NHT Catalyst Activation ORC-I (Updated)

BYCO PETROLEUM PAKISTAN LIMITED
STANDARD OPERATING PROCEDURE

NHT CATALYST GAS PHASE ACTIVATION PROCEDURE
Document No: BPPL-OPS(I)-SP-LEVEL-III-
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Issue Date: 23-Dec-2020 Revision No: 00
CONTROLLED: COPY RIGHT ©Please don’t copy without authorization

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DOCUMENT CHANGE RECORD
REV. NO DESCRIPTION OF CHANGE EFFECTIVE DATE
00 Initial Release 23-12-2020

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DOCUMENT DISTRIBUTION RECORD
DEPARTMENTS/HODS/OTHERS COPY NUMBER SIGNATURE
CCR ORC-I 1
Document Control Room 2

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1.0 TABLE OF CONTENTS

1.0 TABLE OF CONTENTS...........................................................................................4
2.0 PURPOSE...................................................................................................................5
3.0 SCOPE...........................................................................................................................
..........................................................................................................................5
4.0 DEFINITIONS, ABBREVIATIONS AND CONCEPTS........................................5
4.1 ABBREVIATIONS.........................................................................................5
5.0 RESPONSIBILITIES AND AUTHORITIES..........................................................6
6.0 STEPS FOR CATALYST ACTIVATION...............................................................6
6.1 CATALYST DRYING....................................................................................6
6.2 PRE-SULFIDING OF CATALYST................................................................6
7.0 PROCEDURE.............................................................................................................7
7.1 PRE-STARTUP...............................................................................................7
7.2 DRYING..........................................................................................................7
7.3 PRE-SULFIDING............................................................................................7
8.0 REQUIREMENT OF ENVIRONMENT, HEALTH & SAFETY.........................9
8.1 ENVIRONMENT............................................................................................9
8.2 HEALTH.........................................................................................................9
8.3 SAFETY..........................................................................................................9
9.0 REFERENCE.............................................................................................................9

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2.0 PURPOSE
The purpose of this procedure is to set guidelines for HDT unit Catalyst Activation through gas
phase which includes Dry out of Catalyst and Pre-Sulfiding of Catalyst
3.0 SCOPE
This procedure is to be followed by Shift Managers, Shift Incharges, DCS Operators and Area
Operators of ORC-I for dry out and pre-sulfiding activity of NHT Reactor Catalyst
4.0 DEFINITIONS, ABBREVIATIONS AND CONCEPTS

4.1 ABBREVIATIONS
 ORC-I Oil Refining Complex-I
 BPPL Byco Petroleum Pakistan Limited
 HDTU Hydro Treating Unit
 CDU Crude Distillation Unit
 Reformer Plat-former Unit
 PCV Pressure Control Valve
 LCV Level Control Valve
 TCV Temperature Control valve
 FCV Flow Control Valve
 LPG Liquefy Petroleum Gas
 L/N Light Naphtha
 H/N Heavy Naphtha
 H2 Hydrogen
 N2 Nitrogen
 RIT Reactor Inlet Temperature
 ROT Reactor Outlet Temperature
 SDV Emergency Shutdown valve
 SCFB Standard Cubic Feet per Barrel
 LL Low Low
 BPD Barrels Per Day
 Bbl Barrel
 Lbs Pounds
 SV Set Value

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5.0 RESPONSIBILITIES AND AUTHORITIES

 GM Production
 Sr. Manager Production
 Manager Production
 Shift Manager Production
 Shift in-charge (ORC-I) Production
 DCS/Area Operator (ORC-I) Production
6.0 STEPS FOR CATALYST ACTIVATION

Hydro-processing catalysts as manufactured consist of an alumina carrier impregnated with oxides
of different combinations of metals. For the metal oxides to be in the active state, they have to be
converted to sulfides.
The activation step is critical for the subsequent performance of the catalyst charge and therefore
requires careful attention and monitoring. During the activation, the catalyst will typically pick up
sulfur, 5-13wt%, depending on the amount of active metals present in the catalyst.
The procedure for the activation of NHT reactor catalyst (gas phase) encompasses two major steps:
6.1 CATALYST DRYING
The catalyst is hygroscopic due to high porosity and will contain some water from production and
can take up more during loading from the moisture in the air. Drying phase ensures that adsorbed
water will be removed prior to sulfiding phase. Metal dispersion can be affected by water if not
removed.
A fast heat-up can lead to steam formation, and the corresponding rapid volume expansion inside
the catalyst particles can lead to sufficient pressure to break the catalyst. The broken catalyst can
lead to pressure drop issues and, in severe cases, require a skim or complete replacement of
catalysts. During an oil-phase drying, water can be trapped to a greater extent in the catalyst pores.
The potentially higher temperatures can convert the water to steam and lead to structural changes
and a loss of porosity and, in some cases, loss of catalyst activity.
Drying is normally conducted by passing a hydrogen rich stream over the catalyst at the normal
operating pressure of the unit with some help of temperature. The water will then evaporate and will
typically be collected in product separator from where it can conveniently be drained off
6.2 PRE-SULFIDING OF CATALYST
Hydro treating catalysts; both Nickel Molybdenum (Ni-Mo) and Cobalt Molybdenum (Co-Mo) are
manufactured with the promoter metals in an oxide state. Prior to use as for sulfur removal, these
metals must be converted to a sulfided state. This improves the catalyst activity and prolongs the
run length between regenerations.
Pre-Sulfiding is achieved by injecting a Sulfiding agent such as DMDS (Di-Methyl Di-Sulfide) at a
controlled rate, to the naphtha feed with the reactor temperature at a lower level than normal, and
holding these conditions until H2S breakthrough is achieved. Breakthrough is achieved when H2S in
the reactor effluent off-gas reaches 2000-3000 ppm. This should not occur until sufficient sulfur

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added via the MERcaptan has reached 10% wt. of the catalyst. Prior to break through, the
anticipated H2S level will be less than 200 ppm.

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7.0 PROCEDURE
7.1 PRE-STARTUP
7.1.1 Make sure that all the requisites of NHT unit startup are fulfilled refer to HDT Startup
Procedure (BPPL-OPS-SOP-19)
7.1.2 Ensure that DMDS facility is commissioned as per approved procedure followed by
successful leak test
7.1.3 Unit and reactor is Oxygen free (<0.5% vol. O2) and leak test is done
7.1.4 Ensure the availability of fuel gas either from Tankfarm or from ORC-II
7.1.5 Make sure that hydrogen flow is continuous from ORC-II. The requirement of
Hydrogen flow during Pre-Sulfiding will be 1500-1900 lbs/hr. (1.77-2.24 MMSCFD)
as recommended by Technical department
7.1.6 Ensure that the Hydrogen Purity is greater than 70% throughout the activity
7.1.7 Since the catalyst activation is through gas phase, keep the naphtha lineup upstream of
FCV-301 and from D8-302 to LCV-301 isolated
7.1.8 Pressurize the reformer system up to 12.1 kg/cm 2 from ORC-II and put PCV-340B on
auto mode with SV=12.1 kg/cm2
7.1.9 Lineup PCV-340B and PCV-325 to fuel gas and make sure that the flare system is
ready
7.2 DRYING
7.2.1 Pressurize NHT system gradually via PCV-360 bypass line up to 12.1 kg/cm2
7.2.2 Put PCV-325 on auto control with SV=15.5 kg/cm2 (Normal operating pressure)
7.2.3 Commission PCV-340A and PCV-360. Make sure that by-pass valve of both
controllers must be isolated
7.2.4 Fill up start-up checklist for Booster compressor (BPPL-OPS-CL-17A)
7.2.5 Start Booster gas compressor D4-303/D4-304 and gradually increase the hydrogen
flow to maximum though PCV-360
7.2.6 Light up NHT heater D1-301 as per procedure (BPPL-OPS-SOP-21)
7.2.7 Ramp up RIT gradually at the rate of 200C/hr. to 1500C
Caution: In order to minimize the risk of leaks due to thermal expansion, the
recommended maximum rate for heating up the catalyst is 250C/hr
7.2.8 Maintain the reactor inlet temperature at 1500C
7.2.9 Make sure that both fans D2-302 and D2-308 are in operation and cooling water flow
is maximum to D2-303. Check and drain water from product separator
Caution: Reactor Bed Temperature should not exceed 1750C at any time during catalyst
drying operation
7.2.10 When all catalyst bed temperatures have reached a minimum of 1200C or when the
reactor inlet temperature has been kept at 1500C for maximum 12 hours, the heat-up is
considered complete. No separate dry-out step is required

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7.3 PRE-SULFIDING
7.3.1 Make sure that the hydrogen content of circulating gas is measured and in case
hydrogen content drops below 70 vol.% at any time during catalyst sulfiding, the
reactor section must be purged/vented, and hydrogen-rich make-up gas should be
introduced to the unit
7.3.2 Increase RIT to 1900C at the rate of 150C/hr. Keep the gas flow rate to maximum
7.3.3 Check the level of DMDS Vessel (D8-317) and make sure that vessel is filled with
DMDS
7.3.4 When RIT=1900C and catalyst bed temperature have reached minimum of 1750C, start
DMDS injection at initial dosing rate (to be given by Technical department) to the
reactor inlet point
Caution: If an issue arises with the initiation of DMDS injection, temperature ramping
should be suspended until the injection can be started. The reactor inlet
temperature should be maintained below 1900C during this period
7.3.5 After 2-3 hours of DMDS injection, start sampling Separator off gas for H 2S
concentration on hourly basis
7.3.6 Increase RIT to 2250C at the rate of 150C/hr. and steadily increase DMDS injection
rate to recommended dosing rate (as per guidelines by Technical)
Caution: Due to the risk of undesirably high reactor outlet temperature resulting from a
high reactor exotherm, the initial addition of DMDS should be low. The
maximum reactor temperature during this initial sulfiding step should never
exceed 2500C
7.3.7 Maintain the conditions (RIT = 2250C and recommended dosing rate) until H2S
breakthrough is achieved (Breakthrough – when two consecutive measurements of H-
2S shows level above 3000 ppmv)
7.3.8 After confirming breakthrough, rise the RIT to target catalyst bed temperature 3300C
at the rate of 150C/hr.
7.3.9 During this final phase of sulfiding, RIT and DMDS injection should be adjusted in
order to maintain the reactor bed temperatures at maximum 3300C
Caution: Temperature ramp up should be paused if H2S content of gas drops below 3000
ppmv and/or if temperature difference between reactor inlet and outlet is higher
than 100C
7.3.10 When the catalyst beds have been exposed at maximum 3300C for a minimum of four
hours, the catalyst sulfiding is considered complete
7.3.11 At this point, the addition of DMDS can be terminated as long as the recycle gas H 2S
remains above 1,000 ppmv
Caution: Do not disconnect DMDS facilities until after once-through, fresh straight-run
feed flow has been established, and unit is producing H2S
7.3.12 Reduce RIT to maximum 1750C at the rate of 250C/hr.
7.3.13 Introduce naphtha feed as per SOP and gradually increase the feed to design flow rate
while maintaining the temperature

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7.3.14 Adjust the operating conditions to normal start-of-run operation for required product
specification
7.3.15 In order to precondition the catalyst to the operation, the unit should be fed with
straight-run feedstock for a minimum of 48 hours upon completion of catalyst sulfiding
8.0 REQUIREMENT OF ENVIRONMENT, HEALTH & SAFETY

8.1 ENVIRONMENT
 Draining of hydrocarbon into API should be kept control and should not be left unattended
8.2 HEALTH
 Dust mask, Ear plugs/Ear muffs, Hand gloves, safety shoes and safety helmet and safety
glasses must be used while working in the area
 During DMDS handling, chemical suite, chemical gloves and H2S mask must be worn
8.3 SAFETY
 Area should be cleaned and free from all foreign materials such as wooden/steel planks,
nut bolts, cotton waste, drums etc.
 All safety equipment’s are in place and operable
 API sewer freely working without any plugging
 Eye washers are in good working condition
 Maintain good communication system
9.0 REFERENCE
 HDT Startup Procedure (BPPL-OPS-SOP-19)
 NHT/REF Furnace Start-up Procedure (BPPL-OPS-SOP-21)
 Hydroprocessing Catalyst Manual – HALDOR TOPSOE

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BYCO PETROLEUM PAKISTAN LIMITED

STANDARD OPERATING PROCEDURE

CONTROLLED: COPY RIGHT ©Please don’t copy without authorization

REV. NO DESCRIPTION OF CHANGE EFFECTIVE DATE

00 Initial Release 23-12-2020

CONTROLLED: COPY RIGHT ©Please don’t copy without authorization

DEPARTMENTS/HODS/OTHERS COPY NUMBER SIGNATURE

Document Control Room 2

CONTROLLED: COPY RIGHT ©Please don’t copy without authorization

1.0 TABLE OF CONTENTS

CONTROLLED: COPY RIGHT ©Please don’t copy without authorization

4.0 DEFINITIONS, ABBREVIATIONS AND CONCEPTS

CONTROLLED: COPY RIGHT ©Please don’t copy without authorization

5.0 RESPONSIBILITIES AND AUTHORITIES

6.0 STEPS FOR CATALYST ACTIVATION

CONTROLLED: COPY RIGHT ©Please don’t copy without authorization

CONTROLLED: COPY RIGHT ©Please don’t copy without authorization

CONTROLLED: COPY RIGHT ©Please don’t copy without authorization

CONTROLLED: COPY RIGHT ©Please don’t copy without authorization

8.0 REQUIREMENT OF ENVIRONMENT, HEALTH & SAFETY

CONTROLLED: COPY RIGHT ©Please don’t copy without authorization

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