antifoam is not advised. as it tends to foul equipment. Typical symptoms of the latter are: • Low/erratic tower levels and bottoms rates • Erratic offgas rates • Liquid carryover • Increased/erratic tower pressure differential Foaming is commonly attributed to HCs. • Antifoam is adsorbed by carbon. however. they do not cause foam. and excessive dosages can actually promote foaming. Technically. Inc. resin filtration or D-Foam. Ideally. More severe episodes can result in tray flooding. surfactant buildup is avoided by carbon filtration. purging reflux is the first corrective action to try. 05/23/07 Amine Best Practices Group Page 62 . without obvious tower instability. Surfactants may also cause HC emulsions.
05/23/07 Amine Best Practices Group Page 63 . it is easier to routinely monitor the H2S. potentially fouling the header with solid ammonium hydrosulfide (NH4HS). as the NH3 and H2S concentration of the reflux approaches saturation. NH3 will start leaking through to the SRU. Often. Also. where 2 wt-% would be the corresponding target (neglecting CO2). but then reabsorbed in the reflux. Excessive NH3 buildup also increases reboiler steam demand to a predictable degree. It will be stripped out in the regenerator. Initially. relative CO2/H2S levels should be determined to ensure that CO2 corrosion is being adequately mitigated. it will likely contain minor levels of NH3 which will be absorbed in the amine by virtue of its water solubility. Alternatively.Ammonia Unless refinery contactor feed gas is effectively water washed. the first indication is plugged instrument taps. Common industry practice is to periodically measure the NH3 content of the reflux and purge as necessary to maintain ~ 1 wt-%. H2S re-absorption in the reflux will increase in proportion to the NH3 buildup until levels are so high as to become corrosive.
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