Commissioning of first world scale KBR PurifierTM ammonia plant in

North America

The Dyno Nobel Louisiana Ammonia (DNLA) project is one of the biggest expansion activities ever undertaken by its Australian based parent company, Incitec Pivot Ltd (IPL), increasing the annual ammonia production by about 800,000 tonnes per year. The Engineering, Procurement, and Con-struction (EPC) for this project was carried out by the Houston, TX based Kellogg Brown & Root

(KBR) using their PurifierTM ammonia technology and project ground breaking was commenced in August 2013.

In mid-2015, KBR completed the construction of Dyno Nobel's Waggaman ammonia plant in Louisi-ana and commenced start-up activities of its 2300 MTPD Ammonia Plant – the first world scale KBR

PurifierTM technology based ammonia plant in North America.

Commissioning was successfully completed in October 2016 with one of the lowest energy consump-tion figures per tonne of ammonia. This paper presents an overview of the project and its journey

through the various stages of project development, design, engineering, and construction as well as challenges experienced in whole project process. It also describes both KBR and Dyno Nobel experi-ence in the commissioning and start-up of the process facilities, the problems encountered and key

lessons learned during the commissioning.

Venkat Pattabathula, Chris Morgan and Morris Hofman

Dyno Nobel Inc.

George Colman and Avinash Malhotra Kellogg Brown & Root (KBR)

Introduction he growth of ammonia industry has been languishing in the USA for about 30 years. However a step change has oc-curred since the shale gas industry was

developed and the gas prices became affordable and therefore attractive to the ammonia produc-ers. Hence, more ammonia capacity is being

added to supplement existing operating capaci-ties to meet the USA’s ammonia demand. Australia’s, Incitec Pivot, the parent company of Dyno Nobel Louisiana Ammonia (DNLA), in-stalled the plant with an annual ammonia capac-ity of 800,000 metric tons at Cornerstone Chem-ical’s 800-acre Fortier Manufacturing Complex at Waggaman in Louisiana (WALA).

T

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Dyno Nobel operates ammonium nitrate facili-ties in some of the states in the US. Incitec Pivot Limited developed the Dyno Nobel ammonia plant to support its U.S. industrial explosives business and external customers including Cor-nerstone which produces acrylonitrile, mela-mine and sulfuric acid at the Fortier complex. Dyno Nobel’s ammonia plant is integrated with Cornerstone’s existing plant infrastructure and share utilities and facilities such as the river ex-port dock, the rail facilities and the ability to in-ject ammonia in to the 2000 mile Nustar ammo-nia distribution pipeline It is the first ammonia plant to have been built in the state of Louisiana in over 25 years. The Dyno Nobel new ammonia plant utilizes the KBR PurifierTM ammonia technology. The plant is a world scale KBR PurifierTM plant having a design capacity of 2300 MTPD (2536 STPD). Ammonia Process Design Features The Ammonia Plant is based on the KBR Puri-fierTM flowsheet as shown in Figure-A1 and another image of nightline view of the plant is shown in Figure A-2. The plant design is based upon the natural gas composition listed in Table-1 below.

Components Mole Fraction,% CH4 97.98 C2H6 0.78 C3H8 0.11 C4H10 0.04 C5H12 0.02 C6H14 0.01 N2 0.31 CO2 0.75

Table 1. Natural Gas Feed Composition The salient design features of the Dyno Nobel Waggaman, Louisiana (WALA) plant are:

Mild conditions for primary reforming

via excess air to the secondary reformer Primary reformer having only steam tur-

bine driven forced and induced draft fans

KBR’s natural circulation, removable tube bundle water tube Waste Boiler De-sign, downstream of secondary reformer.

KBR’s nonmetallic Mixing Chamber (no metallic mixer or burner) in the Second-ary Reformer.

BASF’s two stage CO2 removal system using the OASE White (activated MDEA) solvent.

KBR PurifierTM for providing a clean, dry makeup of synthesis gas to Synthesis Loop. PurifierTM precisely controls H2: N2 ratio and removes all methane and the majority of the argon present.

KBR’s cold wall single Horizontal Am-monia Synthesis Converter with 3 cata-lyst beds and 2 interchangers

KBR’s four stage Unitized Chiller in synthesis loop.

No separate purge gas - Hydrogen Re-covery System is required.

Two flares one for front and other one for back-end vent headers.

Selective catalytic reduction (SCR) unit in reformer convection section to reduce NOx levels in flue gas

Use of KBR’s operator training simula-tor

Plant uses catalysts supplied by KBR/Clariant that includes non-hexavalent chrome HTS catalyst and Wustite based AmoMax Synthesis cata-lyst.

For plant start-up, the feed gas compressor is utilized for front end nitrogen recirculation.

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Plant Performance The plant performance guarantee test was conducted over a 72-hour period in October 2016 with all guarantees successfully met: Guarantee item Guarantee

value Measured Value

Ammonia production, st/d

2536 2576

Ammonia product quality: NH3,% H2O,%

99.8 min. 0.2 max.

99.99 0.01

Net energy consumption, MMBtu/ton, LHV

25.09 24.84

Inerts in CO2, % 2 max. 0.17 Carbon dioxide purity CO2,%

98.0 min.

99.83

Table 2. Guarantee & Measured Numbers In addition to the above, environmental re-quirements were also met as part of perfor-mance guarantees and those were listed in Table 3. Guarantee Item Guarantee Value NOX 10 ppmv dry basis Carbon Monoxide 50 ppmv dry basis Ammonia 10 ppmv dry basis Particulate Matter PM10

7.1 lbs/hr

Table 3 – Environmental Performance Project Execution The project kick-off was in September 2012 with an Engineering, Procurement and Construction scheme (EPC Contract) as a lump sum turnkey project. The EPC contract was awarded to Kellogg Brown & Root (KBR). Beside the ammonia plant, the project also con-sisted of a 35,000 MT ammonia storage tank, barge and road tanker loading system and utility plants that included water clarifier (Coag unit),

cooling water system, Ultra Filtration (UF), re-verse osmosis (RO) unit and Ion Exchange (mixed beds) units. Ground breaking occurred in August 2013 with the plant mechanical acceptance having achieved in March 2016, and commercial operation declared in September 2016. The main project milestones are listed in Table-4. Major Events Date Effective date of contract 13 April 2013 Basic engineering completion 15 June 2013 Detail engineering completion

End 2014

Ground breaking 5 Aug 2013 Precommissioning phase July 2015 -

March 2016 Natural gas receiving Oct 2015 Commissioning start (Reformer 1st firing)

25April 2016

Feed-in to primary reformer 9 May 2016 Syngas compressor start 26 June 2016 Catalyst reduction of ammo-nia synthesis converter start

24 July 2016

First ammonia produced 27 July 2016 Performance test completed 13 Oct 2016 Plant acceptance 19 Oct 2016 Table 4. Key Milestones of DNLA Project First ammonia production was successfully ac-complished 78 days after the initial introduction of natural gas feed. However, during plant ini-tial operation, numerous issues were encoun-tered which required an additional 3 months be-fore the plant performance tests were successfully completed. The project used a local construction workforce of around 1200 at peak construction activity. Safety Performance The project achieved outstanding Zero Harm performance with 5 million work hours without a single lost time injury (LTI). This is a merito-rious achievement on a project of this size.

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Commissioning and Start-Up As part of EPC contract, KBR has provided a complete team for start-up, supported by Dyno Nobel’s project team and Cornerstone’s opera-tions team. KBR also trained Dyno operations team using a dynamic process simulator in addi-tion to class room training. Problems that arose during plant commissioning were jointly resolved by the KBR EPC, Technology and owner’s process, electrical, instrument, and mechanical teams. Use of Temporary Boilers Due to project contractual and schedule con-straints, very early in the project KBR was to supply the MP steam requirement for plant pre-commissioning, commissioning, and initial startup/operation from portable boilers. To meet the plant’s peak MP steam demand of about 300,000 lbs/hr (136,000 kgs/hr) four port-able boilers were installed. Additionally, an air emissions permit was ob-tained from the state of Louisiana to operate the boilers. Each boiler was capable of producing 75,000 lbs/ hr (34,000 kgs/hr) of steam at a pressure of 750psig (5171 kPag) and a temperature of 750F (400C). The use of the portable boilers required the in-stallation of additional systems for:

a) Supply of boiler feed water, natural gas for fuel, instrument air, steam drum treatment chemicals

b) Collection and cooling of boiler steam drum blowdown water

c) Instrumentation and controls

Figure 1. Temporary Boilers

Figure 1a. Temporary Boilers

Challenges Experienced During Commissioning Below is a summary of some of the main issues encountered during the plant initial start-up and operation. Successful commissioning of an ammonia plant requires careful planning and utilization of les-sons learned from other successful startups. Equipment Preservation Equipment preservation is an essential compo-nent of any project implementation plan. The purpose of an equipment preservation program is to ensure that all new equipment remains in

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the same condition as it left the factory until it is placed in service during the initial plant start-up. Typically equipment preservation programs comprise of the following key elements:

a) Initial preservation – application of pre-servatives and the fitting of specific pro-tection to equipment by suppliers prior to equipment shipment

b) Maintenance preservation – periodic ac-tivities to confirm the initial preservation is intact and functioning. This also in-cludes the repair of deteriorated initial preservation and also performing any additional supplier recommended field preservation activities

c) The regular rotating of pumps and com-pressors is essential to ensure that bear-ings and shafts are not damaged.

d) Preservation renewal – if the time be-tween the initial preservation and plac-ing of the equipment into service ex-ceeds that stated in the equipment supplier preservation guidelines, then it will be necessary to seek the equipment supplier’s advice as to the requirement to renew the initial preservations

During plant construction and commissioning, especially after the start of the hydro test pro-gram additional attention is required to ensuring that equipment preservation requirements are maintained. The following photographs show some exam-ples from the Dyno Nobel ammonia plant pro-ject of equipment damage resulting from com-promised equipment preservation. The WALA project experience highlights the importance of a robust equipment preservation program, thorough plant pre-start-up checkout, and effective pre-commissioning practices.

Figure 2. Steam turbine 108JT Rotor

Figure 2a. Damaged TTV

Damage caused by compromised equipment preservation resulted in additional project costs and numerous delays to the plant pre-commissioning, commissioning, and initial start-up schedules. Process Air Machine Damage Air for the process is supplied by a six stage in-tegrally geared compressor supplied by Sie-mens. The air compressor is fitted with shell and tube inter stage coolers. During machine surge mapping, the process air machine tripped on high 5th stage vibrations. In the ensuing trip an oil leak from the bull gear

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assembly ignited causing a small flash fire which was rapidly extinguished. Also during the machine trip, the 6th stage process air discharge pipe work was dislodged from its supports. Opening of the machine revealed the damage shown in the following photographs.

Figure 3. Parts of hessian sack found in com-

pressor

Figure 4. Impeller damage

Figure 5. Stage 5 Impeller

Figure 6. Stage 6 Impeller

Figure 7. Dislocated piping support

Figure 8. Stage 5 tie bolt

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An incident investigation pinpointed the root cause of the compressor trip and damage to be a hessian (burlap) sack containing bead blast ma-terial which became dis-lodged from the shell side of the intercooler located between the 4th and 5th stages and entered the 5th stage of the machine. Repair work necessitated the complete disman-tling of the compressor/bull gear end of the ma-chine which was then returned to a Siemens workshop in Houston for repair and reassembly. Machine repairs and reassembly took a total of 9 weeks. OASE White Solution System Foaming of the recirculating OASE White solu-tion may cause a major process upset resulting in an interruption to ammonia production or worst case scenario of a loss of containment of the OASE White solution through the carbon dioxide atmospheric vent into the surrounding plant environment. The keys to preventing foaming of the OASE White solution are:

a) System cleaning during plant pre-commissioning to ensure effective re-moval of foam causing agents such as oils, greases, and fine particle/dusts

b) Low temperature shift catalyst de-dusting following catalyst reduction

c) Continuous filtration of the recirculating OASE White solution during plant initial start-up/operation

d) Close management of the anti-foam ad-dition program in the plant initial start-up/operation.

During the Dyno Nobel project due to a multi-tude of reasons the cleaning of the OASE White system was not completely effective. To miti-gate the effect of a less than effective system cleaning upon initial plant operation, a tempo-rary side stream carbon bed filtration unit was installed. The temporary filtration unit has helped to bring the color of the recirculating

OASE solution to normal and side stream filters remained in service for 3 months until the 5 mi-cron filter socks would operate for five continu-ous days without increasing pressure drop. Additionally, to preempt the occurrence of foaming, foaming tests were carried out twice a shift of the recirculating OASE White solution and adjustments were made to the anti-foam in-jection program which comprised of continuous injection using the installed anti-foam injection pump skid and also each shift “shot” dosing us-ing the installed “shot pots”. The aforemen-tioned measures resulted in zero OASE White solution foaming events during the plant initial start-up/operation period. High Pressure Leak Checking The synthesis section of modern day ammonia plants operate at pressures up to 165kg/cm2(g) (2347 psig) temperatures up to 530oC (986F) and contains process gas with hydrogen concen-trations of up to 75 mole%. In the event of a process gas leak from this section of the plant there is a high degree of probability that a hy-drogen jet fire could potentially occur causing severe damage to surrounding plant and equip-ment. To mitigate such an event KBR took the deci-sion to perform a rigorous high pressure leak check before initial plant start-up at a pressure 90% of the lowest set pressure relief device of the ammonia synthesis loop. The leak check was performed after completion of both ammonia synthesis catalyst loading and ammonia synthe-sis converter box-up and included all associated instrumentation. To prevent an uncontrolled oxidation of pre-reduced ammonia synthesis catalyst contained in the 1st bed of the ammonia synthesis convert-er it was necessary to perform the leak check with high pressure gaseous nitrogen supplied at ambient temperature from a liquid nitrogen pumper truck. The leak check was performed in

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pressure increments of 20kg/cm2 (300 psig). While holding at each pressure increment all po-tential leakage points were checked for signs of leakage using a leak detection fluid.

Figure 9. Liquid Nitrogen Pumper Truck

The aforementioned leak checking revealed numerous leaks which were fully remediated prior to the introduction of process gas to the ammonia synthesis loop both eliminating a po-tential serious safety hazard and also shortening the critical path to the production of the 1st drops of ammonia. Tuning Of Synthesis Gas Compressor Perfor-mance Control A key element to the successful operation of the PurifierTM package unit in the Dyno Nobel am-monia plant project is the tuning of the synthesis gas compressor performance controller. The pressure of the process gas at the suction of the synthesis gas compressor is controlled by the synthesis gas compressor performance con-troller which modulate the synthesis gas com-pressor speed to maintain this pressure steady. In the case of the Dyno Nobel plant the synthe-sis gas compressor performance controller was tuned such that the variations in suction pressure are less than +/- 0.25psi.

Figure 10. Syngas compressor suction pressure trend chart Summary Despite the problems faced, the Dyno Nobel, WALA plant successfully met all its energy consumption, production, and product quality guarantees. The project was a great success with more than 5 million work hours LTI free and the project came online ahead of other similar scale major ammonia projects in the continent. Acknowledgement We would like to acknowledge the untiring ef-forts put in by KBR and WALA teams in the successful commissioning of the first world scale KBR PurifierTM plant in North America.

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